section_id,title_number,title_name,chapter,subchapter,part_number,part_name,subpart,subpart_name,section_number,section_heading,agency,authority,source_citation,amendment_citations,full_text 21:21:3.0.1.1.9.2.1.1,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",B,Subpart B—Substances Utilized To Control the Growth of Microorganisms,,§ 178.1005 Hydrogen peroxide solution.,FDA,,,"[46 FR 2342, Jan. 9, 1981, as amended at 49 FR 10111, Mar. 19, 1984; 49 FR 32345, Aug. 14, 1984; 49 FR 37747, Sept. 26, 1984; 51 FR 45881, Dec. 23, 1986; 52 FR 26146, July 13, 1987; 53 FR 47186, Nov. 22, 1988; 54 FR 5604, Feb. 6, 1989; 54 FR 13167, Mar. 31, 1989; 54 FR 6365 Feb. 9, 1989; 55 FR 47055, Nov. 9, 1990; 57 FR 32423, July 22, 1992; 78 FR 71467, Nov. 29, 2013]","Hydrogen peroxide solution identified in this section may be safely used to sterilize polymeric food-contact surfaces identified in paragraph (e)(1) of this section. (a) Identity. For the purpose of this section, hydrogen peroxide solution is an aqueous solution containing not more than 35 percent hydrogen peroxide (CAS Reg. No. 7722-84-1) by weight, meeting the specifications prescribed in paragraph (c) of this section. (b) Optional adjuvant substances. Hydrogen peroxide solution identified in paragraph (a) of this section may contain substances generally recognized as safe in or on food, substances generally recognized for their intended use in food packaging, substances used in accordance with a prior sanction or approval, and substances permitted by applicable regulations in parts 174 through 179 of this chapter. (c) Specifications. Hydrogen peroxide solution shall meet the specifications of the Food Chemicals Codex, 7th ed. (2010), pp. 496-497, which is incorporated by reference. Hydrogen peroxide solution shall also meet the specifications for “Acidity,” “Chloride,” and “Other requirements” for Hydrogen Peroxide Concentrate in the United States Pharmacopeia 36th Revision (2013), pp. 3848-3849, which is incorporated by reference. The Director of the Office of the Federal Register approves this incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. You may obtain copies from the United States Pharmacopeial Convention, 12601 Twinbrook Pkwy., Rockville, MD 20852 (Internet address http://www.usp.org ). Copies may be examined at the Food and Drug Administration's Main Library, 10903 New Hampshire Ave., Bldg. 2, Third Floor, Silver Spring, MD 20993, 301-796-2039, or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030 or go to: http://www.archives.gov/federal-register/cfr/ibr-locations.html. (d) Limitations. No use of hydrogen peroxide solution in the sterilization of food packaging material shall be considered to be in compliance if more than 0.5 part per million of hydrogen peroxide can be determined in distilled water packaged under production conditions (assay to be performed immediately after packaging). (e) Conditions of use. (1) Hydrogen peroxide solution identified in and complying with the specifications in this section may be used by itself or in combination with other processes to treat food-contact surfaces to attain commercial sterility at least equivalent to that attainable by thermal processing for metal containers as provided for in part 113 of this chapter. Food-contact surfaces include the following: (2) The packaging materials identified in paragraph (e)(1) of this section may be used for packaging all commercially sterile foods except that the olefin polymers may be used in articles for packaging foods only of the types identified in § 176.170(c) of this chapter, table 1, under Categories I, II, III, IV-B, V, and VI. (3) Processed foods packaged in the materials identified in paragraph (e)(1) of this section shall conform with parts 108, 110, 113, and 114 of this chapter as applicable." 21:21:3.0.1.1.9.2.1.2,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",B,Subpart B—Substances Utilized To Control the Growth of Microorganisms,,§ 178.1010 Sanitizing solutions.,FDA,,,"[42 FR 14609, Mar. 16, 1977]","Sanitizing solutions may be safely used on food-processing equipment and utensils, and on other food-contact articles as specified in this section, within the following prescribed conditions: (a) Such sanitizing solutions are used, followed by adequate draining, before contact with food. (b) The solutions consist of one of the following, to which may be added components generally recognized as safe and components which are permitted by prior sanction or approval. (1) An aqueous solution containing potassium, sodium, or calcium hypochlorite, with or without the bromides of potassium, sodium, or calcium. (2) An aqueous solution containing dichloroisocyanuric acid, trichloroisocyanuric acid, or the sodium or potassium salts of these acids, with or without the bromides of potassium, sodium, or calcium. (3) An aqueous solution containing potassium iodide, sodium p -toluenesulfonchloroamide, and sodium lauryl sulfate. (4) An aqueous solution containing iodine, butoxy monoether of mixed (ethylene-propylene) polyalkylene glycol having a cloudpoint of 90°-100 °C in 0.5 percent aqueous solution and an average molecular weight of 3,300, and ethylene glycol monobutyl ether. Additionally, the aqueous solution may contain diethylene glycol monoethyl ether as an optional ingredient. (5) An aqueous solution containing elemental iodine, hydriodic acid, a -( p -nonylphenyl)- omega -hydroxypoly-(oxyethylene) (complying with the identity prescribed in § 178.3400(c) and having a maximum average molecular weight of 748) and/or polyoxyethylene-polyoxypropylene block polymers (having a minimum average molecular weight of 1,900). Additionally, the aqueous solution may contain isopropyl alcohol as an optional ingredient. (6) An aqueous solution containing elemental iodine, sodium iodide, sodium dioctylsulfosuccinate, and polyoxyethylene-polyoxypropylene block polymers (having a minimum average molecular weight of 1,900). (7) An aqueous solution containing dodecylbenzenesulfonic acid and either isopropyl alcohol or polyoxyethylene-polyoxypropylene block polymers (having a minimum average molecular weight of 2,800). In addition to use on food-processing equipment and utensils, this solution may be used on glass bottles and other glass containers intended for holding milk. (8) An aqueous solution containing elemental iodine, butoxy monoether of mixed (ethylene-propylene) polyalkylene glycol having a minimum average molecular weight of 2,400 and α-lauroyl- omega -hydroxypoly (oxyethylene) with an average 8-9 moles of ethylene oxide and an average molecular weight of 400. In addition to use on food-processing equipment and utensils, this solution may be used on beverage containers, including milk containers or equipment. Rinse water treated with this solution can be recirculated as a preliminary rinse. It is not to be used as final rinse. (9) An aqueous solution containing n -alkyl (C 12 -C 18 ) benzyldimethylam-monium chloride compounds having average molecular weights of 351 to 380. The alkyl groups consist principally of groups with 12 to 16 carbon atoms and contain not more than 1 percent each of groups with 8 and 10 carbon atoms. Additionally, the aqueous solution may contain either ethyl alcohol or isopropyl alcohol as an optional ingredient. (10) An aqueous solution containing trichloromelamine and either sodium lauryl sulfate or dodecyl- benzenesulfonic acid. In addition to use on food-processing equipment and utensils and other food-contact articles, this solution may be used on beverage containers except milk containers or equipment. (11) An aqueous solution containing equal amounts of n- alkyl (C 12 -C 18 ) benzyl dimethyl ammonium chloride and n- alkyl (C 12 -C 18 ) dimethyl ethylbenzyl ammonium chloride (having an average molecular weight of 384). In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (12) An aqueous solution containing the sodium salt of sulfonated oleic acid, polyoxyethylene-polyoxypropylene block polymers (having an average molecular weight of 2,000 and 27 to 31 moles of polyoxypropylene). In addition to use on food-processing equipment and utensils, this solution may be used on glass bottles and other glass containers intended for holding milk. All equipment, utensils, glass bottles, and other glass containers treated with this sanitizing solution shall have a drainage period of 15 minutes prior to use in contact with food. (13) An aqueous solution containing elemental iodine and alkyl (C 12 -C 15 ) monoether of mixed (ethylene-propylene) polyalkylene glycol, having a cloud-point of 70°-77 °C in 1 percent aqueous solution and an average molecular weight of 807. (14) An aqueous solution containing iodine, butoxy monoether of mixed (ethylene-propylene) polyalkylene glycol, having a cloud-point of 90°-100 °C in 0.5 percent aqueous solution and an average molecular weight of 3,300, and polyoxyethylene-polyoxypropylene block polymers (having a minimum average molecular weight of 2,000). (15) An aqueous solution containing lithium hypochlorite. (16) An aqueous solution containing equal amounts of n- alkyl (C 12 -C 18 ) benzyl dimethyl ammonium chloride and n- alkyl (C 12 -C 14 ) dimethyl ethylbenzyl ammonium chloride (having average molecular weights of 377 to 384), with the optional adjuvant substances tetrasodium ethylenediaminetetraacetate and/or alpha- ( p- nonylphenol) -omega- hydroxy poly (oxyethylene) having an average poly- (oxyethylene) content of 11 moles. Alpha-hydro-omega-hydroxypoly-(oxyethylene) poly(oxypropoylene) (15 to 18 mole minimum) poly (oxyethylene) block copolymer, having a minimum molecular weight of 1,900 (CAS Registry No. 9003-11-6) may be used in lieu of alpha- ( p -nonylphenol)-omega-hydroxy- poly(oxyethylene) having an average poly(oxyethylene) content of 11 moles. In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (17) An aqueous solution containing di- n -alkyl(C 8 -C 10 )dimethyl ammonium chlorides having average molecular weights of 332-361 and either ethyl alcohol or isopropyl alcohol. In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (18) An aqueous solution containing n- alkyl(C 12 -C 18 ) benzyldimethylammo-nium chloride, sodium metaborate, alpha- terpineol and alpha [ p- (1,1,3,3-tetramethylbutyl)phenyl] -omega- hydroxy-poly (oxyethylene) produced with one mole of the phenol and 4 to 14 moles ethylene oxide. (19) An aqueous solution containing sodium dichloroisocyanurate and tetrasodium ethylenediaminetetraacetate. In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (20) An aqueous solution containing ortho- phenylphenol, ortho- benzyl -para- chlorophenol, para-tertiaryamylphenol, sodium -alpha- alkyl(C 12 -C 15 ) -omega- hydroxypoly (oxyethylene) sulfate with the poly(oxyethylene) content averaging one mole, potassium salts of coconut oil fatty acids, and isopropyl alcohol or hexylene glycol. (21) An aqueous solution containing sodium dodecylbenzenesulfonate. In addition to use on food-processing equipment and utensils, this solution may be used on glass bottles and other glass containers intended for holding milk. (22) An aqueous solution containing (1) di- n- alkyl(C 8 -C 10 ) dimethylammonium chloride compounds having average molecular weights of 332-361, (2) n -alkyl (C 12 -C 18 ) benzyldimethylammonium chloride compounds having average molecular weights of 351-380 and consisting principally of alkyl groups with 12 to 16 carbon atoms with or without not over 1 percent each of groups with 8 and 10 carbon atoms, and (3) ethyl alcohol. The ratio of compound (1) to compound (2) is 60 to 40. (23) An aqueous solution containing n -alkyl (C 12 -C 16 ) benzyl-dimethylammonium chloride and didecyldimethylammonium chloride. (24) An aqueous solution containing elemental iodine (CAS Reg. No. 7553-56-2), alpha -[ p -(1,1,3,3-tetramethylbutyl)-phenyl]- omega- hydroxypoly-(oxyethylene) produced with one mole of the phenol and 4 to 14 moles ethylene oxide, and alpha -alkyl(C 12 -C 15 )- omega -hydroxy[poly(oxyethylene) poly(oxypropylene)] (having an average molecular weight of 965). (25) An aqueous solution containing elemental iodine (CAS Reg. No. 7553-56-2), potassium iodide (CAS Reg. No. 7681-11-0), and isopropanol (CAS Reg. No. 67-63-0). In addition to use on food processing equipment and utensils, this solution may be used on beverage containers, including milk containers and equipment and on food-contact surfaces in public eating places. (26) [Reserved] (27) An aqueous solution containing decanoic acid (CAS Reg. No. 334-48-5), octanoic acid (CAS Reg. No. 124-07-2), and sodium 1-octanesulfonate (CAS Reg. No. 5324-84-5). Additionally, the aqueous solution may contain isopropyl alcohol (CAS Reg. No. 67-63-0) as an optional ingredient. (28) An aqueous solution containing sulfonated 9-octadecenoic acid (CAS Reg. No. 68988-76-1) and sodium xylenesulfonate (CAS Reg. No. 1300-72-7). (29) An aqueous solution containing dodecyldiphenyloxidedisulfonic acid (CAS Reg. No. 30260-73-2), sulfonated tall oil fatty acid (CAS Reg. No. 68309-27-3), and neo-decanoic acid (CAS Reg. No. 26896-20-8). In addition to use on food-processing equipment and utensils, this solution may be used on glass bottles and other glass containers intended for holding milk. (30) An aqueous solution containing hydrogen peroxide (CAS Reg. No. 7722-84-1), peracetic acid (CAS Reg. No. 79-21-0), acetic acid (CAS Reg. No. 64-19-7), and 1-hydroxyethylidene-1,1-diphosphonic acid (CAS Reg. No. 2809-21-4). (31) An aqueous solution containing elemental iodine, alpha -alkyl(C 10 -C 14 )- omega -hydroxypoly(oxyethylene)poly-(oxypropylene) of average molecular weight between 768 and 837, and alpha -alkyl(C 12 -C 18 )- omega -hydroxypoly(oxyethylene) poly(oxypropylene) of average molecular weight between 950 and 1,120. In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (32) An aqueous solution containing (i) di- n -alkyl(C 8 -C 10 )dimethyl- ammonium chloride compounds having average molecular weights of 332 to 361, (ii) n -alkyl(C 12 -C 18 )benzyldimethyl- ammonium chloride compounds having average molecular weights of 351 to 380 and consisting principally of alkyl groups with 12 to 16 carbon atoms with no more than 1 percent of groups with 8 and 10, (iii) ethyl alcohol, and (iv) alpha -( p -nonylphenyl)- omega -hydroxypoly(oxyethylene) produced by the condensation of 1 mole of p -nonylphenol with 9 to 12 moles of ethylene oxide. The ratio of compound (i) to compound (ii) is 3 to 2. (33) An aqueous solution containing (i) di- n -alkyl-(C 8 -C 10 )-dimethylammonium chloride compounds having average molecular weights of 332 to 361; (ii) n -alkyl(C 12 -C 18 ) -benzyldimethylammonium chloride compounds having molecular weights of 351 to 380 and consisting principally of alkyl groups with 12 to 16 carbon atoms with no more than 1 percent of the groups with 8 to 10; and (iii) tetrasodium ethylenediamine tetraacetate. Additionally, the aqueous solution contains either alpha -( p -nonylphenyl)- omega -hydroxypoly-(oxyethylene) or alpha -alkyl(C 11 -C 15 )- omega -hydroxypoly-(oxyethylene), each produced with 9 to 13 moles of ethylene oxide. The ratio of compound (i) to compound (ii) is 3 to 2. (34) An aqueous solution of an equilibrium mixture of oxychloro species (predominantly chlorite, chlorate, and chlorine dioxide) generated either (i) by directly metering a concentrated chlorine dioxide solution, prepared just prior to use, into potable water to provide the concentration of available chlorine dioxide stated in paragraph (c)(29) of this section, or (ii) by acidification of an aqueous alkaline solution of oxychloro species (predominantly chlorite and chlorate) followed by dilution with potable water to provide the concentration of available chlorine dioxide described in paragraph (c)(29) of this section. (35) An aqueous solution containing decanoic acid (CAS Reg. No. 334-48-5), octanoic acid (CAS Reg. No. 124-07-2), lactic acid (CAS Reg. No. 050-21-5), phosphoric acid (CAS Reg. No. 7664-38-2) and a mixture of the sodium salt of naphthalenesulfonic acid (CAS Reg. No. 1321-69-3); the methyl, dimethyl, and trimethyl dervatives of the sodium salt of naphthalenesulfonic acid; and a mixture of the sodium salt of naphthalenesulfonic acid, and the methyl, dimethyl, and trimethyl derivatives of the sodium salt of naphthalenesulfonic acid alkylated at 3 percent by weight with C 6 -C 9 linear olefins, as components of a sanitizing solution to be used on food-processing equipment and utensils. The methyl and dimethyl substituted derivatives (described within this paragraph (b)(35)) constitute no less than 70 percent by weight of the mixture of naphthalenesulfonates. (36) The sanitizing solution contains decanoic acid (CAS Reg. No. 334-48-5); octanoic acid (CAS Reg. No. 124-07-2); lactic acid (CAS Reg. No. 050-21-5); phosphoric acid (CAS Reg. No. 7664-38-2); a mixture of 1-octanesulfonic acid (CAS Reg. No. 3944-72-7), and 1-octanesulfonic-2-sulfinic acid (CAS Reg. No. 113652-56-5) or 1,2-octanedisulfonic acid (CAS Reg. No. 113669-58-2); the condensate of four moles of poly(oxyethylene)poly(oxypropylene) block copolymers with one mole of ethylenediamine (CAS Reg. No. 11111-34-5); and the optional ingredient FD&C Yellow No. 5 (CAS Reg. No. 001934210). In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (37) The sanitizing solution contains sodium hypochlorite (CAS Reg. No. 7681-52-9), trisodium phosphate (CAS Reg. No. 7601-54-9), sodium lauryl sulfate (CAS Reg. No. 151-21-3), and potassium permanganate (CAS Reg. No. 7722-64-7). Magnesium oxide (CAS Reg. No. 1309-48-4) and potassium bromide (CAS Reg. No. 7758-02-3) may be added as optional ingredients to this sanitizing solution. In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (38) An aqueous solution containing hydrogen peroxide (CAS Reg. No. 7722-84-1); peroxyacetic acid (CAS Reg. No. 79-21-0); acetic acid (CAS Reg. No. 64-19-7); sulfuric acid (CAS Reg. No. 7664-93-9); and 2,6-pyridinedicarboxylic acid (CAS Reg. No. 499-83-2). In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (39) An aqueous solution containing phosphoric acid (CAS Reg. No. 7664-38-2); octenyl succinic acid (CAS Reg. No. 28805-58-5); N,N -dimethyloctanamine (CAS Reg. No. 7378-99-6); and a mixture of n -carboxylic acids (C 6 -C 12 , consisting of not less than 56 percent octanoic acid and not less than 40 percent decanoic acid). This solution may be used on food-processing equipment and utensils, including dairy-processing equipment. (40) An aqueous solution prepared by combining elemental iodine (CAS Reg. No. 7553-56-2); hydriodic acid (CAS Reg. No. 10034-85-2); sodium N -cyclohexyl- N -palmitoyl taurate (CAS Reg. No. 132-43-4); chloroacetic acid, sodium salt reaction products with 4,5-dihydro-2-undecyl-1 H -imidazole-1-ethanol and sodium hydroxide (CAS Reg. No. 68608-66-2); dodecylbenzene sulfonic acid (CAS Reg. No. 27176-87-0); phosphoric acid (CAS Reg. No. 7664-38-2); isopropyl alcohol (CAS Reg. No. 67-63-0); and calcium chloride (CAS Reg. No. 10043-52-4). In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (41) An aqueous solution containing n -alkyl(C 12 -C 16 )benzyldimethylammonium chloride, having average molecular weights ranging from 351 to 380 wherein the alkyl groups contain principally 12 to 16 carbons and not more than 1 percent each of the groups with 8 and 10 carbon atoms; ammonium chloride (CAS Reg. No. 12125-02-9); calcium stearate (CAS Reg. No. 1592-23-0); sodium bicarbonate (CAS Reg. No. 144-55-8); starch or dextrin, or both starch and dextrin (CAS Reg. No. 9004-53-9); and the optional ingredient methylene blue (CAS Reg. No. 61-73-4). In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places. (42) An aqueous solution containing decanoic acid (CAS Reg. No. 334-48-5), nonanoic acid (CAS Reg. No. 112-05-0), phosphoric acid (CAS Reg. No. 7664-38-2), propionic acid (CAS Reg No. 79-09-04), and sodium 1-octanesulfonate (CAS Reg. No. 5324-84-5). Sulfuric acid (CAS Reg. No. 7664-93-9) may be added as an optional ingredient. In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (43) An aqueous solution of iodine and hypochlorous acid generated by the dilution of an aqueous acidic (21.5 percent nitric acid) solution of iodine monochloride. In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (44) An aqueous solution of citric acid, disodium ethylenediaminetetraacetate, sodium lauryl sulfate, and monosodium phosphate. In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (45) An aqueous solution of hydrogen peroxide, acetic acid, peroxyacetic acid, octanoic acid, peroxyoctanoic acid, sodium 1-octanesulfonate, and 1-hydroxyethylidene-1,1-diphosphonic acid. In addition to use on food-processing equipment and utensils, this solution may be used on food-contact surfaces in public eating places, subject to the limitations in paragraph (c)(39) of this section. (46) An aqueous solution of chlorine dioxide and related oxychloro species generated by acidification of an aqueous solution of sodium chlorite with a solution of sodium gluconate, citric acid, phosphoric acid, and sodium mono- and didodecylphenoxybenzenedisulfonate. In addition to use on food-processing equipment and utensils, this solution may be used on dairy-processing equipment. (c) The solutions identified in paragraph (b) of this section will not exceed the following concentrations: (1) Solutions identified in paragraph (b)(1) of this section will provide not more than 200 parts per million of available halogen determined as available chlorine. (2) Solutions identified in paragraph (b)(2) of this section will provide not more than 100 parts per million of available halogen determined as available chlorine. (3) Solution identified in paragraph (b)(3) of this section will provide not more than 25 parts per million of titratable iodine. The solutions will contain the components potassium iodide, sodium p- toluenesulfonchloramide and sodium lauryl sulfate at a level not in excess of the minimum required to produce their intended functional effect. (4) Solutions identified in paragraph (b)(4), (5), (6), (8), (13), and (14) of this section will contain iodine to provide not more than 25 parts per million of titratable iodine. The adjuvants used with the iodine will not be in excess of the minimum amounts required to accomplish the intended technical effect. (5) Solutions identified in paragraph (b)(7) of this section will provide not more than 400 parts per million dodecylbenzenesulfonic acid and not more than 80 parts per million of polyoxyethylene-polyoxypropylene block polymers (having a minimum average molecular weight of 2,800) or not more than 40 parts per million of isopropyl alcohol. (6) Solutions identified in paragraph (b)(9) of this section shall provide when ready to use no more than 200 parts per million of the active quaternary compound. (7) Solutions identified in paragraph (b)(10) of this section shall provide not more than sufficient trichloromelamine to produce 200 parts per million of available chlorine and either sodium lauryl sulfate at a level not in excess of the minimum required to produce its intended functional effect or not more than 400 parts per million of dodecylbenzenesulfonic acid. (8) Solutions identified in paragraph (b)(11) of this section shall provide, when ready to use, not more than 200 parts per million of active quaternary compound. (9) The solution identified in paragraph (b)(12) of this section shall provide not more than 200 parts per million of sulfonated oleic acid, sodium salt. (10) Solutions identified in paragraph (b)(15) of this section will provide not more than 200 parts per million of available chlorine and not more than 30 ppm lithium. (11) Solutions identified in paragraph (b)(16) of this section shall provide not more than 200 parts per million of active quaternary compound. (12) Solutions identified in paragraph (b)(17) of this section shall provide, when ready to use, a level of 150 parts per million of the active quaternary compound. (13) Solutions identified in paragraph (b)(18) of this section shall provide not more than 200 parts per million of active quaternary compound and not more than 66 parts per million of alpha [ p- (1,1,3,3-tetramethylbutyl) phenyl] -omega- hydroxypoly (oxyethylene). (14) Solutions identified in paragraph (b)(19) of this section shall provide, when ready to use, a level of 100 parts per million of available chlorine. (15) Solutions identified in paragraph (b)(20) of this section are for single use applications only and shall provide, when ready to use, a level of 800 parts per million of total active phenols consisting of 400 parts per million ortho- phenylphenol, 320 parts per million ortho- benzyl -para- chlorophenol and 80 parts per million para- tertiaryamylphenol. (16) Solution identified in paragraph (b)(21) of this section shall provide not more than 430 parts per million and not less than 25 parts per million of sodium dodecylbenzenesulfonate. (17) Solutions identified in paragraph (b)(22) of this section shall provide, when ready to use, at least 150 parts per million and not more than 400 parts per million of active quaternary compound. (18) Solutions identified in paragraph (b)(23) of this section shall provide at least 150 parts per million and not more than 200 parts per million of the active quaternary compound. (19) Solutions identified in paragraphs (b)(24), (b)(25), and (b)(43) of this section shall provide at least 12.5 parts per million and not more than 25 parts per million of titratable iodine. The adjuvants used with the iodine shall not be in excess of the minimum amounts required to accomplish the intended technical effect. (20)-(21) [Reserved] (22) Solutions identified in paragraph (b)(27) of this section shall provide, when ready to use, at least 109 parts per million and not more than 218 parts per million of total active fatty acids and at least 156 parts per million and not more than 312 parts per million of the sodium 1-octanesulfonate. (23) Solutions identified in paragraph (b)(28) of this section shall provide, when ready to use, at least 156 parts per million and not more than 312 parts per million of sulfonated 9-octadecenoic acid, at least 31 parts per million and not more then 62 parts per million of sodium xylenesulfonate. (24) Solutions identified in paragraph (b)(29) of this section will provide at least 237 parts per million and not more than 474 parts per million dodecyldiphenyloxidedisulfonic acid, at least 33 parts per million and not more than 66 parts per million sulfonated tall oil fatty acid, and at least 87 parts per million and not more than 174 parts per million neo-decanoic acid. (25) Solutions identified in paragraph (b)(30) of this section shall provide, when ready to use, not less than 550 parts per million and not more than 1,100 parts per million hydrogen peroxide, not less than 100 parts per million and not more than 200 parts per million peracetic acid, not less than 150 parts per million and not more than 300 parts per million acetic acid, and not less than 15 parts per million and not more than 30 parts per million 1-hydroxyethylidene-1,1-diphosphonic acid. (26) The solution identified in paragraph (b)(31) of this section shall provide, when ready to use, at least 12.5 parts per million and not more than 25 parts per million of titratable iodine. The adjuvants used with the iodine will not be in excess of the minimum amounts required to accomplish the intended technical effect. (27) Solutions identified in paragraph (b)(32) of this section shall provide, when ready to use, at least 150 parts per million and no more than 400 parts per million of active quarternary compounds in solutions containing no more than 600 parts per million water hardness. The adjuvants used with the quarternary compounds will not exceed the amounts required to accomplish the intended technical effect. (28) Solutions identified in paragraph (b)(33) of this section shall provide, when ready to use, at least 150 parts per million and not more than 400 parts per million of active quaternary compounds. The adjuvants used with the quaternary compounds shall not exceed the amounts required to accomplish the intended technical effect. Tetrasodium ethylenediamine tetraacetate shall be added at a minimum level of 60 parts per million. Use of these sanitizing solutions shall be limited to conditions of water hardness not in excess of 300 parts per million. (29) Solutions identified in paragraph (b)(34) of this section should provide, when ready to use, at least 100 parts per million and not more than 200 parts per million available chlorine dioxide as determined by the method titled “Iodometric Method for the Determination of Available Chlorine Dioxide (50-250 ppm available ClO 2 ),” which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (30) Solutions identified in paragraph (b)(35) of this section shall provide, when ready for use, at least 117 parts per million and not more than 234 parts per million of total fatty acids and at least 166 parts per million and not more than 332 parts per million of a mixture of naphthalenesulfonates. The adjuvants phosphoric acid and lactic acid, used with decanoic acid, octanoic acid, and sodium naphthalenesulfonate and its alkylated derivatives, will not be in excess of the minimum amounts required to accomplish the intended technical effects. (31) Solutions identified in paragraph (b)(36) of this section shall provide, when ready for use, at least 29 parts per million and not more than 58 parts per million decanoic acid; at least 88 parts per million and not more than 176 parts per million of octanoic acid; at least 69 parts per million and not more than 138 parts per million of lactic acid; at least 256 parts per million and not more than 512 parts per million of phosphoric acid; at least 86 parts per million and not more than 172 parts per million of 1-octanesulfonic acid; at least 51 parts per million and not more than 102 parts per million of 1-octanesulfonic-2-sulfinic acid or 1,2-octanedisulfonic acid; and at least 10 parts per million and not more than 20 parts per million of the condensate of four moles of poly(oxyethylene)poly(oxypropylene) block copolymers with one mole of ethylenediamine. The colorant adjuvant FD&C Yellow No. 5 shall not be used in excess of the minimum amount required to accomplish the intended technical effect. (32)(i) The solution identified in paragraph (b)(37) of this section without potassium bromide shall provide, when ready to use, at least 100 parts per million and not more than 200 parts per million of available halogen determined as available chlorine; at least 2,958 parts per million and not more than 5,916 parts per million of trisodium phosphate; at least 1 part per million and not more than 3 parts per million of sodium lauryl sulfate; and at least 0.3 part per million and not more than 0.7 part per million on potassium permanganate. (ii) The solution identified in paragraph (b)(37) of this section with potassium bromide shall provide, when ready to use, at least 25 parts per million and not more than 200 parts per million of available halogen determined as available chlorine; at least 15 parts per million and not more than 46 parts per million of potassium bromide; at least 690 parts per million and not more than 2,072 parts per million of trisodium phosphate; at least 0.3 part per million and not more than 1 part per million of sodium lauryl sulfate; and at least 0.1 part per million and not more than 0.3 part per million of potassium permanganate. (iii) Magnesium oxide when used in paragraph (c)(32)(i) or (ii) of this section shall not be used in excess of the minimum amount required to accomplish its intended technical effect. (33) Solutions identified in paragraph (b)(38) of this section shall provide when ready for use not less than 300 parts per million and not more than 465 parts per million of hydrogen peroxide; not less than 200 parts per million and not more than 315 parts per million of peroxyacetic acid; not less than 200 parts per million and not more than 340 parts per million of acetic acid; not less than 10 parts per million and not more than 20 parts per million of sulfuric acid; and not less than 0.75 parts per million and not more than 1.2 parts per million of 2,6-pyridinedicarboxylic acid. (34) Solutions identified in paragraph (b)(39) of this section shall provide when ready for use not less than 460 parts per million and not more than 625 parts per million of phosphoric acid, and all components shall be present in the following proportions: 1 part phosphoric acid to 0.25 octenyl succinic acid to 0.18 part N,N -dimethyloctanamine to 0.062 part of a mixture of n -carboxylic acids (C 6 -C 12 , consisting of not less than 56 percent octanoic acid and not less than 40 percent decanoic acid). (35) Solutions identified in paragraph (b)(40) of this section shall provide when ready for use not less than 12.5 parts per million and not more than 25.0 parts per million of titratable iodine; and not less than 2.7 parts per million and not more than 5.5 parts per million of dodecylbenzene sulfonic acid. All components shall be present in the following proportions: 1.0 part dodecylbenzene sulfonic acid to 43 parts sodium N -cyclohexyl- N -palmitoyl taurate to 7.7 parts chloroacetic acid, sodium salt, reaction products with 4,5-dihydro-2-undecyl-1 H -imidazole-1-ethanol and sodium hydroxide to 114 parts phosphoric acid to 57 parts isopropyl alcohol to 3.0 parts calcium chloride. (36) Solutions identified in paragraph (b)(41) of this section shall provide, when ready for use, not less than 150 parts per million and not more than 200 parts per million of n -alkyl(C 12 -C 16 )benzyldimethylammonium chloride; and not more than 0.4 part per million of the colorant methylene blue. Components shall be present in the product used to prepare the solution in the following proportions: 1 part n -alkyl(C 12 -C 16 )benzyldimethylammonium chloride to 0.24 part ammonium chloride to 0.08 part calcium stearate to 0.60 part sodium bicarbonate to 0.08 part starch or dextrin, or a combination of starch and dextrin. (37)(i) The solution identified in paragraph (b)(42) of this section not containing sulfuric acid shall provide when ready for use not less than 45 parts per million and not more than 90 parts per million of decanoic acid; and all components shall be present in the following proportions (weight/weight (w/w)): 1 part decanoic acid to 1 part nonanoic acid to 9.5 parts phosphoric acid to 3.3 parts propionic acid to 3.3 parts sodium 1-octanesulfonate. (ii) The solution identified in paragraph (b)(42) of this section containing sulfuric acid shall provide when ready for use not less than 45 parts per million and not more than 90 parts per million of decanoic acid; and all components shall be present in the following proportions (w/w): 1 part decanoic acid to 1 part nonanoic acid to 2.8 parts phosphoric acid to 3.3 parts propionic acid to 3.3 parts sodium 1-octanesulfonate to 3.2 parts sulfuric acid. (38) The solution identified in paragraph (b)(44) of this section shall provide, when ready for use, at least 16,450 parts per million and not more than 32,900 parts per million of citric acid; at least 700 parts per million and not more than 1,400 parts per million of disodium ethylenediaminetetraacetate; at least 175 parts per million and not more than 350 parts per million of sodium lauryl sulfate; and at least 175 parts per million and not more than 350 parts per million of monosodium phosphate. (39)(i) The solution identified in paragraph (b)(45) of this section, when used on food processing equipment and utensils, including dairy and beverage-processing equipment but excluding food-contact surfaces in public eating places and dairy and beverage containers, shall provide when ready for use at least 72 parts per million and not more than 216 parts per million of hydrogen peroxide; at least 46 parts per million and not more than 138 parts per million of peroxyacetic acid; at least 40 parts per million and not more than 122 parts per million of octanoic acid (including peroxyoctanoic acid); at least 281 parts per million and not more than 686 parts per million of acetic acid; at least 7 parts per million and not more than 34 parts per million of 1-hydroxyethylidene-1,1-diphosphonic acid; and at least 36 parts per million and not more than 109 parts per million of sodium 1-octanesulfonate. (ii) The solution identified in paragraph (b)(45) of this section, when used on food-contact equipment and utensils in warewashing machines, including warewashing machines in public eating places, at temperatures no less than 120 °F (49 °C) shall provide when ready for use at least 30 parts per million and not more than 91 parts per million of hydrogen peroxide; at least 19 parts per million and not more than 58 parts per million of peroxyacetic acid; at least 17 parts per million and not more than 52 parts per million of octanoic acid (including peroxyoctanoic acid); at least 119 parts per million and not more than 290 parts per million of acetic acid; at least 3 parts per million and not more than 14 parts per million of 1-hydroxyethylidene-1,1-diphosphonic acid; and at least 15 parts per million and not more than 46 parts per million of sodium 1-octanesulfonate. (iii) The solution identified in paragraph (b)(45) of this section, when used on dairy or beverage containers, shall provide when ready for use at least 36 parts per million and not more than 108 parts per million of hydrogen peroxide; at least 23 parts per million and not more than 69 parts per million of peroxyacetic acid; at least 20 parts per million and not more than 61 parts per million of octanoic acid (including peroxyoctanoic acid); at least 140 parts per million and not more than 343 parts per million of acetic acid; at least 3 parts per million and not more than 17 parts per million of 1-hydroxyethylidene-1,1-diphosphonic acid; and at least 18 parts per million and not more than 55 parts per million of sodium 1-octanesulfonate. (40) The solution identified in paragraph (b)(46) of this section shall provide, when ready for use, at least 100 parts per million and not more than 200 parts per million of chlorine dioxide as determined by the method developed by Bio-cide International, Inc., entitled, “Iodometric Method for the Determination of Available Chlorine Dioxide (50-250 ppm Available ClO 2 ),” dated June 11, 1987, which is incorporated by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of this method are available from the Office of Food Additive Safety (HFS-200), Center for Food Safety and Applied Nutrition, Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, 240-402-1200, and may be examined at the Food and Drug Administration's Main Library, 10903 New Hampshire Ave., Bldg. 2, Third Floor, Silver Spring, MD 20993, 301-796-2039, or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html ; at least 380 parts per million and not more than 760 parts per million of sodium gluconate; and at least 960 parts per million and not more than 1,920 parts per million of sodium mono- and didodecylphenoxybenzenedisulfonate. Other components listed under paragraph (b)(46) of this section shall be used in the minimum amount necessary to produce the intended effect. (d) Sanitizing agents for use in accordance with this section will bear labeling meeting the requirements of the Federal Insecticide, Fungicide, and Rodenticide Act." 21:21:3.0.1.1.9.3.1.1,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",C,Subpart C—Antioxidants and Stabilizers,,§ 178.2010 Antioxidants and/or stabilizers for polymers.,FDA,,,"[42 FR 14609, Mar. 15, 1977]","The substances listed in paragraph (b) of this section may be safely used as antioxidants and/or stabilizers in polymers used in the manufacture of articles or components of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section: (a) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect. (b) List of substances: 1 Copies are available from the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pa. 19103." 21:21:3.0.1.1.9.3.1.2,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",C,Subpart C—Antioxidants and Stabilizers,,"§ 178.2550 4-Hydroxymethyl-2,6-di-",FDA,,,,"4-Hydroxymethyl-2,6-di -tert- butyl-phenol may be safely used as an antioxidant in articles intended for use in contact with food, in accordance with the following prescribed conditions: (a) The additive has a solidification point of 140°-141 °C. (b) The concentration of the additive and any other permitted antioxidants in the finished food-contact article does not exceed a total of 0.5 milligram per square inch of food-contact surface." 21:21:3.0.1.1.9.3.1.3,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",C,Subpart C—Antioxidants and Stabilizers,,§ 178.2650 Organotin stabilizers in vinyl chloride plastics.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11847, Mar. 19, 1982; 48 FR 7170, Feb. 18, 1983; 48 FR 42972, Sept. 21, 1983; 48 FR 51612, Nov. 10, 1983; 49 FR 8432, Mar. 7, 1984; 50 FR 62, Jan. 2, 1985; 50 FR 3510, Jan. 25, 1985; 50 FR 37998, Sept. 19, 1985; 50 FR 47212, Nov. 15, 1985; 54 FR 24898, June 12, 1989]","The organotin chemicals identified in paragraph (a) of this section may be safety used alone or in combination, at levels not to exceed a total of 3 parts per hundred of resin, as stabilizers in vinyl chloride homopolymers and copolymers complying with the provisions of § 177.1950 or § 177.1980 of this chapter and that are identified for use in contact with food of types I, II, III, IV (except liquid milk), V, VI (except malt beverages and carbonated nonalcoholic beverages), VII, VIII, and IX described in table 1 of § 176.170(c) of this chapter, except for the organotin chemical identified in paragraph (a)(3) of this section, which may be used in contact with food of types I through IX at temperatures not exceeding 75 °C (167 °F), and further that the organotin chemicals identified in paragraphs (a)(5) and (6) of this section may be used in contact with food of types I through IX at temperatures not exceeding 66 °C (150 °F), conditions of use D through G described in table 2 of § 176.170(c) of this chapter, and further that dodecyltin chemicals identified in paragraph (a)(7) of this section which may be used in contact with food of types I, II, III, IV (except liquid milk), V, VI (except malt beverages and carbonated nonalcoholic beverages), VII, VIII, and IX described in table 1 of § 176.170(c) of this chapter at temperatures not exceeding 71 °C (160 °F), in accordance with the following prescribed conditions: (a) For the purpose of this section, the organotin chemicals are those listed in paragraphs (a)(1), (2), (3), (4), (5), (6), and (7) of this section. (1) Di( n -octyl)tin S,S′-bis(isooctylmercaptoacetate) is an octyltin chemical having 15.1 to 16.4 percent by weight of tin (Sn) and having 8.1 to 8.9 percent by weight of mercapto sulfur. It is made from di( n -octyl)tin dichloride or di( n -octyl)tin oxide. The isooctyl radical in the mercaptoacetate is derived from oxo process isooctyl alcohol. Di( n -octyl)tin dichloride has an organotin composition that is not less than 95 percent by weight of di( n -octyl)tin dichloride and not more than 5 percent by weight of tri( n -octyl)tin chloride. Di( n -octyl)tin oxide has an organotin composition that is not less than 95 percent by weight of di( n -octyl)tin oxide and not more than 5 percent by weight of bis[tri( n -octyl)tin] oxide, and/or mono n -octyltin oxide. (2) Di( n- octyl) tin maleate polymer is an octyltin chemical having the formula [(C 8 H 17 ) 2 SnC 4 H 2 O 4 ] n (where n is between 2 and 4 inclusive), having 25.2 to 26.6 percent by weight of tin (Sn) and having a saponification number of 225 to 255. It is made from di( n- octyl)tin dichloride or di( n- octyl)tin oxide meeting the specifications prescribed for di( n- octyl) tin dichloride or di( n- octyl) tin oxide in paragraph (a)(1) of this section. (3) C 10-16 -Alkyl mercaptoacetates reaction products with dichlorodioctylstannane and trichlorooctylstannane (CAS Reg. No. 83447-69-2) is an organotin chemical mixture having 10.8 to 11.8 percent by weight of tin (Sn) and having 8.0 to 8.6 percent by weight of mercapto sulfur. It is made from a mixture of di( n -octyl)tin dichloride and ( n -octyl)tin trichloride which has an organotin composition that is not less than 95 percent by weight di( n -octyl)tin dichloride/( n -octyl)tin trichloride, and not more than 1.5 percent by weight of tri( n -octyl)tin chloride. The alkyl radical in the mercaptoacetate is derived from a mixture of saturated n -alcohols which has a composition that is not less than 50 percent by weight tetradecyl alcohol, and that is not more than 50 percent by weight total of decyl alcohol and/or dodecyl alcohol, and/or hexadecyl alcohol. (4) ( n -Octyl)tin S,S′S″ tris(isooctyl-mercaptoacetate) is an octyltin chemical having the formula n -C 8 H 17 Sn(SCH 2 CO 2 C 8 H 17 ) 3 (CAS Reg. No. 26401-86-5) having 13.4 to 14.8 percent by weight of tin (Sn) and having 10.9 to 11.9 percent by weight of mercapto sulfur. It is made from ( n -octyl)tin trichloride. The isooctyl radical in the mercaptoacetate is derived from oxo process isooctyl alcohol. The ( n -octyl)tin trichloride has an organotin composition that is not less than 95 percent by weight of ( n -octyl)tin trichloride and not more than 5 percent by weight of tri( n -octyl)tin chloride. (5) Bis( beta -carbobutoxyethyl)tin bis(isooctylmercaptoacetate) (CAS Reg. No. 63397-60-4) is an estertin chemical having 14.0 to 15.0 percent by weight of tin (Sn) and having 7.5 to 8.5 percent by weight of mercapto sulfur. It is made from bis( beta -carbobutoxyethyl)tin dichloride. The isooctyl radical in the mercaptoacetate is derived from oxo process primary octyl alcohols. The bis( beta -carbobutoxyethyl)tin dichloride has an organotin composition that is not less than 95 percent by weight of bis( beta -carbobutoxyethyl)tin dichloride and not more than 5 percent by weight of bis( beta -carbobutoxyethyltin trichloride. The triestertin chloride content of bis( beta -carbobutoxyethyltin) dichloride shall not exceed 0.02 percent. p (6) Beta -carbobutoxyethyltin tris(isooctylmercaptoacetate) (CAS Reg. No. 63438-80-2) is an estertin chemical having 13.0 to 14.0 percent by weight of tin (Sn) and having 10.5 to 11.5 percent by weight of mercapto sulfur. It is made from beta -carbobutoxyethyltin trichloride. The isooctyl radical in the mercaptoacetate is derived from oxo process primary octyl alcohol. The beta -carbobutoxyethyltin trichloride has an organotin composition that is not less than 95 percent by weight of beta- carbobutoxyethyltin trichloride and not more than 5 percent total of triestertin chloride and diestertin chloride. (7) The dodecyltin stabilizer is a mixture of 50 to 60 percent by weight of n -dodecyltin S,S′,S″-tris(isooctylmercaptoacetate) (CAS Reg. No. 67649-65-4) and 40 to 50 percent by weight of di( n -dodecyl)tin S,S′-di(isooctylmercaptoacetate) (CAS Reg. No. 84030-61-5) having 13 to 14 percent by weight of tin (Sn) and having 8 to 9 percent by weight of mercapto sulfur. It is made from a mixture of dodecyltin trichloride and di(dodecyl)tin dichloride which has not more than 0.2 percent by weight of dodecyltin trichloride, not more than 2 percent by weight of dodecylbutyltin dichloride and not more than 3 percent by weight of tri(dodecyl)tin chloride. The isooctyl radical in the mercaptoacetate is derived from oxo process primary octyl alcohols. (b) The vinyl chloride plastic containers, film or panels in the finished form in which they are to contact food, shall meet the following limitations: (1) The finished plastics intended for contact with foods of the types listed in this section shall be extracted with the solvent or solvents characterizing those types of foods as determined from table 2 of § 176.170(c) of this chapter at the temperature reflecting the conditions of intended use as determined therein. Additionally, extraction tests for acidic foods shall be included and simulated by 3-percent acetic acid at temperatures specified for water in table 2 of § 176.170(c) of this chapter. The extraction tests shall cover at least three equilibrium periodic determinations, as follows: (i) The exposure time for the first determination shall be at least 72 hours for aqueous solvents, and at least 6 hours for heptane. (ii) Subsequent determinations shall be at a minimum of 24-hour intervals for aqueous solvents, and 2-hour intervals for heptane. These tests shall yield total octylin stabilizers not to exceed 0.5 parts per million as determined by analytical method entitled “Atomic Absorption Spectrometric Determination of Sub-part-per-Million Quantities of Tin in Extracts and Biological Materials with Graphite Furnace,” Analytical Chemistry, Vol. 49, p. 1090-1093 (1977), which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (iii) Subsequent determinations for the dodecyltin mixture described in paragraph (a)(7) of this section shall be at a minimum of 24-hour intervals for aqueous solvents and 2-hour intervals for heptane. These tests shall yield di( n -octyl)tin S,S′-bis(isooctylmercaptoacetate), or di( n -octyl)tin maleate polymer, or (C 10 -C 16 )-alkylmercaptoacetate reaction products with dichlorodioctylstannane and trichlorooctylstannane, or n -octyltin S,S′,S″-tris(isooctylmercaptoacetate), tris(isooctylmercaptoacetate) and di( n -dodecyl)tin bis(isooctylmercaptoacetate) or any combination thereof, not to exceed 0.5 parts per million as determined by an analytical method entitled “Atomic Absorption Spectrophotometric Determination of Sub-part-per-Million Quantities of Tin in Extracts and Biological Materials with Graphite Furnace,” Analytical Chemistry, Vol. 49, pp. 1090-1093 (1977), which is incorporated by reference in accordance with 5 U.S.C. 552(a). The availability of this incorporation by reference is given in paragraph (b)(1)(ii) of this section. (2) In lieu of the tests prescribed in paragraph (b)(1) of this section, the finished plastics intended for contact with foods only of Types II, V, VI-A (except malt beverages), and VI-C may be end-tested with food-simulating solvents, under conditions of time and temperature, as specified below, whereby such tests shall yield the octyltin residues cited in paragraph (b)(1) of this section not in excess of 0.5 ppm:" 21:21:3.0.1.1.9.4.1.1,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3010 Adjuvant substances used in the manufacture of foamed plastics.,FDA,,,"[47 FR 22090, May 21, 1982, as amended at 58 FR 64895, Dec. 10, 1993]","The following substances may be safely used as adjuvants in the manufacture of foamed plastics intended for use in contact with food, subject to any prescribed limitations:" 21:21:3.0.1.1.9.4.1.10,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3400 Emulsifiers and/or surface-active agents.,FDA,,,"[42 FR 14609, Mar. 15, 1977]","The substances listed in paragraph (c) of this section may be safely used as emulsifiers and/or surface-active agents in the manufacture of articles or components of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section. (a) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect; and the quantity that may become a component of food as a result of such use shall not be intended to, nor in fact, accomplish any physical or technical effect in the food itself. (b) The use as an emulsifier and/or surface-active agent in any substance or article that is the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter conforms with any specifications and limitations prescribed by such regulation for the finished form of the substance or article. (c) List of substances: (d) The provisions of this section are not applicable to emulsifiers and/or surface-active agents listed in § 175.105(c)(5) of this chapter and used in food-packaging adhesives complying with § 175.105 of this chapter." 21:21:3.0.1.1.9.4.1.11,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3450 Esters of stearic and palmitic acids.,FDA,,,,"The ester stearyl palmitate or palmityl stearate or mixtures thereof may be safely used as adjuvants in food-packaging materials when used in accordance with the following prescribed conditions: (a) They are used or intended for use as plasticizers or lubricants in polystyrene intended for use in contact with food. (b) They are added to the formulated polymer prior to extrusion. (c) The quantity used shall not exceed that required to accomplish the intended technical effect." 21:21:3.0.1.1.9.4.1.12,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3480 Fatty alcohols, synthetic.",FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11847, Mar. 19, 1982; 54 FR 24898, June 12, 1989]","Synthetic fatty alcohols may be safely used as components of articles intended for use in contact with food, and in synthesizing food additives and other substances permitted for use as components of articles intended for use in contact with food in accordance with the following prescribed conditions: (a) The food additive consists of fatty alcohols meeting the specifications and definition prescribed in § 172.864 of this chapter, except as provided in paragraph (c) of this section. (b) It is used or intended for use as follows: (1) As substitutes for the corresponding naturally derived fatty alcohols permitted for use as components of articles intended for use in contact with food by existing regulations in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter: Provided, That the use is in compliance with any prescribed limitations. (2) As substitutes for the corresponding naturally derived fatty alcohols used as intermediates in the synthesis of food additives and other substances permitted for use as components of food-contact articles. (c) Synthetic fatty alcohols identified in paragraph (c)(1) of this section may contain not more than 0.8 weight percent of total diols as determined by a method titled “Diols in Monohydroxy Alcohol by Miniature Thin Layer Chromatography (MTLC),” which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (1) Synthetic fatty alcohols. (i) Hexyl, octyl, decyl, lauryl, myristyl, cetyl, and stearyl alcohols meeting the specifications and definition prescribed in § 172.864 of this chapter, except that they may contain not more than 0.8 weight percent total diols. (ii) Lauryl, myristyl, cetyl, and stearyl alcohols manufactured by the process described in § 172.864(a)(2) of this chapter such that lauryl and myristyl alcohols meet the specifications in § 172.864(a)(1)(i) of this chapter, and cetyl and stearyl alcohols meet the specifications in § 172.864(a)(1)(ii) of this chapter. (2) Conditions of use. (i) Synthetic fatty alcohols as substitutes for the corresponding naturally derived fatty alcohols permitted for use in compliance with § 178.3910. (ii) Synthetic lauryl alcohol as a substitute for the naturally derived lauryl alcohol permitted as an intermediate in the synthesis of sodium lauryl sulfate used in compliance with § 178.3400." 21:21:3.0.1.1.9.4.1.13,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3500 Glycerin, synthetic.",FDA,,,,"Synthetic glycerin may be safely used as a component of articles intended for use in packaging materials for food, subject to the provisions of this section: (a) It is produced by the hydrogenolysis of carbohydrates, and shall contain not in excess of 0.2 percent by weight of a mixture of butanetriols. (b) It is used in a quantity not to exceed that amount reasonably required to produce its intended physical or technical effect, and in accordance with any limitations prescribed by applicable regulations in parts 174, 175, 176, 177, 178 and 179 of this chapter. It shall not be intended to, nor in fact accomplish, any direct physical or technical effect in the food itself." 21:21:3.0.1.1.9.4.1.14,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3505 Glyceryl tri-(12-acetoxystearate).,FDA,,,"[50 FR 1503, Jan. 11, 1985]","Glyceryl tri-(12-acetoxystearate) (CAS Reg. No. 139-43-5) may be safely used as a component of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section. (a) The additive is applied to the surface of calcium carbonate at a level not to exceed 1 weight-percent of the total mixture. (b) The calcium carbonate/glyceryl tri-(12-acetoxystearate) mixture is used as an adjuvant in polymers in contact with nonfatty foods at a level not to exceed 20 weight-percent of the polymer." 21:21:3.0.1.1.9.4.1.15,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3520 Industrial starch-modified.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 42 FR 49453, Sept. 27, 1977]","Industrial starch-modified may be safely used as a component of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section. (a) Industrial starch-modified is identified as follows: (1) A food starch-modified or starch or any combination thereof that has been modified by treatment with one of the reactants hereinafter specified, in an amount reasonably required to achieve the desired functional effect but in no event in excess of any limitation prescribed, with or without subsequent treatment as authorized in § 172.892 of this chapter. (2) A starch irradiated under one of the following conditions to produce free radicals for subsequent graft polymerization with the reactants listed in this paragraph (a)(2): (i) Radiation from a sealed cobalt 60 source, maximum absorbed dose not to exceed 5.0 megarads. (ii) An electron beam source at a maximum energy of 7 million electron volts of ionizing radiation, maximum absorbed dose not to exceed 5.0 megarads. (b) The following adjuvants may be used as surface-active agents in the processing of industrial starch-modified: Polyethylene glycol (400) dilaurate. Polyethylene glycol (400) monolaurate. Polyoxyethylene (4) lauryl ether. Polyethylene glycol (400) dilaurate. Polyethylene glycol (400) monolaurate. Polyoxyethylene (4) lauryl ether. (c) To insure safe use of the industrial starch-modified, the label of the food additive container shall bear the name of the additive “industrial starch-modified,” and in the instance of an industrial starch-modified which is limited with respect to conditions of use, the label of the food additive container shall contain a statement of such limited use." 21:21:3.0.1.1.9.4.1.16,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3530 Isoparaffinic petroleum hydrocarbons, synthetic.",FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11847, Mar. 19, 1982; 49 FR 10112, Mar. 19, 1984]","Isoparaffinic petroleum hydrocarbons, synthetic, may be safely used in the production of nonfood articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section. (a) The isoparaffinic petroleum hydrocarbons, produced by synthesis from petroleum gases consist of a mixture of liquid hydrocarbons meeting the following specifications: Boiling point 63°-260 °C, as determined by ASTM method D86-82, “Standard Method for Distillation of Petroleum Products,” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Ultraviolet absorbance: 260-319 millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residue 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum hydrocarbons containing antioxidants shall meet the specified ultraviolet absorbance limits after correction for any absorbance due to the antioxidants. The ultraviolet absorbance shall be determined by the procedure described for application to mineral oil under “Specifications” on page 66 of the “Journal of the Association of Official Agricultural Chemists,” Vol. 45 (February 1962), which is incorporated by reference, disregarding the last sentence of that procedure. For hydrocarbons boiling below 121 °C, the nonvolatile residue shall be determined by ASTM method D1353-78, “Standard Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Related Products;” for those boiling above 121 °C, ASTM procedure D381-80, “Standard Test Method for Existent Gum in Fuels by Jet Evaporation,” which are incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Boiling point 63°-260 °C, as determined by ASTM method D86-82, “Standard Method for Distillation of Petroleum Products,” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Ultraviolet absorbance: Nonvolatile residue 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum hydrocarbons containing antioxidants shall meet the specified ultraviolet absorbance limits after correction for any absorbance due to the antioxidants. The ultraviolet absorbance shall be determined by the procedure described for application to mineral oil under “Specifications” on page 66 of the “Journal of the Association of Official Agricultural Chemists,” Vol. 45 (February 1962), which is incorporated by reference, disregarding the last sentence of that procedure. For hydrocarbons boiling below 121 °C, the nonvolatile residue shall be determined by ASTM method D1353-78, “Standard Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Related Products;” for those boiling above 121 °C, ASTM procedure D381-80, “Standard Test Method for Existent Gum in Fuels by Jet Evaporation,” which are incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (b) Isoparaffinic petroleum hydrocarbons may contain antioxidants authorized for use in food in an amount not to exceed that reasonably required to accomplish the intended technical effect. (c) Isoparaffinic petroleum hydrocarbons are used in the production of nonfood articles. The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect, and the residual remaining in the finished article shall be the minimum amount reasonably attainable." 21:21:3.0.1.1.9.4.1.17,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3570 Lubricants with incidental food contact.,FDA,,,"[42 FR 14609, Mar. 15, 1977]","Lubricants with incidental food contact may be safely used on machinery used for producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section: (a) The lubricants are prepared from one or more of the following substances: (1) Substances generally recognized as safe for use in food. (2) Substances used in accordance with the provisions of a prior sanction or approval. (3) Substances identified in this paragraph (a)(3). (b) The lubricants are used on food-processing equipment as a protective antirust film, as a release agent on gaskets or seals of tank closures, and as a lubricant for machine parts and equipment in locations in which there is exposure of the lubricated part to food. The amount used is the minimum required to accomplish the desired technical effect on the equipment, and the addition to food of any constituent identified in this section does not exceed the limitations prescribed. (c) Any substance employed in the production of the lubricants described in this section that is the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter conforms with any specification in such regulation." 21:21:3.0.1.1.9.4.1.18,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3600 Methyl glucoside-coconut oil ester.,FDA,,,,"Methyl glucoside-coconut oil ester identified in § 172.816(a) of this chapter may be safely used as a processing aid (filter aid) in the manufacture of starch, including industrial starch-modified complying with § 178.3520, intended for use as a component of articles that contact food." 21:21:3.0.1.1.9.4.1.19,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3610 α-Methylstyrene-vinyltoluene resins, hydrogenated.",FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11847, Mar. 19, 1982; 54 FR 24898, June 12, 1989]","Hydrogenated α-methylstyrene-vinyltoluene copolymer resins having a molar ratio of 1 α-methylstyrene to 3 vinyltoluene may be safely used as components of polyolefin film intended for use in contact with food, subject to the following provisions: (a) Hydrogenated α-methylstyrene-vinyltoluene copolymer resins have a drop-softening point of 125° to 165 °C and a maximum absorptivity of 0.17 liter per gram centimeter at 266 nanometers, as determined by methods titled “Determination of Softening Point (Drop Method)” and “Determination of Unsaturation of Resin 1977,” which are incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (b) The polyolefin film is produced from olefin polymers complying with § 177.1520 of this chapter, and the average thickness of the film in the form in which it contacts food does not exceed 0.002 inch." 21:21:3.0.1.1.9.4.1.2,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3120 Animal glue.,FDA,,,,"Animal glue may be safely used as a component of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section. (a) Animal glue consists of the proteinaceous extractives obtained from hides, bones, and other collagen-rich substances of animal origin (excluding diseased or rotted animals), to which may be added other optional adjuvant substances required in its production or added to impart desired properties. (b) The quantity of any substance employed in the production of animal glue does not exceed the amount reasonably required to accomplish the intended physical or technical effect nor any limitation further provided. (c) Any substance employed in the production of animal glue and which is the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter conforms with any specification in such regulation. (d) Optional adjuvant substances employed in the production of animal glue include: (1) Substances generally recognized as safe in food. (2) Substances subject to prior sanction or approval for use in animal glue and used in accordance with such sanction or approval. (3) Substances identified in this paragraph (d)(3) and subject to such limitations as are provided: (e) The conditions of use are as follows: (1) The use of animal glue in any substance or article that is the subject of a regulation in this subpart conforms with any specifications or limitations prescribed by such regulation for the finished form of the substance or article. (2) It is used as an adhesive or component of an adhesive in accordance with the provisions of § 175.105 of this chapter. (3) It is used as a colloidal flocculant added to the pulp suspension prior to the sheet-forming operation in the manufacture of paper and paperboard. (4) It is used as a protective colloid in resinous and polymeric emulsion coatings." 21:21:3.0.1.1.9.4.1.20,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3620 Mineral oil.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11847, Mar. 19, 1982; 49 FR 10112, Mar. 19, 1984; 54 FR 24898, June 12, 1989]","Mineral oil may be safely used as a component of nonfood articles intended for use in contact with food, subject to the provisions of this section: (a) White mineral oil meeting the specifications prescribed in § 172.878 of this chapter may be used as a component of nonfood articles provided such use complies with any applicable limitations in parts 170 through 189 of this chapter. The use of white mineral oil in or on food itself, including the use of white mineral oil as a protective coating or release agent for food, is subject to the provisions of § 172.878 of this chapter. (b) Technical white mineral oil identified in paragraph (b)(1) of this section may be used as provided in paragraph (b)(2) of this section. (1) Technical white mineral oil consists of specially refined distillates of virgin petroleum or of specially refined distillates that are produced synthetically from petroleum gases. Technical white mineral oil meets the following specifications: (i) Saybolt color 20 minimum as determined by ASTM method D156-82, “Standard Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method),” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (ii) Ultraviolet absorbance limits as follows: Technical white mineral oil containing antioxidants shall meet the specified ultraviolet absorbance limits after correction for any absorbance due to the antioxidants. The ultraviolet absorbance shall be determined by the procedure described for application to mineral oil under “Specification” on page 66 of the “Journal of the Association of Official Agricultural Chemists,” Volume 45 (February 1962) (which is incorporated by reference; copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. ), disregarding the last two sentences of that procedure and substituting therefor the following: Determine the absorbance of the mineral oil extract in a 10-millimeter cell in the range from 260-350 mµ, inclusive, compared to the solvent control. If the absorbance so measured exceeds 2.0 at any point in range 280-350 mµ, inclusive, dilute the extract and the solvent control, respectively, to twice their volume with dimethyl sulfoxide and remeasure the absorbance. Multiply the remeasured absorbance values by 2 to determine the absorbance of the mineral oil extract per centimeter optical pathlength. (2) Technical white mineral oil may be used wherever mineral oil is permitted for use as a component of nonfood articles complying with §§ 175.105, 176.200, 176.210, 177.2260, 177.2600, and 177.2800 of this chapter and §§ 178.3570 and 178.3910. (3) Technical white mineral oil may contain any antioxidant permitted in food by regulations issued in accordance with section 409 of the Act, in an amount not greater than that required to produce its intended effect. (c) Mineral oil identified in paragraph (c)(1) of this section may be used as provided in paragraph (c)(2) of this section. (1) The mineral oil consists of virgin petroleum distillates refined to meet the following specifications: (i) Initial boiling point of 450 °F minimum. (ii) Color 5.5 maximum as determined by ASTM method D1500-82, “Standard Test Method for ASTM Color of Petroleum Products (ASTM Color Scale),” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (b)(1)(i) of this section. (iii) Ultraviolet absorbance limits as follows as determined by the analytical method described in paragraph (c)(3) of this section: (2) The mineral oil may be used wherever mineral oil is permitted for use as a component of nonfood articles complying with §§ 175.105 and 176.210 of this chapter and § 178.3910 (for use only in rolling of metallic foil and sheet stock), §§ 176.200, 177.2260, 177.2600, and 177.2800 of this chapter. (3) The analytical method for determining ultraviolet absorbance limit is as follows: general instructions Because of the sensitivity of the test, the possibility of errors arising from contamination is great. It is of the greatest importance that all glassware be scrupulously cleaned to remove all organic matter such as oil, grease, detergent residues, etc. Examine all glassware, including stoppers and stopcocks, under ultraviolet light to detect any residual fluorescent contamination. As a precautionary measure it is recommended practice to rinse all glassware with purified isooctane immediately before use. No grease is to be used on stopcocks or joints. Great care to avoid contamination of oil samples in handling and to assure absence of any extraneous material arising from inadequate packaging is essential. Because some of the polynuclear hydrocarbons sought in this test are very susceptible to photo-oxidation, the entire procedure is to be carried out under subdued light. apparatus Separatory funnels. 250-milliliter, 500-milliliter, 1,000-milliliter, and preferably 2,000-milliliter capacity, equipped with tetrafluoroethylene polymer stopcocks. Reservoir. 500-milliliter capacity, equipped with a 24/40 standard taper male fitting at the bottom and a suitable ball-joint at the top for connecting to the nitrogen supply. The male fitting should be equipped with glass hooks. Chromatographic tube. 180 millimeters in length, inside diameter to be 15.7 millimeters ±0.1 millimeter, equipped with a coarse, fritted-glass disc, a tetrafluoroethylene polymer stopcock, and a female 24/40 standard tapered fitting at the opposite end. (Overall length of the column with the female joint is 235 millimeters.) The female fitting should be equipped with glass hooks. Disc. Tetrafluoroethylene polymer 2-inch diameter disk approximately 3/16 -inch thick with a hole bored in the center to closely fit the stem of the chromatographic tube. Suction flask. 250-milliliter or 500-milliliter filter flask. Condenser. 24/40 joints, fitted with a drying tube, length optional. Evaporation flask (optional). 250-milliliter or 500-milliliter capacity all-glass flask equipped with standard taper stopper having inlet and outlet tubes to permit passage of nitrogen across the surface of contained liquid to be evaporated. Spectrophotometric cells. Fused quartz cells, optical path length in the range of 5,000 centimeter ±0.005 centimeter; also for checking spectrophotometer performance only, optical path length in the range 1,000 centimeter ±0.005 centimeter. With distilled water in the cells, determine any absorbance differences. Spectrophotometer. Spectral range 250 millimicrons—400 millimicrons with spectral slit width of 2 millimicrons or less; under instrument operating conditions for these absorbance measurements, the spectrophotometer shall also meet the following performance requirements: Absorbance repeatability, ±0.01 at 0.4 absorbance. Absorbance accuracy 1 ±0.05 at 0.4 absorbance. 1 As determined by procedure using potassium chromate for reference standard and described in National Bureau of Standards Circular 484, Spectrophotometry, U.S. Department of Commerce (1949). The accuracy is to be determined by comparison with the standard values at 290, 345, and 400 millimicrons. Circular 484 is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Wavelength accuracy, ±1.0 millimicron. Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in cylinder equipped with regulator and valve to control flow at 5 p.s.i.g. reagents and materials Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this specification. The isooctane, benzene, acetone, and methyl alcohol designated in the list following this paragraph shall pass the following test: To the specified quantity of solvent in a 250-milliliter Erlenmeyer flask, add 1 milliliter of purified n- hexadecane and evaporate on the steam bath under a stream of nitrogen (a loose aluminum foil jacket around the flask will speed evaporation). Discontinue evaporation when not over 1 milliliter of residue remains. (To the residue from benzene add a 10-milliliter portion of purified isooctane, reevaporate, and repeat once to insure complete removal of benzene.) Alternatively, the evaporation time can be reduced by using the optional evaporation flask. In this case the solvent and n- hexadecane are placed in the flask on the steam bath, the tube assembly is inserted, and a stream of nitrogen is fed through the inlet tube while the outlet tube is connected to a solvent trap and vacuum line in such a way as to prevent any flow-back of condensate into the flask. Dissolve the 1 milliliter of hexadecane residue in isooctane and make to 25 milliliters volume. Determine the absorbance in the 5-centimeter path length cells compared to isooctane as reference. The absorbance of the solution of the solvent residue (except for methyl alcohol) shall not exceed 0.01 per centimeter path length between 280 and 400 mµ. For methyl alcohol this absorbance value shall be 0.00. Isooctane (2,2,4-trimethylpentane). Use 180 milliliters for the test described in the preceding paragraph. Purify, if necessary, by passage through a column of activated silica gel (Grade 12, Davison Chemical Company, Baltimore, Maryland, or equivalent) about 90 centimeters in length and 5 centimeters to 8 centimeters in diameter. Benzene, A.C.S. reagent grade. Use 150 milliliters for the test. Purify, if necessary, by distillation or otherwise. Acetone, A.C.S. reagent grade. Use 200 milliliters for the test. Purify, if necessary, by distillation. Eluting mixtures: 1. 10 percent benzene in isooctane. Pipet 50 milliliters of benzene into a 250-milliliter glass-stoppered volumetric flask and adjust to volume with isooctane, with mixing. 2. 20 percent benzene in isooctane. Pipet 50 milliliters of benzene into a 250-milliliter glass-stoppered volumetric flask and adjust to volume with isooctane, with mixing. 3. Acetone-benzene-water mixture. Add 20 milliliters of water to 380 milliliters of acetone and 200 milliliters of benzene, and mix. n-Hexadecane, 99-percent olefin-free. Dilute 1.0 milliliter of n- hexadecane to 25 milliliters with isooctane and determine the absorbance in a 5-centimeter cell compared to isooctane as reference point between 280 mµ-400 mµ. The absorbance per centimeter path length shall not exceed 0.00 in this range. Purify, if necessary, by percolation through activated silica gel or by distillation. Methyl alcohol, A.C.S. reagent grade. Use 10.0 milliliters of methyl alcohol. Purify, if necessary, by distillation. Dimethyl sulfoxide. Spectrophotometric grade (Crown Zellerbach Corporation, Camas, Washington, or equivalent). Absorbance (1-centimeter cell, distilled water reference, sample completely saturated with nitrogen). Wavelength Absorbance (maximum) 261.5 1.00 270 .20 275 .09 280 .06 300 .015 There shall be no irregularities in the absorbance curve within these wavelengths. Phosphoric acid. 85 percent A.C.S. reagent grade. Sodium borohydride. 98 percent. Magnesium oxide (Sea Sorb 43, Food Machinery Company, Westvaco Division, distributed by chemical supply firms, or equivalent). Place 100 grams of the magnesium oxide in a large beaker, add 700 milliliters of distilled water to make a thin slurry, and heat on a steam bath for 30 minutes with intermittent stirring. Stir well initially to insure that all the adsorbent is completely wetted. Using a Buchner funnel and a filter paper (Schleicher & Schuell No. 597, or equivalent) of suitable diameter, filter with suction. Continue suction until water no longer drips from the funnel. Transfer the adsorbent to a glass trough lined with aluminum foil (free from rolling oil). Break up the magnesia with a clean spatula and spread out the adsorbent on the aluminum foil in a layer about 1 centimeter to 2 centimeters thick. Dry for 24 hours at 160 °C ±1 °C. Pulverize the magnesia with mortar and pestle. Sieve the pulverized adsorbent between 60-180 mesh. Use the magnesia retained on the 180-mesh sieve. Celite 545. Johns Mansville Company, diatomaceous earth, or equivalent. Magnesium oxide-Celite 545 mixture (2 + 1) by weight. Place the magnesium oxide (60-180 mesh) and the Celite 545 in 2 to 1 proportions, respectively, by weight in a glass-stoppered flask large enough for adequate mixing. Shake vigorously for 10 minutes. Transfer the mixture to a glass trough lined with aluminum foil (free from rolling oil) and spread it out on a layer about 1 centimeter to 2 centimeters thick. Reheat the mixture at 160 °C ±1 °C for 2 hours, and store in a tightly closed flask. Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in granular form. For each bottle of sodium sulfate reagent used, establish as follows the necessary sodium sulfate prewash to provide such filters required in the method: Place approximately 35 grams of anhydrous sodium sulfate in a 30-milliliter course, fritted-glass funnel or in a 65-millimeter filter funnel with glass wool plug; wash with successive 15-milliliter portions of the indicated solvent until a 15-milliliter portion of the wash shows 0.00 absorbance per centimeter path length between 280 mµ and 400 mµ when tested as prescribed under “Organic solvents.” Usually three portions of wash solvent are sufficient. Before proceeding with analysis of a sample, determine the absorbance in a 5-centimeter path cell between 250 millimicrons and 400 millimicrons for the reagent blank by carrying out the procedure, without an oil sample, recording the spectra after the extraction stage and after the complete procedure as prescribed. The absorbance per centimeter pathlength following the extraction stage should not exceed 0.02 in the wavelength range from 280 mµ to 400 mµ; the absorbance per centimeter pathlength following the complete procedure should not exceed 0.02 in the wavelength range from 280 mµ to 400 mµ. If in either spectrum the characteristic benzene peaks in the 250 mµ-260 mµ region are present, remove the benzene by the procedure under “Organic solvents” and record absorbance again. Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory funnel and add 75 milliliters of phosphoric acid. Mix the contents of the funnel and allow to stand for 10 minutes. (The reaction between the sulfoxide and the acid is exothermic. Release pressure after mixing, then keep funnel stoppered.) Add 150 milliliters of isooctane and shake to pre-equilibrate the solvents. Draw off the individual layers and store in glass-stoppered flasks. Weigh a 20-gram sample of the oil and transfer to a 500-milliliter separatory funnel containing 100 milliliters of pre-equilibrated sulfoxide-phosphoric acid mixture. Complete the transfer of the sample with small portions of preequilibrated isooctane to give a total volume of the oil and solvent of 75 milliliters. Shake the funnel vigorously for 2 minutes. Set up three 250-milliliter separatory funnels with each containing 30 milliliters of pre-equilibrated isooctane. After separation of liquid phases, carefully draw off lower layer into the first 250-milliliter separatory funnel and wash in tandem with the 30-milliliter portions of isooctane contained in the 250-milliliter separatory funnels. Shaking time for each wash is 1 minute. Repeat the extraction operation with two additional portions of the sulfoxide-acid mixture and wash each extractive in tandem through the same three portions of isooctane. Collect the successive extractives (300 milliliters total) in a separatory funnel (preferably 2-liter) containing 480 milliliters of distilled water; mix, and allow to cool for a few minutes after the last extractive has been added. Add 80 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second separatory funnel (preferably 2-liter) and repeat the extraction with 80 milliliters of isooctane. Draw off and discard the aqueous layer. Wash each of the 80-milliliter extractives three times with 100-milliliter portions of distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate prewashed with isooctane (see Sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the first separatory funnel with the second 80-milliliter isooctane extractive and pass through the sodium sulfate. Then wash the second and first separatory funnels successively with a 20-milliliter portion of isooctane and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane on the steam bath under nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane, reevaporate to 1 milliliter of hexadecane, and repeat this operation once. Quantitatively transfer the residue with isooctane to a 200-milliliter volumetric flask, make to volume, and mix. Determine the absorbance of the solution in the 1-centimeter pathlength cells compared to isooctane as reference between 280 mµ-400 mµ (take care to lose none of the solution in filling the sample cell). Correct the absorbance values for any absorbance derived from reagents as determined by carrying out the procedure without an oil sample. If the corrected absorbance does not exceed the limits prescribed in this paragraph, the oil meets the ultraviolet absorbance specifications. If the corrected absorbance per centimeter pathlength exceeds the limits prescribed in this paragraph, proceed as follows: Quantitatively transfer the isooctane solution to a 125-milliliter flask equipped with 24/40 joint, and evaporate the isooctane on the steam bath under a stream of nitrogen to a volume of 1 milliliter of hexadecane. Add 10 milliliters of methyl alcohol and approximately 0.3 gram of sodium borohydride. (Minimize exposure of the borohydride to the atmosphere. A measuring dipper may be used.) Immediately fit a water-cooled condenser equipped with a 24/40 joint and with a drying tube into the flask, mix until the borohydride is dissolved, and allow to stand for 30 minutes at room temperature, with intermittent swirling. At the end of this period, disconnect the flask and evaporate the methyl alcohol on the steam bath under nitrogen until the sodium borohydride begins to come out of the solution. Then add 10 milliliters of isooctane and evaporate to a volume of about 2-3 milliliters. Again, add 10 milliliters of isooctane and concentrate to a volume of approximately 5 milliliters. Swirl the flask repeatedly to assure adequate washing of the sodium borohydride residues. Fit the tetrafluoroethylene polymer disc on the upper part of the stem of the chromatographic tube, then place the tube with the disc on the suction flask and apply the vacuum (approximately 135 millimeters Hg pressure). Weigh out 14 grams of the 2:1 magnesium oxide-Celite 545 mixture and pour the adsorbent mixture into the chromatographic tube in approximately 3-centimeter layers. After the addition of each layer, level off the top of the adsorbent with a flat glass rod or metal plunger by pressing down firmly until the adsorbent is well packed. Loosen the topmost few millimeters of each adsorbent layer with the end of a metal rod before the addition of the next layer. Continue packing in this manner until all the 14 grams of the adsorbent is added to the tube. Level off the top of the adsorbent by pressing down firmly with a flat glass rod or metal plunger to make the depth of the adsorbent bed approximately 12.5 centimeters in depth. Turn off the vacuum and remove the suction flask. Fit the 500-milliliter reservoir onto the top of the chromatographic column and prewet the column by passing 100 milliliters of isooctane through the column. Adjust the nitrogen pressure so that the rate of descent of the isooctane coming off the column is between 2-3 milliliters per minute. Discontinue pressure just before the last of the isooctane reaches the level of the adsorbent. (Caution: Do not allow the liquid level to recede below the adsorbent level at any time.) Remove the reservoir and decant the 5-milliliter isooctane concentrate solution onto the column and with slight pressure again allow the liquid level to recede to barely above the adsorbent level. Rapidly complete the transfer similarly with two 5-milliliter portions of isooctane, swirling the flask repeatedly each time to assure adequate washing of the residue. Just before the final 5-milliliter wash reaches the top of the adsorbent, add 100 milliliters of isooctane to the reservoir and continue the percolation at the 2-3 milliliters per minute rate. Just before the last of the isooctane reaches the adsorbent level, add 100 milliliters of 10 percent benzene in isooctane to the reservoir and continue the percolation at the aforementioned rate. Just before the solvent mixture reaches adsorbent level, add 25 milliliters of 20 percent benzene in isooctane to the reservoir and continue the percolation at 2-3 milliliters per minute until all this solvent mixture has been removed from the column. Discard all the elution solvents collected up to this point. Add 300 milliliters of the acetone-benzene-water mixture to the reservoir and percolate through the column to eluate the polynuclear compounds. Collect the eluate in a clean 1-liter separatory funnel. Allow the column to drain until most of the solvent mixture is removed. Wash the eluate three times with 300-milliliter portions of distilled water, shaking well for each wash. (The addition of small amounts of sodium chloride facilitates separation.) Discard the aqueous layer after each wash. After the final separation, filter the residual benzene through anhydrous sodium sulfate pre-washed with benzene (see Sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the separatory funnel with two additional 20-milliliter portions of benzene which are also filtered through the sodium sulfate. Add 1 milliliter of n -hexadecane and completely remove the benzene by evaporation under nitrogen, using the special procedure to eliminate benzene as previously described under “Organic solvents.” Quantitatively transfer the residue with isooctane to a 200-milliliter volumetric flask and adjust to volume. Determine the absorbance of the solution in the 1-centimeter pathlength cells compared to isooctane as reference between 250 mµ-400 mµ. Correct for any absorbance derived from the reagents as determined by carrying out the procedure without an oil sample. If either spectrum shows the characteristic benzene peaks in the 250 mµ-260 mµ region, evaporate the solution to remove benzene by the procedure under “Organic solvents.” Dissolve the residue, transfer quantitatively, and adjust to volume in isooctane in a 200-milliliter volumetric flask. Record the absorbance again. If the corrected absorbance does not exceed the limits proposed in this paragraph, the oil meets the proposed ultraviolet absorbance specifications. Because of the sensitivity of the test, the possibility of errors arising from contamination is great. It is of the greatest importance that all glassware be scrupulously cleaned to remove all organic matter such as oil, grease, detergent residues, etc. Examine all glassware, including stoppers and stopcocks, under ultraviolet light to detect any residual fluorescent contamination. As a precautionary measure it is recommended practice to rinse all glassware with purified isooctane immediately before use. No grease is to be used on stopcocks or joints. Great care to avoid contamination of oil samples in handling and to assure absence of any extraneous material arising from inadequate packaging is essential. Because some of the polynuclear hydrocarbons sought in this test are very susceptible to photo-oxidation, the entire procedure is to be carried out under subdued light. Separatory funnels. 250-milliliter, 500-milliliter, 1,000-milliliter, and preferably 2,000-milliliter capacity, equipped with tetrafluoroethylene polymer stopcocks. Reservoir. 500-milliliter capacity, equipped with a 24/40 standard taper male fitting at the bottom and a suitable ball-joint at the top for connecting to the nitrogen supply. The male fitting should be equipped with glass hooks. Chromatographic tube. 180 millimeters in length, inside diameter to be 15.7 millimeters ±0.1 millimeter, equipped with a coarse, fritted-glass disc, a tetrafluoroethylene polymer stopcock, and a female 24/40 standard tapered fitting at the opposite end. (Overall length of the column with the female joint is 235 millimeters.) The female fitting should be equipped with glass hooks. Disc. Tetrafluoroethylene polymer 2-inch diameter disk approximately 3/16 -inch thick with a hole bored in the center to closely fit the stem of the chromatographic tube. Suction flask. 250-milliliter or 500-milliliter filter flask. Condenser. 24/40 joints, fitted with a drying tube, length optional. Evaporation flask (optional). 250-milliliter or 500-milliliter capacity all-glass flask equipped with standard taper stopper having inlet and outlet tubes to permit passage of nitrogen across the surface of contained liquid to be evaporated. Spectrophotometric cells. Fused quartz cells, optical path length in the range of 5,000 centimeter ±0.005 centimeter; also for checking spectrophotometer performance only, optical path length in the range 1,000 centimeter ±0.005 centimeter. With distilled water in the cells, determine any absorbance differences. Spectrophotometer. Spectral range 250 millimicrons—400 millimicrons with spectral slit width of 2 millimicrons or less; under instrument operating conditions for these absorbance measurements, the spectrophotometer shall also meet the following performance requirements: Absorbance repeatability, ±0.01 at 0.4 absorbance. Absorbance accuracy 1 ±0.05 at 0.4 absorbance. 1 As determined by procedure using potassium chromate for reference standard and described in National Bureau of Standards Circular 484, Spectrophotometry, U.S. Department of Commerce (1949). The accuracy is to be determined by comparison with the standard values at 290, 345, and 400 millimicrons. Circular 484 is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Wavelength accuracy, ±1.0 millimicron. Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in cylinder equipped with regulator and valve to control flow at 5 p.s.i.g. Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this specification. The isooctane, benzene, acetone, and methyl alcohol designated in the list following this paragraph shall pass the following test: To the specified quantity of solvent in a 250-milliliter Erlenmeyer flask, add 1 milliliter of purified n- hexadecane and evaporate on the steam bath under a stream of nitrogen (a loose aluminum foil jacket around the flask will speed evaporation). Discontinue evaporation when not over 1 milliliter of residue remains. (To the residue from benzene add a 10-milliliter portion of purified isooctane, reevaporate, and repeat once to insure complete removal of benzene.) Alternatively, the evaporation time can be reduced by using the optional evaporation flask. In this case the solvent and n- hexadecane are placed in the flask on the steam bath, the tube assembly is inserted, and a stream of nitrogen is fed through the inlet tube while the outlet tube is connected to a solvent trap and vacuum line in such a way as to prevent any flow-back of condensate into the flask. Dissolve the 1 milliliter of hexadecane residue in isooctane and make to 25 milliliters volume. Determine the absorbance in the 5-centimeter path length cells compared to isooctane as reference. The absorbance of the solution of the solvent residue (except for methyl alcohol) shall not exceed 0.01 per centimeter path length between 280 and 400 mµ. For methyl alcohol this absorbance value shall be 0.00. Isooctane (2,2,4-trimethylpentane). Use 180 milliliters for the test described in the preceding paragraph. Purify, if necessary, by passage through a column of activated silica gel (Grade 12, Davison Chemical Company, Baltimore, Maryland, or equivalent) about 90 centimeters in length and 5 centimeters to 8 centimeters in diameter. Benzene, A.C.S. reagent grade. Use 150 milliliters for the test. Purify, if necessary, by distillation or otherwise. Acetone, A.C.S. reagent grade. Use 200 milliliters for the test. Purify, if necessary, by distillation. Eluting mixtures: 1. 10 percent benzene in isooctane. Pipet 50 milliliters of benzene into a 250-milliliter glass-stoppered volumetric flask and adjust to volume with isooctane, with mixing. 2. 20 percent benzene in isooctane. Pipet 50 milliliters of benzene into a 250-milliliter glass-stoppered volumetric flask and adjust to volume with isooctane, with mixing. 3. Acetone-benzene-water mixture. Add 20 milliliters of water to 380 milliliters of acetone and 200 milliliters of benzene, and mix. n-Hexadecane, 99-percent olefin-free. Dilute 1.0 milliliter of n- hexadecane to 25 milliliters with isooctane and determine the absorbance in a 5-centimeter cell compared to isooctane as reference point between 280 mµ-400 mµ. The absorbance per centimeter path length shall not exceed 0.00 in this range. Purify, if necessary, by percolation through activated silica gel or by distillation. Methyl alcohol, A.C.S. reagent grade. Use 10.0 milliliters of methyl alcohol. Purify, if necessary, by distillation. Dimethyl sulfoxide. Spectrophotometric grade (Crown Zellerbach Corporation, Camas, Washington, or equivalent). Absorbance (1-centimeter cell, distilled water reference, sample completely saturated with nitrogen). There shall be no irregularities in the absorbance curve within these wavelengths. Phosphoric acid. 85 percent A.C.S. reagent grade. Sodium borohydride. 98 percent. Magnesium oxide (Sea Sorb 43, Food Machinery Company, Westvaco Division, distributed by chemical supply firms, or equivalent). Place 100 grams of the magnesium oxide in a large beaker, add 700 milliliters of distilled water to make a thin slurry, and heat on a steam bath for 30 minutes with intermittent stirring. Stir well initially to insure that all the adsorbent is completely wetted. Using a Buchner funnel and a filter paper (Schleicher & Schuell No. 597, or equivalent) of suitable diameter, filter with suction. Continue suction until water no longer drips from the funnel. Transfer the adsorbent to a glass trough lined with aluminum foil (free from rolling oil). Break up the magnesia with a clean spatula and spread out the adsorbent on the aluminum foil in a layer about 1 centimeter to 2 centimeters thick. Dry for 24 hours at 160 °C ±1 °C. Pulverize the magnesia with mortar and pestle. Sieve the pulverized adsorbent between 60-180 mesh. Use the magnesia retained on the 180-mesh sieve. Celite 545. Johns Mansville Company, diatomaceous earth, or equivalent. Magnesium oxide-Celite 545 mixture (2 + 1) by weight. Place the magnesium oxide (60-180 mesh) and the Celite 545 in 2 to 1 proportions, respectively, by weight in a glass-stoppered flask large enough for adequate mixing. Shake vigorously for 10 minutes. Transfer the mixture to a glass trough lined with aluminum foil (free from rolling oil) and spread it out on a layer about 1 centimeter to 2 centimeters thick. Reheat the mixture at 160 °C ±1 °C for 2 hours, and store in a tightly closed flask. Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in granular form. For each bottle of sodium sulfate reagent used, establish as follows the necessary sodium sulfate prewash to provide such filters required in the method: Place approximately 35 grams of anhydrous sodium sulfate in a 30-milliliter course, fritted-glass funnel or in a 65-millimeter filter funnel with glass wool plug; wash with successive 15-milliliter portions of the indicated solvent until a 15-milliliter portion of the wash shows 0.00 absorbance per centimeter path length between 280 mµ and 400 mµ when tested as prescribed under “Organic solvents.” Usually three portions of wash solvent are sufficient. Before proceeding with analysis of a sample, determine the absorbance in a 5-centimeter path cell between 250 millimicrons and 400 millimicrons for the reagent blank by carrying out the procedure, without an oil sample, recording the spectra after the extraction stage and after the complete procedure as prescribed. The absorbance per centimeter pathlength following the extraction stage should not exceed 0.02 in the wavelength range from 280 mµ to 400 mµ; the absorbance per centimeter pathlength following the complete procedure should not exceed 0.02 in the wavelength range from 280 mµ to 400 mµ. If in either spectrum the characteristic benzene peaks in the 250 mµ-260 mµ region are present, remove the benzene by the procedure under “Organic solvents” and record absorbance again. Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory funnel and add 75 milliliters of phosphoric acid. Mix the contents of the funnel and allow to stand for 10 minutes. (The reaction between the sulfoxide and the acid is exothermic. Release pressure after mixing, then keep funnel stoppered.) Add 150 milliliters of isooctane and shake to pre-equilibrate the solvents. Draw off the individual layers and store in glass-stoppered flasks. Weigh a 20-gram sample of the oil and transfer to a 500-milliliter separatory funnel containing 100 milliliters of pre-equilibrated sulfoxide-phosphoric acid mixture. Complete the transfer of the sample with small portions of preequilibrated isooctane to give a total volume of the oil and solvent of 75 milliliters. Shake the funnel vigorously for 2 minutes. Set up three 250-milliliter separatory funnels with each containing 30 milliliters of pre-equilibrated isooctane. After separation of liquid phases, carefully draw off lower layer into the first 250-milliliter separatory funnel and wash in tandem with the 30-milliliter portions of isooctane contained in the 250-milliliter separatory funnels. Shaking time for each wash is 1 minute. Repeat the extraction operation with two additional portions of the sulfoxide-acid mixture and wash each extractive in tandem through the same three portions of isooctane. Collect the successive extractives (300 milliliters total) in a separatory funnel (preferably 2-liter) containing 480 milliliters of distilled water; mix, and allow to cool for a few minutes after the last extractive has been added. Add 80 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second separatory funnel (preferably 2-liter) and repeat the extraction with 80 milliliters of isooctane. Draw off and discard the aqueous layer. Wash each of the 80-milliliter extractives three times with 100-milliliter portions of distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate prewashed with isooctane (see Sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the first separatory funnel with the second 80-milliliter isooctane extractive and pass through the sodium sulfate. Then wash the second and first separatory funnels successively with a 20-milliliter portion of isooctane and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane on the steam bath under nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane, reevaporate to 1 milliliter of hexadecane, and repeat this operation once. Quantitatively transfer the residue with isooctane to a 200-milliliter volumetric flask, make to volume, and mix. Determine the absorbance of the solution in the 1-centimeter pathlength cells compared to isooctane as reference between 280 mµ-400 mµ (take care to lose none of the solution in filling the sample cell). Correct the absorbance values for any absorbance derived from reagents as determined by carrying out the procedure without an oil sample. If the corrected absorbance does not exceed the limits prescribed in this paragraph, the oil meets the ultraviolet absorbance specifications. If the corrected absorbance per centimeter pathlength exceeds the limits prescribed in this paragraph, proceed as follows: Quantitatively transfer the isooctane solution to a 125-milliliter flask equipped with 24/40 joint, and evaporate the isooctane on the steam bath under a stream of nitrogen to a volume of 1 milliliter of hexadecane. Add 10 milliliters of methyl alcohol and approximately 0.3 gram of sodium borohydride. (Minimize exposure of the borohydride to the atmosphere. A measuring dipper may be used.) Immediately fit a water-cooled condenser equipped with a 24/40 joint and with a drying tube into the flask, mix until the borohydride is dissolved, and allow to stand for 30 minutes at room temperature, with intermittent swirling. At the end of this period, disconnect the flask and evaporate the methyl alcohol on the steam bath under nitrogen until the sodium borohydride begins to come out of the solution. Then add 10 milliliters of isooctane and evaporate to a volume of about 2-3 milliliters. Again, add 10 milliliters of isooctane and concentrate to a volume of approximately 5 milliliters. Swirl the flask repeatedly to assure adequate washing of the sodium borohydride residues. Fit the tetrafluoroethylene polymer disc on the upper part of the stem of the chromatographic tube, then place the tube with the disc on the suction flask and apply the vacuum (approximately 135 millimeters Hg pressure). Weigh out 14 grams of the 2:1 magnesium oxide-Celite 545 mixture and pour the adsorbent mixture into the chromatographic tube in approximately 3-centimeter layers. After the addition of each layer, level off the top of the adsorbent with a flat glass rod or metal plunger by pressing down firmly until the adsorbent is well packed. Loosen the topmost few millimeters of each adsorbent layer with the end of a metal rod before the addition of the next layer. Continue packing in this manner until all the 14 grams of the adsorbent is added to the tube. Level off the top of the adsorbent by pressing down firmly with a flat glass rod or metal plunger to make the depth of the adsorbent bed approximately 12.5 centimeters in depth. Turn off the vacuum and remove the suction flask. Fit the 500-milliliter reservoir onto the top of the chromatographic column and prewet the column by passing 100 milliliters of isooctane through the column. Adjust the nitrogen pressure so that the rate of descent of the isooctane coming off the column is between 2-3 milliliters per minute. Discontinue pressure just before the last of the isooctane reaches the level of the adsorbent. (Caution: Do not allow the liquid level to recede below the adsorbent level at any time.) Remove the reservoir and decant the 5-milliliter isooctane concentrate solution onto the column and with slight pressure again allow the liquid level to recede to barely above the adsorbent level. Rapidly complete the transfer similarly with two 5-milliliter portions of isooctane, swirling the flask repeatedly each time to assure adequate washing of the residue. Just before the final 5-milliliter wash reaches the top of the adsorbent, add 100 milliliters of isooctane to the reservoir and continue the percolation at the 2-3 milliliters per minute rate. Just before the last of the isooctane reaches the adsorbent level, add 100 milliliters of 10 percent benzene in isooctane to the reservoir and continue the percolation at the aforementioned rate. Just before the solvent mixture reaches adsorbent level, add 25 milliliters of 20 percent benzene in isooctane to the reservoir and continue the percolation at 2-3 milliliters per minute until all this solvent mixture has been removed from the column. Discard all the elution solvents collected up to this point. Add 300 milliliters of the acetone-benzene-water mixture to the reservoir and percolate through the column to eluate the polynuclear compounds. Collect the eluate in a clean 1-liter separatory funnel. Allow the column to drain until most of the solvent mixture is removed. Wash the eluate three times with 300-milliliter portions of distilled water, shaking well for each wash. (The addition of small amounts of sodium chloride facilitates separation.) Discard the aqueous layer after each wash. After the final separation, filter the residual benzene through anhydrous sodium sulfate pre-washed with benzene (see Sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the separatory funnel with two additional 20-milliliter portions of benzene which are also filtered through the sodium sulfate. Add 1 milliliter of n -hexadecane and completely remove the benzene by evaporation under nitrogen, using the special procedure to eliminate benzene as previously described under “Organic solvents.” Quantitatively transfer the residue with isooctane to a 200-milliliter volumetric flask and adjust to volume. Determine the absorbance of the solution in the 1-centimeter pathlength cells compared to isooctane as reference between 250 mµ-400 mµ. Correct for any absorbance derived from the reagents as determined by carrying out the procedure without an oil sample. If either spectrum shows the characteristic benzene peaks in the 250 mµ-260 mµ region, evaporate the solution to remove benzene by the procedure under “Organic solvents.” Dissolve the residue, transfer quantitatively, and adjust to volume in isooctane in a 200-milliliter volumetric flask. Record the absorbance again. If the corrected absorbance does not exceed the limits proposed in this paragraph, the oil meets the proposed ultraviolet absorbance specifications. (d) Mineral oil identified in paragraph (d)(1) of this section may be used as provided in paragraph (d)(2) of this section. (1) The mineral oil consists of virgin petroleum distillates refined to meet the following specifications: (i) Distillation endpoint at 760 millimeters pressure not to exceed 371 °C, with a maximum residue not to exceed 2 percent, as determined by ASTM method D86-82, “Standard Method for Distillation of Petroleum Products,” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (b)(1)(i) of this section. (ii) Ultraviolet absorbance limits as follows as determined by the method described in paragraph (d)(3) of this section. (iii) Pyrene content not to exceed a maximum of 25 parts per million as determined by the method described in paragraph (d)(3) of this section. (2) The mineral oil may be used only in the processing of jute fiber employed in the production of textile bags intended for use in contact with the following types of food: Dry grains and dry seeds (for example, beans, peas, rice, and lentils); whole root crop vegetables of the types identified in 40 CFR 180.34(f); unshelled and shelled nuts (including peanuts); and dry animal feed. The finished processed jute fiber shall contain no more than 6 percent by weight of residual mineral oil. (3) The analytical method for determining ultraviolet absorbance limits and pyrene content is as follows: I. Apparatus. A. Assorted beakers, separatory funnels fitted with tetrafluoroethylene polymer stopcocks, and graduated cylinders. B. Volumetric flasks, 200-milliliter. C. A chromatographic column made from nominal 1.3 centimeters outside diameter × 75 centimeters glass tubing tapered at one end and joined to a 2-millimeter-bore tetrafluoroethylene polymer stopcock. The opposite end is flanged and joined to a female 24/40 standard taper fitting. This provides for accommodating the 500-milliliter reservoir described in item I.E below. D. A chromatographic column made from nominal 1.7 centimeters outside diameter × 115 centimeters glass tubing tapered at one end and joined to a 2-millimeter-bore tetrafluoroethylene polymer stopcock. The opposite end is flanged and joined to a 2.5 centimeters outside diameter × 9.0 centimeters glass tube having a female 24/40 standard taper fitting. This provides for accommodating the 500-milliliter reservoir described in item I. E below. E. A 500-milliliter reservoir having a 24/40 standard taper male fitting at bottom and a suitable ball joint at the top for connecting to the nitrogen supply. The female fitting of the chromatographic columns described in items I. C and D above and the male fitting of the reservoir described in this item E should both be equipped with glass hooks. ( Note: Rubber stoppers are not to be used. Stopcock grease is not to be used on ground-glass joints in this method.) F. A spectrophotometer equipped to automatically record absorbance of liquid samples in 1-centimeter pathlength cells in the spectral region of 280-400 mµ with a spectral slit width of 2 mµ or less. At an absorbance level of about 0.4, absorbance measurements shall be repeatable within ±0.01 and accurate within ±0.05. Wavelength measurements shall be repeatable with ±0.2 mµ and accurate within ±1.0 mµ. Instrument operating conditions are selected to realize this performance under dynamic (automatic) recording operations. Accuracy of absorbance measurements are determined at 290, 345, and 400 mµ, using potassium chromate as the reference standard. (National Bureau of Standards Circular 484, Spectrophotometry, U.S. Department of Commerce, 1949.) G. Two fused quartz cells having pathlengths of 1.00±0.005 centimeter or better. II. Purity of reagents and materials. Reagent-grade chemicals shall be used in all tests. It is further specified that each chemical shall be tested for purity in accordance with the instruction given under “Reagents and Materials” in III below. In addition, a blank run by the procedure shall be made on each purified lot of reagents and materials. Unless otherwise indicated, references to water shall be understood to mean distilled water. III. Reagents and materials— A. Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this section III. The isooctane, benzene, cyclohexane, nitromethane, and n -hexadecane designated shall pass the following test: To the specified quantity of solvent in a 150-milliliter beaker, add 1 milliliter of purified n -hexadecane and evaporate on the steam bath under a stream of nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains (to the residue from benzene and nitromethane add a 10-milliliter portion of purified isooctane, re-evaporate, and repeat once to insure complete removal of solvent). Dissolve the 1 milliliter of n -hexadecane residue in isooctane and make to 10-milliliter volume. Determine the absorbance in 1.0-centimeter pathlength cells compared to water as reference. The absorbance of the solution of solvent residue shall not exceed 0.05 between 280 and 400 mµ. 1. Isooctane ( 2,2,4-trimethylpentane ). Use 240 milliliters for the above test. Purify, if necessary, by passage through a column of activated silica gel. 2. Benzene. Use 200 milliliters for the above test. Purify, if necessary, by distillation or otherwise. 3. Cyclohexane. Use 70 milliliters for the above test. Purify, if necessary, by distillation, silica gel percolation, or otherwise. 4. Nitromethane. Use 125 milliliters for the above test. Purify, if necessary, by distillation or otherwise. 5. n-Hexadecane. Determine the absorbance on this solvent directly. Purify, if necessary, by silica gel percolation or otherwise. B. Other materials— 1. Pyrene standard reference. Pyrene, reagent grade, melting point range 150-152 °C. (Organic Chemical 3627, Eastman Kodak Co., Rochester, N.Y., or equivalent). The standard reference absorbance is the absorbance at 334 millimicrons of a standard reference solution of pyrene containing a concentration of 1.0 milligram per liter in purified isooctane measured against isooctane of the same spectral purity in 1.0-centimeter cells. (This absorbance will be approximately 0.28.) 2. Chrysene solution. Prepare a solution at a concentration of 5.0 milligrams per liter by dissolving 5.0 milligrams of chrysene in purified isooctane in a 1-liter volumetric flask. Adjust to volume with isooctane. 3. Nitrogen gas. Water pumped or equivalent purity, cylinder with regulator, and valve control flow at 5 p.s.i. 4. Silica gel. 100-200 mesh (Davison Chemical, Baltimore, Md., Grade 923, or equivalent), purified and activated by the following procedure: Place about 1 kilogram of silica gel in a large column and wash with contaminant-free benzene until a 200-milliliter sample of the benzene coming off the column will pass the ultraviolet absorption test for benzene. This test is performed as stipulated under “Organic solvents” in A under III above. When the silica gel has been sufficiently cleaned, activate the gel before use by placing the 1-kilogram batch in a shallow container in a layer no greater than 1 inch in depth and heating in an oven (Caution! Explosion Hazard) at 130 °C. for 16 hours, and store in a vacuum desiccator. Reheating about once a week is necessary if the silica gel is repeatedly removed from the desiccator. 5. Aluminum oxide ( Aluminum Co. of America, Grade F-20, or equivalent grade ). 80-200 mesh, purified and activated by the following procedure: Place about 1 kilogram of aluminum oxide in a large column and wash with contaminant-free benzene until a 200-milliliter sample of the benzene coming off the column will pass the ultraviolet absorption test for benzene. This test is performed as stipulated under “Organic solvents” in A under III above. (Caution! Remove Benzene From Adsorbent Under Vacuum To Minimize Explosion Hazard in Subsequent Heating!) When the aluminum oxide has been sufficiently cleaned and freed of solvent, activate it before use by placing the 1-kilogram batch in a shallow container in a layer no greater than 1 inch in depth. Heat in an oven at 130 °C for 16 hours. Upon removal from heat, store at atmospheric pressure over 80 percent (by weight) sulfuric acid in a desiccator for at least 36 hours before use. This gives aluminum oxide with between 6 to 9.5 percent volatiles. This is determined by heating a weighed sample of the prepared aluminum oxide at 2,000 °F for 2 hours and then quickly reweighing. To insure the proper adsorptive properties of the aluminum oxide, perform the following test: a. Weigh 50 grams ±1 gram of the activated aluminum oxide and pack into the chromatographic column (1.3 centimeters × 75 centimeters) described under “Apparatus” in C under I above. Use glass wool at the column exit to prevent the aluminum oxide from passing through the column. b. Place a 250-milliliter graduated cylinder under the column to measure the amount of eluate coming from the column. c. Prewet the aluminum oxide by passing 40 milliliters of isooctane through the column. Adjust the nitrogen pressure so that the rate of descent of the isooctane coming off the column is between 1.5 to 2.5 milliliters per minute. d. Just prior to the last of the isooctane reaching the top of the aluminum oxide bed, add 10 milliliters of the isooctane solution containing 5.0 milligrams of chrysene per liter. e. Continue percolation until the isooctane is just above the aluminum oxide. Then add 200 milliliters of a mixture of benzene and isooctane (33 1/3 percent benzene and 66 2/3 percent isooctane by volume) to the reservoir and continue percolation. f. Continue percolation, collecting the eluates (40 milliliters of the prewet solution, 10 milliliters of the sample solution, and 200 milliliters of the gradient solution) in the 250-milliliter graduated cylinder until the level of the gradient solution is just above the aluminum oxide. Add 200 milliliters of the eluting solution of benzene and isooctane (90 percent benzene and 10 percent isooctane by volume) to the column and continue collecting until a total of 250 milliliters of solution has been obtained. This may be discarded. Now begin to collect the final eluate. g. Place a 100-milliliter graduated cylinder under the column and continue the percolation until a 100-milliliter eluate has been obtained. h. Measure the amount of chrysene in this 100-milliliter fraction by ultraviolet analysis. If the aluminum oxide is satisfactory, more than 80 percent of the original amount of chrysene should be found in this fraction. ( Note: If the amount of chrysene recovered is less than 80 percent, the original batch of aluminum oxide should be sieved between 100-160 mesh. Activation and testing of this sieved batch should indicate a satisfactory aluminum oxide for use.) IV. Sampling. Precautions must be taken to insure that an uncontaminated sample of the mineral oil is obtained since ultraviolet absorption is very sensitive to small amounts of extraneous material contaminating the sample through careless handling. V. Procedure. A. Blank. Before proceeding with the analysis of a sample, determine the absorbance of the solvent residues by carrying out the procedure without a sample. B. Sample. 1. Weigh out 20.0 grams ±0.1 gram of the mineral oil into a beaker and transfer to a 250-milliliter separatory funnel fitted with a tetrafluoroethylene polymer stopcock, using enough cyclohexane (25 milliliters) to give a final total volume of 50 milliliters (mineral oil plus cyclohexane). 2. Add 25 milliliters of nitromethane saturated with cyclohexane and shake by hand vigorously for 3 minutes. Recover the lower nitromethane layer in a 150-milliliter beaker containing 1 milliliter of n -hexadecane and evaporate on the steam bath under nitrogen. Repeat the extraction four more times, recovering each extract in the 150-milliliter beaker. Exercise care not to fill the beaker to such a capacity that solvent losses may occur. Evaporate the combined nitromethane extracts to 1 milliliter of n -hexadecane residue containing the nitromethane-soluble mineral oil extractives. ( Note: Complete removal of the nitromethane is essential. This can be assured by two successive additions of 5 milliliters of isooctane and reevaporation.) 3. Remove the beaker from the steam bath and allow to cool. 4. Weigh 50 grams ±1 gram of activated aluminum oxide and pack into the chromatographic column (1.3 centimeters × 75 centimeters) described under “Apparatus” in C under I above. ( Note: A small plug of glass wool is placed at the column exit to prevent the aluminum oxide from passing through the column. After adding aluminum oxide, tap the column lightly to remove air voids. All percolations using aluminum oxide are performed under nitrogen pressure. The 500-milliliter reservoir described under “Apparatus” in E under I above is to be used to hold the elution solvents.) 5. Prewet the column by adding 40 milliliters of isooctane to the column. Adjust nitrogen pressure so that rate of descent of the isooctane coming off the column is 2.0 to 3.0 milliliters per minute. Be careful to maintain the level of solvent in the reservoir to prevent air from entering the aluminum oxide bed. New or additional solvent is added just before the last portion of the previous solvent enters the bed. To minimize possible photo-oxidation effects, the following procedures (steps 6 through 18) shall be carried out in subdued light. 6. Before the last of the isooctane reaches the top of the aluminum oxide bed, release the nitrogen pressure and turn off the stopcock on the column. Transfer the n -hexadecane residue from the 150-milliliter beaker from procedure step 3 above onto the column, using several washes of isooctane (total volume of washes should be no greater than 10-15 milliliters). 7. Open the stopcock and continue percolation until the isooctane is about 1 centimeter above the top of the aluminum oxide bed. Add 200 milliliters of isooctane to the reservoir, and continue the percolation at the specified rate. 8. Just before the isooctane surface reaches the top of the aluminum oxide bed, add 200 milliliters of a mixture of benzene and isooctane (33 1/3 percent benzene and 66 2/3 percent isooctane by volume) to the reservoir, and continue the percolation. 9. Just before the surface of this mixture reaches the top of the aluminum oxide bed, release the nitrogen pressure, turn off the stopcock, and discard all the elution solvents collected up to this point. 10. Add to the reservoir 300 milliliters of a mixture of benzene and isooctane (90 percent benzene and 10 percent isooctane by volume), place a 25-milliliter graduated cylinder under the column, continue the percolation until 20 milliliters of eluate has been collected, and then discard the eluate. 11. At this point, place a clean 250-milliliter Erlenmeyer flask under the column. Continue the percolation and collect all the remaining eluate. ( Note: Allow the column to drain completely. An increase in the nitrogen pressure may be necessary as the last of the solvent comes off the column.) 12. Place 1 milliliter of n -hexadecane into a 150-milliliter beaker. Place this onto a steam bath under a nitrogen stream and transfer in small portions the eluate from step 11 above. Wash out the Erlenmeyer flask with small amounts of benzene and transfer to the evaporation beaker. Evaporate until only 1 milliliter of hexadecane residue remains. ( Note: Complete removal of the benzene is essential. This can be assured by two successive additions of 5 milliliters of isooctane and reevaporation.) 13. Remove the beaker from the steam bath and cool. 14. Place a sample of 113.5 grams activated 100- 200-mesh silica gel in a 500-milliliter glass-stoppered Erlenmeyer flask. Add to the silica gel 46.2 grams (41 milliliters) of nitromethane. Stopper and shake the flask vigorously until no lumps of silica gel are observed and then shake occasionally during a period of 1 hour. The resultant nitromethane-treated silica gel is 29 weight-percent nitro-methane and 71 weight-percent silica gel. 15. Place a small plug of glass wool in the tapered end of the 1.7 centimeters outside diameter × 115 centimeters column, described under “Apparatus” in D of I above, adjacent to the stopcock to prevent silica gel from passing through the stopcock. Pack the nitromethane-treated silica gel into the column, tapping lightly. The resultant silica gel bed should be about 95 centimeters in depth. Place into a flask 170 milliliters of isooctane saturated with nitromethane. 16. Place a 100-milliliter graduated cylinder under the column and transfer the residue from the beaker in procedure step 13 above with several washes of the 170 milliliters of isooctane, saturated with nitromethane, onto the top of the column. (Total volume of washes should be no greater than 10 to 15 milliliters.) Permit isooctane solution to enter the silica gel bed until the liquid level is at the top bed level. Place the remaining amount of the 170 milliliters of isooctane, saturated with nitromethane, in the reservoir above the bed for percolation through the silica gel. Apply nitrogen pressure to the top of the column, adjusting the pressure so that the isooctane is collected at the rate of 2.5 to 3.5 milliliters per minute, and percolate isooctane through the bed until a quantity of 75.0 milliliters of eluate is collected. Discard the 75 milliliters of eluate. Turn off the stopcock and add 250 milliliters of benzene to the reservoir above the bed. Use a 400-milliliter beaker to collect the remaining eluate. 17. Open the stopcock, renew the pressure, and percolate the remaining isooctane and benzene through the column eluting the remaining aromatics. Transfer the eluate in small portions from the 400 milliliter beaker to a 150-milliliter beaker containing 1 milliliter of n -hexadecane and evaporate on the steam bath under nitrogen. Rinse the 400-milliliter beaker well with small portions of isooctane to obtain a complete transfer. ( Note: Complete removal of the nitromethane and benzene is essential. This can be assured by successive additions of 5 milliliters of isooctane and reevaporation.) 18. Transfer the residue with several washes of isooctane into a 200-milliliter volumetric flask. Add isooctane to mark. 19. Record the spectrum of the sample solution in a 1-centimeter cell compared to isooctane from 270 to 400 mµ. After making necessary corrections in the spectrum for cell differences and for the blank absorbance, record the maximum absorbance in each of the wavelength intervals (mµ), 280-299, 300-319, 320-359, 360-400. a. If the spectrum then shows no discernible peak corresponding to the absorbance maximum of the pyrene reference standard solution at 334 mµ, the maximum absorbances in the respective wavelength intervals recorded shall not exceed those prescribed in paragraph (d)(1)(ii) of this section. b. If such a peak is evident in the spectrum of the sample solution, and the spectrum as a whole is not incompatible with that of a pyrene contaminant yielding such a peak of the observed absorbance, calculate the concentration of pyrene that would yield this peak (334 m) by the base-line technique described in ASTM method E169-63 (Reapproved 1981), “Standard Recommended Practices for General Techniques of Ultraviolet Quantitative Analysis,” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (b)(1)(i) of this section. Correct each of the maximum absorbances in the respective specified wavelength intervals by subtracting the absorbance due to pyrene, determined as follows: where: Cp = Calculated concentration of pyrene in sample solution; Sp = Concentration of pyrene reference standard solution in same units of concentration; Sa = Absorbance of pyrene reference standard solution at wavelength of maximum absorbance of sample solution in the respective specified wavelength intervals. Also calculate the pyrene content of the oil sample in parts per million as follows: where: C = Calculated concentration of pyrene in milligrams per liter of sample solution. c. The pyrene content so determined shall not exceed 25 p.p.m. The maximum absorbances corrected for pyrene content as described in this step 19 for each of the specified wavelength intervals shall not exceed the limits prescribed in paragraph (d)(1)(ii) of this section. d. If the spectrum as a whole of the sample solution is in any respect clearly incompatible with the presence of pyrene as the source of the peak at 334 mµ, then the maximum absorbances in the respective wavelength intervals without correction for any assumed pyrene content shall not exceed the limits prescribed in paragraph (d)(1)(ii) of this section. I. Apparatus. A. Assorted beakers, separatory funnels fitted with tetrafluoroethylene polymer stopcocks, and graduated cylinders. B. Volumetric flasks, 200-milliliter. C. A chromatographic column made from nominal 1.3 centimeters outside diameter × 75 centimeters glass tubing tapered at one end and joined to a 2-millimeter-bore tetrafluoroethylene polymer stopcock. The opposite end is flanged and joined to a female 24/40 standard taper fitting. This provides for accommodating the 500-milliliter reservoir described in item I.E below. D. A chromatographic column made from nominal 1.7 centimeters outside diameter × 115 centimeters glass tubing tapered at one end and joined to a 2-millimeter-bore tetrafluoroethylene polymer stopcock. The opposite end is flanged and joined to a 2.5 centimeters outside diameter × 9.0 centimeters glass tube having a female 24/40 standard taper fitting. This provides for accommodating the 500-milliliter reservoir described in item I. E below. E. A 500-milliliter reservoir having a 24/40 standard taper male fitting at bottom and a suitable ball joint at the top for connecting to the nitrogen supply. The female fitting of the chromatographic columns described in items I. C and D above and the male fitting of the reservoir described in this item E should both be equipped with glass hooks. ( Note: Rubber stoppers are not to be used. Stopcock grease is not to be used on ground-glass joints in this method.) F. A spectrophotometer equipped to automatically record absorbance of liquid samples in 1-centimeter pathlength cells in the spectral region of 280-400 mµ with a spectral slit width of 2 mµ or less. At an absorbance level of about 0.4, absorbance measurements shall be repeatable within ±0.01 and accurate within ±0.05. Wavelength measurements shall be repeatable with ±0.2 mµ and accurate within ±1.0 mµ. Instrument operating conditions are selected to realize this performance under dynamic (automatic) recording operations. Accuracy of absorbance measurements are determined at 290, 345, and 400 mµ, using potassium chromate as the reference standard. (National Bureau of Standards Circular 484, Spectrophotometry, U.S. Department of Commerce, 1949.) G. Two fused quartz cells having pathlengths of 1.00±0.005 centimeter or better. II. Purity of reagents and materials. Reagent-grade chemicals shall be used in all tests. It is further specified that each chemical shall be tested for purity in accordance with the instruction given under “Reagents and Materials” in III below. In addition, a blank run by the procedure shall be made on each purified lot of reagents and materials. Unless otherwise indicated, references to water shall be understood to mean distilled water. III. Reagents and materials— A. Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this section III. The isooctane, benzene, cyclohexane, nitromethane, and n -hexadecane designated shall pass the following test: To the specified quantity of solvent in a 150-milliliter beaker, add 1 milliliter of purified n -hexadecane and evaporate on the steam bath under a stream of nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains (to the residue from benzene and nitromethane add a 10-milliliter portion of purified isooctane, re-evaporate, and repeat once to insure complete removal of solvent). Dissolve the 1 milliliter of n -hexadecane residue in isooctane and make to 10-milliliter volume. Determine the absorbance in 1.0-centimeter pathlength cells compared to water as reference. The absorbance of the solution of solvent residue shall not exceed 0.05 between 280 and 400 mµ. 1. Isooctane ( 2,2,4-trimethylpentane ). Use 240 milliliters for the above test. Purify, if necessary, by passage through a column of activated silica gel. 2. Benzene. Use 200 milliliters for the above test. Purify, if necessary, by distillation or otherwise. 3. Cyclohexane. Use 70 milliliters for the above test. Purify, if necessary, by distillation, silica gel percolation, or otherwise. 4. Nitromethane. Use 125 milliliters for the above test. Purify, if necessary, by distillation or otherwise. 5. n-Hexadecane. Determine the absorbance on this solvent directly. Purify, if necessary, by silica gel percolation or otherwise. B. Other materials— 1. Pyrene standard reference. Pyrene, reagent grade, melting point range 150-152 °C. (Organic Chemical 3627, Eastman Kodak Co., Rochester, N.Y., or equivalent). The standard reference absorbance is the absorbance at 334 millimicrons of a standard reference solution of pyrene containing a concentration of 1.0 milligram per liter in purified isooctane measured against isooctane of the same spectral purity in 1.0-centimeter cells. (This absorbance will be approximately 0.28.) 2. Chrysene solution. Prepare a solution at a concentration of 5.0 milligrams per liter by dissolving 5.0 milligrams of chrysene in purified isooctane in a 1-liter volumetric flask. Adjust to volume with isooctane. 3. Nitrogen gas. Water pumped or equivalent purity, cylinder with regulator, and valve control flow at 5 p.s.i. 4. Silica gel. 100-200 mesh (Davison Chemical, Baltimore, Md., Grade 923, or equivalent), purified and activated by the following procedure: Place about 1 kilogram of silica gel in a large column and wash with contaminant-free benzene until a 200-milliliter sample of the benzene coming off the column will pass the ultraviolet absorption test for benzene. This test is performed as stipulated under “Organic solvents” in A under III above. When the silica gel has been sufficiently cleaned, activate the gel before use by placing the 1-kilogram batch in a shallow container in a layer no greater than 1 inch in depth and heating in an oven (Caution! Explosion Hazard) at 130 °C. for 16 hours, and store in a vacuum desiccator. Reheating about once a week is necessary if the silica gel is repeatedly removed from the desiccator. 5. Aluminum oxide ( Aluminum Co. of America, Grade F-20, or equivalent grade ). 80-200 mesh, purified and activated by the following procedure: Place about 1 kilogram of aluminum oxide in a large column and wash with contaminant-free benzene until a 200-milliliter sample of the benzene coming off the column will pass the ultraviolet absorption test for benzene. This test is performed as stipulated under “Organic solvents” in A under III above. (Caution! Remove Benzene From Adsorbent Under Vacuum To Minimize Explosion Hazard in Subsequent Heating!) When the aluminum oxide has been sufficiently cleaned and freed of solvent, activate it before use by placing the 1-kilogram batch in a shallow container in a layer no greater than 1 inch in depth. Heat in an oven at 130 °C for 16 hours. Upon removal from heat, store at atmospheric pressure over 80 percent (by weight) sulfuric acid in a desiccator for at least 36 hours before use. This gives aluminum oxide with between 6 to 9.5 percent volatiles. This is determined by heating a weighed sample of the prepared aluminum oxide at 2,000 °F for 2 hours and then quickly reweighing. To insure the proper adsorptive properties of the aluminum oxide, perform the following test: a. Weigh 50 grams ±1 gram of the activated aluminum oxide and pack into the chromatographic column (1.3 centimeters × 75 centimeters) described under “Apparatus” in C under I above. Use glass wool at the column exit to prevent the aluminum oxide from passing through the column. b. Place a 250-milliliter graduated cylinder under the column to measure the amount of eluate coming from the column. c. Prewet the aluminum oxide by passing 40 milliliters of isooctane through the column. Adjust the nitrogen pressure so that the rate of descent of the isooctane coming off the column is between 1.5 to 2.5 milliliters per minute. d. Just prior to the last of the isooctane reaching the top of the aluminum oxide bed, add 10 milliliters of the isooctane solution containing 5.0 milligrams of chrysene per liter. e. Continue percolation until the isooctane is just above the aluminum oxide. Then add 200 milliliters of a mixture of benzene and isooctane (33 1/3 percent benzene and 66 2/3 percent isooctane by volume) to the reservoir and continue percolation. f. Continue percolation, collecting the eluates (40 milliliters of the prewet solution, 10 milliliters of the sample solution, and 200 milliliters of the gradient solution) in the 250-milliliter graduated cylinder until the level of the gradient solution is just above the aluminum oxide. Add 200 milliliters of the eluting solution of benzene and isooctane (90 percent benzene and 10 percent isooctane by volume) to the column and continue collecting until a total of 250 milliliters of solution has been obtained. This may be discarded. Now begin to collect the final eluate. g. Place a 100-milliliter graduated cylinder under the column and continue the percolation until a 100-milliliter eluate has been obtained. h. Measure the amount of chrysene in this 100-milliliter fraction by ultraviolet analysis. If the aluminum oxide is satisfactory, more than 80 percent of the original amount of chrysene should be found in this fraction. ( Note: If the amount of chrysene recovered is less than 80 percent, the original batch of aluminum oxide should be sieved between 100-160 mesh. Activation and testing of this sieved batch should indicate a satisfactory aluminum oxide for use.) IV. Sampling. Precautions must be taken to insure that an uncontaminated sample of the mineral oil is obtained since ultraviolet absorption is very sensitive to small amounts of extraneous material contaminating the sample through careless handling. V. Procedure. A. Blank. Before proceeding with the analysis of a sample, determine the absorbance of the solvent residues by carrying out the procedure without a sample. B. Sample. 1. Weigh out 20.0 grams ±0.1 gram of the mineral oil into a beaker and transfer to a 250-milliliter separatory funnel fitted with a tetrafluoroethylene polymer stopcock, using enough cyclohexane (25 milliliters) to give a final total volume of 50 milliliters (mineral oil plus cyclohexane). 2. Add 25 milliliters of nitromethane saturated with cyclohexane and shake by hand vigorously for 3 minutes. Recover the lower nitromethane layer in a 150-milliliter beaker containing 1 milliliter of n -hexadecane and evaporate on the steam bath under nitrogen. Repeat the extraction four more times, recovering each extract in the 150-milliliter beaker. Exercise care not to fill the beaker to such a capacity that solvent losses may occur. Evaporate the combined nitromethane extracts to 1 milliliter of n -hexadecane residue containing the nitromethane-soluble mineral oil extractives. ( Note: Complete removal of the nitromethane is essential. This can be assured by two successive additions of 5 milliliters of isooctane and reevaporation.) 3. Remove the beaker from the steam bath and allow to cool. 4. Weigh 50 grams ±1 gram of activated aluminum oxide and pack into the chromatographic column (1.3 centimeters × 75 centimeters) described under “Apparatus” in C under I above. ( Note: A small plug of glass wool is placed at the column exit to prevent the aluminum oxide from passing through the column. After adding aluminum oxide, tap the column lightly to remove air voids. All percolations using aluminum oxide are performed under nitrogen pressure. The 500-milliliter reservoir described under “Apparatus” in E under I above is to be used to hold the elution solvents.) 5. Prewet the column by adding 40 milliliters of isooctane to the column. Adjust nitrogen pressure so that rate of descent of the isooctane coming off the column is 2.0 to 3.0 milliliters per minute. Be careful to maintain the level of solvent in the reservoir to prevent air from entering the aluminum oxide bed. New or additional solvent is added just before the last portion of the previous solvent enters the bed. To minimize possible photo-oxidation effects, the following procedures (steps 6 through 18) shall be carried out in subdued light. 6. Before the last of the isooctane reaches the top of the aluminum oxide bed, release the nitrogen pressure and turn off the stopcock on the column. Transfer the n -hexadecane residue from the 150-milliliter beaker from procedure step 3 above onto the column, using several washes of isooctane (total volume of washes should be no greater than 10-15 milliliters). 7. Open the stopcock and continue percolation until the isooctane is about 1 centimeter above the top of the aluminum oxide bed. Add 200 milliliters of isooctane to the reservoir, and continue the percolation at the specified rate. 8. Just before the isooctane surface reaches the top of the aluminum oxide bed, add 200 milliliters of a mixture of benzene and isooctane (33 1/3 percent benzene and 66 2/3 percent isooctane by volume) to the reservoir, and continue the percolation. 9. Just before the surface of this mixture reaches the top of the aluminum oxide bed, release the nitrogen pressure, turn off the stopcock, and discard all the elution solvents collected up to this point. 10. Add to the reservoir 300 milliliters of a mixture of benzene and isooctane (90 percent benzene and 10 percent isooctane by volume), place a 25-milliliter graduated cylinder under the column, continue the percolation until 20 milliliters of eluate has been collected, and then discard the eluate. 11. At this point, place a clean 250-milliliter Erlenmeyer flask under the column. Continue the percolation and collect all the remaining eluate. ( Note: Allow the column to drain completely. An increase in the nitrogen pressure may be necessary as the last of the solvent comes off the column.) 12. Place 1 milliliter of n -hexadecane into a 150-milliliter beaker. Place this onto a steam bath under a nitrogen stream and transfer in small portions the eluate from step 11 above. Wash out the Erlenmeyer flask with small amounts of benzene and transfer to the evaporation beaker. Evaporate until only 1 milliliter of hexadecane residue remains. ( Note: Complete removal of the benzene is essential. This can be assured by two successive additions of 5 milliliters of isooctane and reevaporation.) 13. Remove the beaker from the steam bath and cool. 14. Place a sample of 113.5 grams activated 100- 200-mesh silica gel in a 500-milliliter glass-stoppered Erlenmeyer flask. Add to the silica gel 46.2 grams (41 milliliters) of nitromethane. Stopper and shake the flask vigorously until no lumps of silica gel are observed and then shake occasionally during a period of 1 hour. The resultant nitromethane-treated silica gel is 29 weight-percent nitro-methane and 71 weight-percent silica gel. 15. Place a small plug of glass wool in the tapered end of the 1.7 centimeters outside diameter × 115 centimeters column, described under “Apparatus” in D of I above, adjacent to the stopcock to prevent silica gel from passing through the stopcock. Pack the nitromethane-treated silica gel into the column, tapping lightly. The resultant silica gel bed should be about 95 centimeters in depth. Place into a flask 170 milliliters of isooctane saturated with nitromethane. 16. Place a 100-milliliter graduated cylinder under the column and transfer the residue from the beaker in procedure step 13 above with several washes of the 170 milliliters of isooctane, saturated with nitromethane, onto the top of the column. (Total volume of washes should be no greater than 10 to 15 milliliters.) Permit isooctane solution to enter the silica gel bed until the liquid level is at the top bed level. Place the remaining amount of the 170 milliliters of isooctane, saturated with nitromethane, in the reservoir above the bed for percolation through the silica gel. Apply nitrogen pressure to the top of the column, adjusting the pressure so that the isooctane is collected at the rate of 2.5 to 3.5 milliliters per minute, and percolate isooctane through the bed until a quantity of 75.0 milliliters of eluate is collected. Discard the 75 milliliters of eluate. Turn off the stopcock and add 250 milliliters of benzene to the reservoir above the bed. Use a 400-milliliter beaker to collect the remaining eluate. 17. Open the stopcock, renew the pressure, and percolate the remaining isooctane and benzene through the column eluting the remaining aromatics. Transfer the eluate in small portions from the 400 milliliter beaker to a 150-milliliter beaker containing 1 milliliter of n -hexadecane and evaporate on the steam bath under nitrogen. Rinse the 400-milliliter beaker well with small portions of isooctane to obtain a complete transfer. ( Note: Complete removal of the nitromethane and benzene is essential. This can be assured by successive additions of 5 milliliters of isooctane and reevaporation.) 18. Transfer the residue with several washes of isooctane into a 200-milliliter volumetric flask. Add isooctane to mark. 19. Record the spectrum of the sample solution in a 1-centimeter cell compared to isooctane from 270 to 400 mµ. After making necessary corrections in the spectrum for cell differences and for the blank absorbance, record the maximum absorbance in each of the wavelength intervals (mµ), 280-299, 300-319, 320-359, 360-400. a. If the spectrum then shows no discernible peak corresponding to the absorbance maximum of the pyrene reference standard solution at 334 mµ, the maximum absorbances in the respective wavelength intervals recorded shall not exceed those prescribed in paragraph (d)(1)(ii) of this section. b. If such a peak is evident in the spectrum of the sample solution, and the spectrum as a whole is not incompatible with that of a pyrene contaminant yielding such a peak of the observed absorbance, calculate the concentration of pyrene that would yield this peak (334 m) by the base-line technique described in ASTM method E169-63 (Reapproved 1981), “Standard Recommended Practices for General Techniques of Ultraviolet Quantitative Analysis,” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (b)(1)(i) of this section. Correct each of the maximum absorbances in the respective specified wavelength intervals by subtracting the absorbance due to pyrene, determined as follows: where: Cp = Calculated concentration of pyrene in sample solution; Sp = Concentration of pyrene reference standard solution in same units of concentration; Sa = Absorbance of pyrene reference standard solution at wavelength of maximum absorbance of sample solution in the respective specified wavelength intervals. Also calculate the pyrene content of the oil sample in parts per million as follows: where: C = Calculated concentration of pyrene in milligrams per liter of sample solution. c. The pyrene content so determined shall not exceed 25 p.p.m. The maximum absorbances corrected for pyrene content as described in this step 19 for each of the specified wavelength intervals shall not exceed the limits prescribed in paragraph (d)(1)(ii) of this section. d. If the spectrum as a whole of the sample solution is in any respect clearly incompatible with the presence of pyrene as the source of the peak at 334 mµ, then the maximum absorbances in the respective wavelength intervals without correction for any assumed pyrene content shall not exceed the limits prescribed in paragraph (d)(1)(ii) of this section." 21:21:3.0.1.1.9.4.1.21,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3650 Odorless light petroleum hydrocarbons.,FDA,,,,"Odorless light petroleum hydrocarbons may be safely used, as a component of nonfood articles intended for use in contact with food, in accordance with the following prescribed conditions: (a) The additive is a mixture of liquid hydrocarbons derived from petroleum or synthesized from petroleum gases. The additive is chiefly paraffinic, isoparaffinic, or naphthenic in nature. (b) The additive meets the following specifications: (1) Odor is faint and not kerosenic. (2) Initial boiling point is 300 °F minimum. (3) Final boiling point is 650 °F maximum. (4) Ultraviolet absorbance limits determined by method specified in § 178.3620(b)(1)(ii), as follows: (c) The additive is used as follows:" 21:21:3.0.1.1.9.4.1.22,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3690 Pentaerythritol adipate-stearate.,FDA,,,"[45 FR 1018, Jan. 4, 1980, as amended at 47 FR 11848, Mar. 19, 1982; 49 FR 10112, Mar. 19, 1984; 54 FR 24898, June 12, 1989; 57 FR 18082, Apr. 29, 1992; 70 FR 40880, July 15, 2005; 70 FR 67651, Nov. 8, 2005]","Pentaerythritol adipate-stearate identified in paragraph (a) of this section may be safely used as a lubricant in the fabrication of rigid and semi-rigid polyvinyl chloride and/or vinyl chloride-propylene copolymers complying with § 177.1980 of this chapter used as articles or components of articles that contact food, excluding food with alcohol content greater than 8 percent under conditions of use of E, F, and G described in table 2 in § 175.300(d) of this chapter, subject to the provisions of this section. (a) Identity. For the purpose of this section, pentaerythritol adipate-stearate is an ester of pentaerythritol with adipic acid and stearic acid and its associated fatty acids (chiefly palmitic), with adipic acid comprising 14 percent and stearic acid and its associated acids (chiefly palmitic) comprising 71 percent of the organic moieties. (b) Specifications. Pentaerythritol adipate-stearate has the following specifications: (1) Melting point (dropping) of 55-58 °C as determined by ASTM method D566-76 (Reapproved 1982), “Standard Test Method for Dropping Point of Lubricating Grease,” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (2) Acid value not to exceed 15 as determined by ASTM method D1386-78, “Standard Test Method for Saponification Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), which is incorporated by reference. Copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (3) Saponification number of 270-280 as determined by ASTM method D1387-78, “Standard Test Method for Acid Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), which is incorporated by reference. Copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (4) Iodine number not to exceed 2 as determined by Iodine Absorption Number, Hanus Method, of the “Official Methods of Analysis of the Association of Official Analytical Chemists,” sections 28.018-28.019, 13th Ed. (1980), which is incorporated by reference. Copies may be obtained from the AOAC INTERNATIONAL, 481 North Frederick Ave., suite 500, Gaithersburg, MD 20877, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (c) The total amount of ester (calculated as free pentaerythritol) shall not exceed 0.4 percent by weight of the polyvinyl chloride and/or the vinyl chloride-propylene copolymers complying with § 177.1980." 21:21:3.0.1.1.9.4.1.23,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3700 Petrolatum.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 49 FR 10113, Mar. 19, 1984; 55 FR 12172, Apr. 2, 1990]","Petrolatum may be safety used as a component of nonfood articles in contact with food, in accordance with the following conditions: (a) Petrolatum complies with the specifications set forth in the United States Pharmacopeia XX (1980) for white petrolatum or in the National Formulary XV (1980) for yellow petrolatum. (b) Petrolatum meets the following ultraviolet absorbance limits when subjected to the analytical procedure described in § 172.886(b) of this chapter: Ultraviolet absorbance per centimeter pathlength: (c) It is used or intended for use as a protective coating of the surfaces of metal or wood tanks used in fermentation process, in an amount not in excess of that required to produce its intended effect. (d) Petrolatum as defined by this section may be used for the functions described and within the limitations prescribed by specific regulations in parts 175, 176, 177, and 178 of this chapter which prescribe uses of petrolatum. For the purpose of cross-reference, such specific regulations include: §§ 175.105, 175.125, 175.300, 176.170, 176.200, 176.210, 177.2600, 177.2800, and 178.3570 of this chapter. (e) Petrolatum may contain any antioxidant permitted in food by regulations issued pursuant to section 409 of the act, in an amount not greater than that required to produce its intended effect." 21:21:3.0.1.1.9.4.1.24,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3710 Petroleum wax.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 51 FR 19545, May 30, 1986]","Petroleum wax may be safely used as a component of nonfood articles in contact with food, in accordance with the following conditions: (a) Petroleum wax is a mixture of solid hydrocarbons, paraffinic in nature, derived from petroleum, and refined to meet the specifications prescribed in this section. (b) The petroleum wax meets the following ultraviolet absorbance limits when subjected to the analytical procedure described in § 172.886(b) of this chapter. Ultraviolet absorbance per centimeter pathlength: (c) Petroleum wax may contain any antioxidant permitted in food by regulations issued in accordance with section 409 of the act, in an amount not greater than that required to produce its intended effect. (d) Petroleum wax may contain a total of not more than 1 weight percent of residues of the following polymers when such residues result from use of the polymers as processing aids (filter aids) in the production of the petroleum wax: Homopolymers and/or copolymers derived from one or more of the mixed n -alkyl (C 12 , C 14 , C 16 , and C 18 ) methacrylate esters where the C 12 and C 14 alkyl groups are derived from coconut oil and the C 16 and C 18 groups are derived from tallow. (e) Petroleum wax may contain 2-hydroxy-4- n -octoxybenzophenone as a stabilizer at a level not to exceed 0.01 weight percent of the petroleum wax. (f) Petroleum wax may contain poly(alkylacrylate) (CAS Reg. No. 27029-57-8), as described in § 172.886(c)(2) of this chapter, as a processing aid in the manufacture of petroleum wax." 21:21:3.0.1.1.9.4.1.25,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3720 Petroleum wax, synthetic.",FDA,,,,"Synthetic petroleum wax may be safely used in applications and under the same conditions where naturally derived petroleum wax is permitted in subchapter B of this chapter as a component of articles intended to contact food, provided that the synthetic petroleum wax meets the definition and specifications prescribed in § 172.888 of this chapter." 21:21:3.0.1.1.9.4.1.26,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3725 Pigment dispersants.,FDA,,,"[61 FR 43157, Aug. 21, 1996, as amended at 63 FR 35799, July 1, 1998; 64 FR 48292, Sept. 3, 1999; 64 FR 72273, Dec. 27, 1999; 65 FR 52909, Aug. 31, 2000]","Subject to the provisions of this regulation, the substances listed in this section may be safely used as pigment dispersants in food-contact materials." 21:21:3.0.1.1.9.4.1.27,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3730 Piperonyl butoxide and pyrethrins as components of bags.,FDA,,,"[85 FR 72907, Nov. 16, 2020]",Piperonyl butoxide in combination with pyrethrins may be safely used for insect control on bags that are intended for use in contact with dried feed or dried food in compliance with 40 CFR 180.127 and 40 CFR 180.128. 21:21:3.0.1.1.9.4.1.28,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3740 Plasticizers in polymeric substances.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 42 FR 44223, Sept. 2, 1977; 45 FR 56052, Aug. 22, 1980; 48 FR 5748, Feb. 15, 1984; 49 FR 10113, Mar. 19, 1984; 51 FR 47011, Dec. 30, 1986; 87 FR 31089, May 20, 2022]","Subject to the provisions of this regulation, the substances listed in paragraph (b) of this section may be safely used as plasticizers in polymeric substances used in the manufacture of articles or components of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food. (a) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect. (b) List of substances: (c) The use of the plasticizers in any polymeric substance or article subject to any regulation in parts 174, 175, 176, 177, 178 and 179 of this chapter must comply with any specifications and limitations prescribed by such regulation for the finished form of the substance or article." 21:21:3.0.1.1.9.4.1.29,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3750 Polyethylene glycol (mean molecular weight 200-9,500).",FDA,,,,"Polyethylene glycol identified in this section may be safely used as a component of articles intended for use in contact with food, in accordance with the following prescribed conditions: (a) The additive is an addition polymer of ethylene oxide and water with a mean molecular weight of 200 to 9,500. (b) It contains no more than 0.2 percent total by weight of ethylene and diethylene glycols if its mean molecular weight is 350 or higher and no more than 0.5 percent total by weight of ethylene and diethylene glycols if its mean molecular weight is below 350, when tested by the analytical methods prescribed in § 172.820(b) of this chapter. (c) The provisions of paragraph (b) of this section are not applicable to polyethylene glycols used in food-packaging adhesives complying with § 175.105 of this chapter." 21:21:3.0.1.1.9.4.1.3,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3125 Anticorrosive agents.,FDA,,,"[50 FR 21835, May 29, 1985]",The substances listed in this section may be used as anticorrosive agents in food-contact materials subject to the provisions of this section: 21:21:3.0.1.1.9.4.1.30,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3760 Polyethylene glycol (400) monolaurate.,FDA,,,,Polyethylene glycol (400) monolaurate containing not more than 0.1 percent by weight of ethylene and/or diethylene glycol may be used at a level not to exceed 0.3 percent by weight of twine as a finish on twine to be used for tying meat provided the twine fibers are produced from nylon resins complying with § 177.1500 of this chapter. 21:21:3.0.1.1.9.4.1.31,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3770 Polyhydric alcohol esters of oxidatively refined (Gersthofen process) montan wax acids.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11848, Mar. 19, 1982; 49 FR 10113, Mar. 19, 1984; 51 FR 33895, Sept. 24, 1986; 54 FR 24898, June 12, 1989; 55 FR 28020, July 9, 1990; 58 FR 17512, Apr. 5, 1993; 69 FR 24512, May 4, 2004]","Polyhydric alcohol esters of oxidatively refined (Gersthofen process) montan wax acids identified in this section may be safely used as components of articles intended for use in contact with food in accordance with the following prescribed conditions: (a) The polyhydric alcohol esters identified in this paragraph may be used as lubricants in the fabrication of vinyl chloride plastic food-contact articles prepared from polyvinyl chloride and/or from vinyl chloride copolymers complying with § 177.1980 of this chapter. Such esters meet the following specifications and are produced by partial esterification of oxidatively refined (Gersthofen process) montan wax acids by either ethylene glycol or 1,3-butanediol with or without neutralization of unreacted carboxylic groups with calcium hydroxide: (1) Dropping point 76°-105 °C, as determined by ASTM method D566-76 (Reapproved 1982), “Standard Test Method for Dropping Point of Lubricating Grease,” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (2) Acid value 10-20, as determined by ASTM method D1386-78 (“Standard Test Method for Acid Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), which is incorporated by reference; copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. ) using as solvent xylene-ethyl alcohol in a 2:1 ratio instead of toluene-ethyl alcohol in a 2:1 ratio. (3) Saponification value 100-160, as determined by ASTM method D1387-78 (“Standard Test Method for Saponification Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), which is incorporated by reference; copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. ) using xylene-ethyl alcohol in a 2:1 ratio instead of ethyl alcohol in preparation of potassium hydroxide solution. (4) Ultraviolet absorbance limits as follows, as determined by the analytical method described in this subparagraph: Ultraviolet absorbance per centimeter pathlength. Analytical Method general instructions Because of the sensitivity of the test, the possibility of errors arising from contamination is great. It is of the greatest importance that all glassware be scrupulously cleaned to remove all organic matter such as oil, grease, detergent residues, etc. Examine all glassware, including stoppers and stopcocks, under ultraviolet light to detect any residual fluorescent contamination. As a precautionary measure it is recommended practice to rinse all glassware with purified isooctane immediately before use. No grease is to be used on stopcocks or joints. Great care to avoid contamination of wax samples in handling and to assure absence of any extraneous material arising from inadequate packaging is essential. Because some of the polynuclear hydrocarbons sought in this test are very susceptible to photo-oxidation, the entire procedure is to be carried out under subdued light. apparatus Separatory funnels. 250-milliliter, 500-milliliter, 1,000-milliliter, and preferably 2,000-milliliter capacity, equipped with tetrafluoroethylene polymer stopcocks. Reservoir. 1,000-milliliter capacity, equipped with a 24/40 standard taper male fitting at the bottom and a suitable balljoint at the top. Chromatographic tube. 1,200 millimeters in length, inside diameter to be 16.5 millimeters ±0.5 millimeter, equipped with a coarse, fritted-glass disc, a tetrafluoroethylene polymer stopcock, and a female 24/40 standard tapered fitting at the opposite end. (Overall length of the column with the female joint is 1,255 millimeters.) The female fitting should be equipped with glass hooks. Disc. Tetrafluoroethylene polymer 2-inch diameter disc approximately 3/16 -inch thick with a hole bored in the center to closely fit the stem of the chromatographic tube. Heating jackets. Conical, for 500-milliliter and 1,000-milliliter separatory funnels. (Used with variable transformer heat control.) Suction flask. 250-milliliter or 500-milliliter filter flask. Condenser. 24/40 joints, fitted with a drying tube, length optional. Evaporation flasks ( optional ). A 250-milliliter or 500-milliliter capacity and a 1-liter capacity all-glass flask equipped with standard taper stopper having inlet and outlet tubes to permit passage of nitrogen across the surface of contained liquid to be evaporated. Vacuum distillation assembly. All glass (for purification of dimethyl sulfoxide) 2-liter distillation flask with heating mantle; Vigreaux vacuum-jacketed condenser (or equivalent) about 45 centimeters in length and distilling head with separable cold finger condenser. Use of tetrafluoroethylene polymer sleeves on the glass joints will prevent freezing. Do not use grease on stopcocks or joints. Oil bath. Capable of heating to 90 °C. Spectrophotometric cells. Fused quartz cells, optical pathlength in the range 1.000 centimeter ±0.005 centimeter. With distilled water in the cells, determine any absorbance differences. Spectrophotometer. Spectral range 250 millimicrons-400 millimicrons with spectral slit width of 0.2 millimicron or less; under instrument operating conditions for these absorbance measurements. The spectrophotometer shall also meet the following performance requirements: Absorbance repeatability, ±0.01 at 0.4 absorbance. Absorbance accuracy, 1 ±0.05 at 0.4 absorbance. 1 As determined by procedure using potassium chromate for reference standard and described in National Bureau of Standards Circular 484, Spectrometry, U.S. Department of Commerce (1949). The accuracy is to be determined by comparison with the standard values at 290, 345, and 400 millimicrons. Circular 484 is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Wavelength repeatability, ±0.2 millimicron. Wavelength accuracy, ±1.0 millimicron. Recording time, 50 seconds. Time constant, 0.6 second. Sensitivity, 30. Ordinate scale, 90-100 percent transmission through scale. Abscissa scale, 8X. Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in cylinder equipped with regulator and valve to control flow at 5 p.s.i.g. reagents and materials Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this specification. The isooctane and benzene designated in the list following this paragraph shall pass the following test: To be specified quantity of solvent in a 250-milliliter Erlenmeyer flask, add 1 milliliter of purified n -hexadecane and evaporate on the steam bath under a stream of nitrogen (a loose aluminum foil jacket around the flask will speed evaporation). Discontinue evaporation when not over 1 milliliter of residue remains. (To the residue from benzene add a 10-milliliter portion of purified isooctane, reevaporate, and repeat once to insure complete removal of benzene.) Alternatively, the evaporation time can be reduced by using the optional evaporation flask. In this case the solvent and n -hexadecane are placed in the flask on the steam bath, the tube assembly is inserted, and a stream of nitrogen is fed through the inlet tube while the outlet tube is connected to a solvent trap and vacuum line in such a way as to prevent any flow-back of condensate into the flask. Dissolve the 1 milliliter of hexadecane residue in isooctane and make up to 25 milliliters volume. Determine the absorbance in the 1-centimeter pathlength cells compared to isooctane as reference. The absorbance of the solution of the solvent residue (except for methyl alcohol) shall not exceed 0.01 per centimeter pathlength between 280 mµ and 400 mµ. Isooctane ( 2,2,4-trimethylpentane ). Use 180 milliliters for the test described in the preceding paragraph. Purify, if necessary, by passage through a column of activated silica gel (Grade 12, Davison Chemical Co., Baltimore, Md., or equivalent) about 90 centimeters in length and 5 centimeters to 8 centimeters in diameter. Benzene, A.C.S. reagent grade. Use 150 milliliters for the test. Purify, if necessary, by distillation or otherwise. n-Hexadecane, 99 percent olefin-free. Dilute 1.0 milliliter of n -hexadecane to 25 milliliters with isooctane and determine the absorbance in a 1-centimeter cell compared to isooctane as reference point between 280 mµ-400 mµ. The absorbance per centimeter pathlength shall not exceed 0.00 in this range. If necessary, purify by filtering through a column containing 100 grams of aluminum oxide (use same grade as described below) in the lower half and 100 grams of activated silica gel in the upper half keeping the column at 150 °C., for a period of 15 hours or overnight. The first 100 milliliters of eluate are used. Purification can also be accomplished by distillation. Dimethyl sulfoxide. Pure grade, clear, water-white, m.p. 18° minimum. Dilute 120 milliliters of dimethyl sulfoxide with 240 milliliters of distilled water in a 500-milliliter separatory funnel, mix and allow to cool for 5-10 minutes. Add 40 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second 500-milliliter separatory funnel and repeat the extraction with 40 milliliters of isooctane. Draw off and discard the aqueous layer. Wash each of the 40-milliliter extractives three times with 50-milliliter portions of distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate prewashed with isooctane (see Sodium sulfate under “Reagents and materials” for preparation of filter), into a 250-milliliter Erlenmeyer flask, or optionally into the evaporating flask. Wash the first separatory funnel with the second 40-milliliter isooctane extractive, and pass through the sodium sulfate into the flask. Then wash the second and first separatory funnels successively with a 10-milliliter portion of isooctane, and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane on the steam bath under nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane and reevaporate to 1 milliliter of hexadecane. Again, add 10 milliliters of isooctane to the residue and evaporate to 1 milliliter of hexadecane to insure complete removal of all volatile materials. Dissolve the 1 milliliter of hexadecane in isooctane and make to 25-milliliter volume. Determine the absorbance in 1-centimeter pathlength cells compared to isooctane as reference. The absorbance of the solution should not exceed 0.02 per centimeter pathlength in the 280 mµ-400 mµ range. ( Note: Difficulty in meeting this absorbance specification may be due to organic impurities in the distilled water. Repetition of the test omitting the dimethyl sulfoxide will disclose their presence. If necessary to meet the specification, purify the water by redistillation, passage through an ion-exchange resin, or otherwise.) Purify, if necessary, by the following procedure: To 1,500 milliliters of dimethyl sulfoxide in a 2-liter glass-stoppered flask, add 6.0 milliliters of phosphoric acid and 50 grams of Norit A (decolorizing carbon, alkaline) or equivalent. Stopper the flask, and with the use of a magnetic stirrer (tetrafluoroethylene polymer coated bar) stir the solvent for 15 minutes. Filter the dimethyl sulfoxide through four thicknesses of fluted paper (18.5 centimeters, Schleicher & Schuell, No. 597, or equivalent). If the initial filtrate contains carbon fines, refilter through the same filter until a clear filtrate is obtained. Protect the sulfoxide from air and moisture during this operation by covering the solvent in the funnel and collection flask with a layer of isooctane. Transfer the filtrate to a 2-liter separatory funnel and draw off the dimethyl sulfoxide into the 2-liter distillation flask of the vacuum distillation assembly and distill at approximately 3-millimeter Hg pressure or less. Discard the first 200-milliliter fraction of the distillate and replace the distillate collection flask with a clean one. Continue the distillation until approximately 1 liter of the sulfoxide has been collected. At completion of the distillation, the reagent should be stored in glass-stoppered bottles since it is very hygroscopic and will react with some metal containers in the presence of air. Phosphoric acid. 85 percent A.C.S. reagent grade. Aluminum oxide ( 80-200 mesh Woelm neutral activity grade 1 [ Brockmann ], Alupharm Chemicals, New Orleans, La., or equivalent ). Pipette 1 milliliter of distilled water into a dry 250-milliliter Erlenmeyer flask equipped with a ground-glass stopper. Stopper the flask and rotate it in such a manner as to completely wet out the inside surfaces. When this has been done add 180 grams of the aluminum oxide and shake until no lumps or wet spots remain. Allow to stand at room temperature for a period of 2 hours. At the end of this time the water should be evenly distributed throughout the aluminum oxide powder, and it should have the same free flowing properties as the original material (flow velocity with water 0.2 milliliter per minute). At this point the aluminum oxide has an activity of 1 as expressed in Brockmann degrees, and the amount of added water is 0.5 percent by volume. This product is used in toto and as is, without further screening. Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in granular form. For each bottle of sodium sulfate reagent used, establish as follows the necessary sodium sulfate prewash to provide such filters required in the method: Place approximately 35 grams of anhydrous sodium sulfate in a 30-milliliter coarse, fritted-glass funnel or in a 65-millimeter filter funnel with glass wool plug; wash with successive 15-milliliter portions of the indicated solvent until a 15-milliliter portion of the wash shows 0.00 absorbance per centimeter pathlength between 280 mµ and 400 mµ when tested as prescribed under “Organic solvents.” Usually three portions of wash solvent are sufficient. procedure Before proceeding with analysis of a sample, determine the absorbance in a 1-centimeter path cell between 250 mµ and 400 mµ for the reagent blank by carrying out the procedure, without a wax sample, at room temperature, recording the spectrum after the complete procedure as prescribed. The absorbance per centimeter pathlength following the complete procedure should not exceed 0.04 in the wavelength range from 280 mµ to 299 mµ, inclusive, nor 0.02 in the wavelength range from 300 mµ to 400 mµ. If in either spectrum the characteristic benzene peaks in the 250 mµ-260 mµ region are present, remove the benzene by the procedure under “Organic solvents” and record absorbance again. Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory funnel and add 75 milliliters of phosphoric acid. Mix the contents of the funnel and allow to stand for 10 minutes. (The reaction between the sulfoxide and the acid is exothermic. Release pressure after mixing, then keep funnel stoppered.) Add 150 milliliters of isooctane and shake to preequilibrate the solvents. Draw off the individual layers and store in glass-stoppered flasks. In a 1-liter separatory funnel place a representative 25-gram sample of wax, add 50 milliliters of isooctane, heat gently, stir until the wax is in solution; add 100 milliliters of preequilibrated sulfoxide-phosphoric acid mixture and shake, making sure it remains in solution. If the wax comes out of solution during these operations, let the stoppered funnel remain in the jacket until the wax redissolves. (Remove stopper from the funnel at intervals to release pressure.) When the wax is in solution, remove the funnel from the jacket and shake it vigorously for 2 minutes. Set up three 250-milliliter separatory funnels with each containing 30 milliliters of preequilibrated isooctane. After separation of the liquid phases, allow to cool until the main portion of the wax-isooctane solution begins to show a precipitate. Gently swirl the funnel when precipitation first occurs on the inside surface of the funnel to accelerate this process. Carefully draw off the lower layer, filter it slowly through a thin layer of glass wool fitted loosely in a filter funnel into the first 250-milliliter separatory funnel, and wash in tandem with the 30-milliliter portions of isooctane contained in the 250-milliliter separatory funnels. Shaking time for each wash is 1 minute. Repeat the extraction operation with two additional portions of the sulfoxide-acid mixture, replacing the funnel in the jacket after each extraction to keep the wax in solution and washing each extractive in tandem through the same three portions of isooctane. Collect the successive extractives (300 milliliters total) in a separatory funnel (preferably 2-liter), containing 480 milliliters of distilled water, mix, and allow to cool for a few minutes after the last extractive has been added. Add 80 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second separatory funnel (preferably 2-liter) and repeat the extraction with 80 milliliters of isooctane. Draw off and discard the aqueous layer. Wash each of the 80-milliliter extractives three times with 100-milliliter portions of distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate prewashed with isooctane (see Sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the first separatory funnel with the second 80-milliliter isooctane extractive and pass through the sodium sulfate. Then wash the second and first separatory funnels successively with a 20-milliliter portion of isooctane and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane using an aspirator vacuum under nitrogen and in an oil bath temperature of approximately 90 °C. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane, reevaporate to 1 milliliter of hexadecane, and repeat this operation once. Reserve the residue for column chromatography on the aluminum oxide. Fit the tetrafluoroethylene polymer disc on the upper part of the stem of the chromatographic tube, then place the tube with the disc on the suction flask and apply the vacuum (approximately 135 millimeters Hg pressure). Weigh out 180 grams of the aluminum oxide and pour the adsorbent mixture into the chromatographic tube in approximately 30-centimeter layers. After the addition of each layer, level off the top of the adsorbent with a flat glass rod or metal plunger by pressing down firmly until the adsorbent is well packed. Loosen the topmost few millimeters of each adsorbent layer with the end of a metal rod before the addition of the next layer. Continue packing in this manner until all the 180 grams of the adsorbent is added to the tube. Level off the top of the adsorbent by pressing down firmly with a flat glass rod or metal plunger to make the depth of the adsorbent bed approximately 80 centimeters in depth. Turn off the vacuum and remove the suction flask. Dissolve the hexadecane residue in 10 milliliters of warm benzene and decant the solution onto the column and allow the liquid level to recede to barely above the adsorbent level. Rapidly complete the transfer similarly with two 10-milliliter portions of benzene swirling the flask repeatedly each time to assure adequate washing of the residue. Fix the 1,000-milliliter reservoir onto the top of the chromatographic column. Just before the final 10-milliliter wash reaches the top of the adsorbent, add 670 milliliters of benzene to the reservoir and continue the percolation at the 2-3 milliliter per minute rate until a total of 670 milliliters of benzene has been utilized. Collect the eluate in a clean 1-liter Erlenmeyer flask (or optionally into a 1-liter evaporation flask). Allow the column to drain until most of the solvent mixture is removed. Add 1 milliliter of n -hexadecane and completely remove the benzene by evaporation under nitrogen, using the special procedure to eliminate benzene as previously described under “Organic Solvents.” Quantitatively transfer the residue with isooctane to a 25-milliliter volumetric flask and adjust to volume. Determine the absorbance of the solution in the 1-centimeter pathlength cells compared to isooctane as reference between 250 mµ-400 mµ. Correct for any absorbance derived from the reagents as determined by carrying out the procedure without a wax sample. If either spectrum shows the characteristic benzene peaks in the 250 mµ-260 mµ region, evaporate the solution to remove benzene by the procedure under “Organic Solvents.” Dissolve the residue, transfer quantitatively, and adjust to volume in isooctane in a 25-milliliter volumetric flask. Record the absorbance again. If the corrected absorbance does not exceed the limits prescribed in paragraph (a) of this section, the wax meets the ultraviolet absorbance specifications. Because of the sensitivity of the test, the possibility of errors arising from contamination is great. It is of the greatest importance that all glassware be scrupulously cleaned to remove all organic matter such as oil, grease, detergent residues, etc. Examine all glassware, including stoppers and stopcocks, under ultraviolet light to detect any residual fluorescent contamination. As a precautionary measure it is recommended practice to rinse all glassware with purified isooctane immediately before use. No grease is to be used on stopcocks or joints. Great care to avoid contamination of wax samples in handling and to assure absence of any extraneous material arising from inadequate packaging is essential. Because some of the polynuclear hydrocarbons sought in this test are very susceptible to photo-oxidation, the entire procedure is to be carried out under subdued light. Separatory funnels. 250-milliliter, 500-milliliter, 1,000-milliliter, and preferably 2,000-milliliter capacity, equipped with tetrafluoroethylene polymer stopcocks. Reservoir. 1,000-milliliter capacity, equipped with a 24/40 standard taper male fitting at the bottom and a suitable balljoint at the top. Chromatographic tube. 1,200 millimeters in length, inside diameter to be 16.5 millimeters ±0.5 millimeter, equipped with a coarse, fritted-glass disc, a tetrafluoroethylene polymer stopcock, and a female 24/40 standard tapered fitting at the opposite end. (Overall length of the column with the female joint is 1,255 millimeters.) The female fitting should be equipped with glass hooks. Disc. Tetrafluoroethylene polymer 2-inch diameter disc approximately 3/16 -inch thick with a hole bored in the center to closely fit the stem of the chromatographic tube. Heating jackets. Conical, for 500-milliliter and 1,000-milliliter separatory funnels. (Used with variable transformer heat control.) Suction flask. 250-milliliter or 500-milliliter filter flask. Condenser. 24/40 joints, fitted with a drying tube, length optional. Evaporation flasks ( optional ). A 250-milliliter or 500-milliliter capacity and a 1-liter capacity all-glass flask equipped with standard taper stopper having inlet and outlet tubes to permit passage of nitrogen across the surface of contained liquid to be evaporated. Vacuum distillation assembly. All glass (for purification of dimethyl sulfoxide) 2-liter distillation flask with heating mantle; Vigreaux vacuum-jacketed condenser (or equivalent) about 45 centimeters in length and distilling head with separable cold finger condenser. Use of tetrafluoroethylene polymer sleeves on the glass joints will prevent freezing. Do not use grease on stopcocks or joints. Oil bath. Capable of heating to 90 °C. Spectrophotometric cells. Fused quartz cells, optical pathlength in the range 1.000 centimeter ±0.005 centimeter. With distilled water in the cells, determine any absorbance differences. Spectrophotometer. Spectral range 250 millimicrons-400 millimicrons with spectral slit width of 0.2 millimicron or less; under instrument operating conditions for these absorbance measurements. The spectrophotometer shall also meet the following performance requirements: Absorbance repeatability, ±0.01 at 0.4 absorbance. Absorbance accuracy, 1 ±0.05 at 0.4 absorbance. 1 As determined by procedure using potassium chromate for reference standard and described in National Bureau of Standards Circular 484, Spectrometry, U.S. Department of Commerce (1949). The accuracy is to be determined by comparison with the standard values at 290, 345, and 400 millimicrons. Circular 484 is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Wavelength repeatability, ±0.2 millimicron. Wavelength accuracy, ±1.0 millimicron. Recording time, 50 seconds. Time constant, 0.6 second. Sensitivity, 30. Ordinate scale, 90-100 percent transmission through scale. Abscissa scale, 8X. Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in cylinder equipped with regulator and valve to control flow at 5 p.s.i.g. Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this specification. The isooctane and benzene designated in the list following this paragraph shall pass the following test: To be specified quantity of solvent in a 250-milliliter Erlenmeyer flask, add 1 milliliter of purified n -hexadecane and evaporate on the steam bath under a stream of nitrogen (a loose aluminum foil jacket around the flask will speed evaporation). Discontinue evaporation when not over 1 milliliter of residue remains. (To the residue from benzene add a 10-milliliter portion of purified isooctane, reevaporate, and repeat once to insure complete removal of benzene.) Alternatively, the evaporation time can be reduced by using the optional evaporation flask. In this case the solvent and n -hexadecane are placed in the flask on the steam bath, the tube assembly is inserted, and a stream of nitrogen is fed through the inlet tube while the outlet tube is connected to a solvent trap and vacuum line in such a way as to prevent any flow-back of condensate into the flask. Dissolve the 1 milliliter of hexadecane residue in isooctane and make up to 25 milliliters volume. Determine the absorbance in the 1-centimeter pathlength cells compared to isooctane as reference. The absorbance of the solution of the solvent residue (except for methyl alcohol) shall not exceed 0.01 per centimeter pathlength between 280 mµ and 400 mµ. Isooctane ( 2,2,4-trimethylpentane ). Use 180 milliliters for the test described in the preceding paragraph. Purify, if necessary, by passage through a column of activated silica gel (Grade 12, Davison Chemical Co., Baltimore, Md., or equivalent) about 90 centimeters in length and 5 centimeters to 8 centimeters in diameter. Benzene, A.C.S. reagent grade. Use 150 milliliters for the test. Purify, if necessary, by distillation or otherwise. n-Hexadecane, 99 percent olefin-free. Dilute 1.0 milliliter of n -hexadecane to 25 milliliters with isooctane and determine the absorbance in a 1-centimeter cell compared to isooctane as reference point between 280 mµ-400 mµ. The absorbance per centimeter pathlength shall not exceed 0.00 in this range. If necessary, purify by filtering through a column containing 100 grams of aluminum oxide (use same grade as described below) in the lower half and 100 grams of activated silica gel in the upper half keeping the column at 150 °C., for a period of 15 hours or overnight. The first 100 milliliters of eluate are used. Purification can also be accomplished by distillation. Dimethyl sulfoxide. Pure grade, clear, water-white, m.p. 18° minimum. Dilute 120 milliliters of dimethyl sulfoxide with 240 milliliters of distilled water in a 500-milliliter separatory funnel, mix and allow to cool for 5-10 minutes. Add 40 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second 500-milliliter separatory funnel and repeat the extraction with 40 milliliters of isooctane. Draw off and discard the aqueous layer. Wash each of the 40-milliliter extractives three times with 50-milliliter portions of distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate prewashed with isooctane (see Sodium sulfate under “Reagents and materials” for preparation of filter), into a 250-milliliter Erlenmeyer flask, or optionally into the evaporating flask. Wash the first separatory funnel with the second 40-milliliter isooctane extractive, and pass through the sodium sulfate into the flask. Then wash the second and first separatory funnels successively with a 10-milliliter portion of isooctane, and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane on the steam bath under nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane and reevaporate to 1 milliliter of hexadecane. Again, add 10 milliliters of isooctane to the residue and evaporate to 1 milliliter of hexadecane to insure complete removal of all volatile materials. Dissolve the 1 milliliter of hexadecane in isooctane and make to 25-milliliter volume. Determine the absorbance in 1-centimeter pathlength cells compared to isooctane as reference. The absorbance of the solution should not exceed 0.02 per centimeter pathlength in the 280 mµ-400 mµ range. ( Note: Difficulty in meeting this absorbance specification may be due to organic impurities in the distilled water. Repetition of the test omitting the dimethyl sulfoxide will disclose their presence. If necessary to meet the specification, purify the water by redistillation, passage through an ion-exchange resin, or otherwise.) Purify, if necessary, by the following procedure: To 1,500 milliliters of dimethyl sulfoxide in a 2-liter glass-stoppered flask, add 6.0 milliliters of phosphoric acid and 50 grams of Norit A (decolorizing carbon, alkaline) or equivalent. Stopper the flask, and with the use of a magnetic stirrer (tetrafluoroethylene polymer coated bar) stir the solvent for 15 minutes. Filter the dimethyl sulfoxide through four thicknesses of fluted paper (18.5 centimeters, Schleicher & Schuell, No. 597, or equivalent). If the initial filtrate contains carbon fines, refilter through the same filter until a clear filtrate is obtained. Protect the sulfoxide from air and moisture during this operation by covering the solvent in the funnel and collection flask with a layer of isooctane. Transfer the filtrate to a 2-liter separatory funnel and draw off the dimethyl sulfoxide into the 2-liter distillation flask of the vacuum distillation assembly and distill at approximately 3-millimeter Hg pressure or less. Discard the first 200-milliliter fraction of the distillate and replace the distillate collection flask with a clean one. Continue the distillation until approximately 1 liter of the sulfoxide has been collected. At completion of the distillation, the reagent should be stored in glass-stoppered bottles since it is very hygroscopic and will react with some metal containers in the presence of air. Phosphoric acid. 85 percent A.C.S. reagent grade. Aluminum oxide ( 80-200 mesh Woelm neutral activity grade 1 [ Brockmann ], Alupharm Chemicals, New Orleans, La., or equivalent ). Pipette 1 milliliter of distilled water into a dry 250-milliliter Erlenmeyer flask equipped with a ground-glass stopper. Stopper the flask and rotate it in such a manner as to completely wet out the inside surfaces. When this has been done add 180 grams of the aluminum oxide and shake until no lumps or wet spots remain. Allow to stand at room temperature for a period of 2 hours. At the end of this time the water should be evenly distributed throughout the aluminum oxide powder, and it should have the same free flowing properties as the original material (flow velocity with water 0.2 milliliter per minute). At this point the aluminum oxide has an activity of 1 as expressed in Brockmann degrees, and the amount of added water is 0.5 percent by volume. This product is used in toto and as is, without further screening. Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in granular form. For each bottle of sodium sulfate reagent used, establish as follows the necessary sodium sulfate prewash to provide such filters required in the method: Place approximately 35 grams of anhydrous sodium sulfate in a 30-milliliter coarse, fritted-glass funnel or in a 65-millimeter filter funnel with glass wool plug; wash with successive 15-milliliter portions of the indicated solvent until a 15-milliliter portion of the wash shows 0.00 absorbance per centimeter pathlength between 280 mµ and 400 mµ when tested as prescribed under “Organic solvents.” Usually three portions of wash solvent are sufficient. Before proceeding with analysis of a sample, determine the absorbance in a 1-centimeter path cell between 250 mµ and 400 mµ for the reagent blank by carrying out the procedure, without a wax sample, at room temperature, recording the spectrum after the complete procedure as prescribed. The absorbance per centimeter pathlength following the complete procedure should not exceed 0.04 in the wavelength range from 280 mµ to 299 mµ, inclusive, nor 0.02 in the wavelength range from 300 mµ to 400 mµ. If in either spectrum the characteristic benzene peaks in the 250 mµ-260 mµ region are present, remove the benzene by the procedure under “Organic solvents” and record absorbance again. Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory funnel and add 75 milliliters of phosphoric acid. Mix the contents of the funnel and allow to stand for 10 minutes. (The reaction between the sulfoxide and the acid is exothermic. Release pressure after mixing, then keep funnel stoppered.) Add 150 milliliters of isooctane and shake to preequilibrate the solvents. Draw off the individual layers and store in glass-stoppered flasks. In a 1-liter separatory funnel place a representative 25-gram sample of wax, add 50 milliliters of isooctane, heat gently, stir until the wax is in solution; add 100 milliliters of preequilibrated sulfoxide-phosphoric acid mixture and shake, making sure it remains in solution. If the wax comes out of solution during these operations, let the stoppered funnel remain in the jacket until the wax redissolves. (Remove stopper from the funnel at intervals to release pressure.) When the wax is in solution, remove the funnel from the jacket and shake it vigorously for 2 minutes. Set up three 250-milliliter separatory funnels with each containing 30 milliliters of preequilibrated isooctane. After separation of the liquid phases, allow to cool until the main portion of the wax-isooctane solution begins to show a precipitate. Gently swirl the funnel when precipitation first occurs on the inside surface of the funnel to accelerate this process. Carefully draw off the lower layer, filter it slowly through a thin layer of glass wool fitted loosely in a filter funnel into the first 250-milliliter separatory funnel, and wash in tandem with the 30-milliliter portions of isooctane contained in the 250-milliliter separatory funnels. Shaking time for each wash is 1 minute. Repeat the extraction operation with two additional portions of the sulfoxide-acid mixture, replacing the funnel in the jacket after each extraction to keep the wax in solution and washing each extractive in tandem through the same three portions of isooctane. Collect the successive extractives (300 milliliters total) in a separatory funnel (preferably 2-liter), containing 480 milliliters of distilled water, mix, and allow to cool for a few minutes after the last extractive has been added. Add 80 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second separatory funnel (preferably 2-liter) and repeat the extraction with 80 milliliters of isooctane. Draw off and discard the aqueous layer. Wash each of the 80-milliliter extractives three times with 100-milliliter portions of distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate prewashed with isooctane (see Sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the first separatory funnel with the second 80-milliliter isooctane extractive and pass through the sodium sulfate. Then wash the second and first separatory funnels successively with a 20-milliliter portion of isooctane and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane using an aspirator vacuum under nitrogen and in an oil bath temperature of approximately 90 °C. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane, reevaporate to 1 milliliter of hexadecane, and repeat this operation once. Reserve the residue for column chromatography on the aluminum oxide. Fit the tetrafluoroethylene polymer disc on the upper part of the stem of the chromatographic tube, then place the tube with the disc on the suction flask and apply the vacuum (approximately 135 millimeters Hg pressure). Weigh out 180 grams of the aluminum oxide and pour the adsorbent mixture into the chromatographic tube in approximately 30-centimeter layers. After the addition of each layer, level off the top of the adsorbent with a flat glass rod or metal plunger by pressing down firmly until the adsorbent is well packed. Loosen the topmost few millimeters of each adsorbent layer with the end of a metal rod before the addition of the next layer. Continue packing in this manner until all the 180 grams of the adsorbent is added to the tube. Level off the top of the adsorbent by pressing down firmly with a flat glass rod or metal plunger to make the depth of the adsorbent bed approximately 80 centimeters in depth. Turn off the vacuum and remove the suction flask. Dissolve the hexadecane residue in 10 milliliters of warm benzene and decant the solution onto the column and allow the liquid level to recede to barely above the adsorbent level. Rapidly complete the transfer similarly with two 10-milliliter portions of benzene swirling the flask repeatedly each time to assure adequate washing of the residue. Fix the 1,000-milliliter reservoir onto the top of the chromatographic column. Just before the final 10-milliliter wash reaches the top of the adsorbent, add 670 milliliters of benzene to the reservoir and continue the percolation at the 2-3 milliliter per minute rate until a total of 670 milliliters of benzene has been utilized. Collect the eluate in a clean 1-liter Erlenmeyer flask (or optionally into a 1-liter evaporation flask). Allow the column to drain until most of the solvent mixture is removed. Add 1 milliliter of n -hexadecane and completely remove the benzene by evaporation under nitrogen, using the special procedure to eliminate benzene as previously described under “Organic Solvents.” Quantitatively transfer the residue with isooctane to a 25-milliliter volumetric flask and adjust to volume. Determine the absorbance of the solution in the 1-centimeter pathlength cells compared to isooctane as reference between 250 mµ-400 mµ. Correct for any absorbance derived from the reagents as determined by carrying out the procedure without a wax sample. If either spectrum shows the characteristic benzene peaks in the 250 mµ-260 mµ region, evaporate the solution to remove benzene by the procedure under “Organic Solvents.” Dissolve the residue, transfer quantitatively, and adjust to volume in isooctane in a 25-milliliter volumetric flask. Record the absorbance again. If the corrected absorbance does not exceed the limits prescribed in paragraph (a) of this section, the wax meets the ultraviolet absorbance specifications. (b) The polyhydric alcohol esters identified in this paragraph may be used as release agents in resinous and polymeric coatings for polyolefin films complying with § 175.320 of this chapter. Such esters meet the following specifications and are produced by partial esterification of oxidatively refined (Gersthofen process) montan wax acids with equimolar proportions of ethylene glycol and 1,3-butanediol: (1) Dropping point 77°-82 °C, as determined by ASTM method D566-76 (Reapproved 1982), “Standard Test Method for Dropping Point of Lubricating Grease,” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (a)(1) of this section. (2) Acid value 25-35, as determined by ASTM method D1386-78 (“Standard Test Method for Acid Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), which is incorporated by reference; copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. ) using as solvent xylene-ethyl alcohol in a 2:1 ratio instead of toluene-ethyl alcohol in a 1:2 ratio. (3) Saponification value 135-150, as determined by ASTM method D1387-78 (“Standard Test Method for Saponification Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), which is incorporated by reference; copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. ) using xylene-ethyl alcohol in a 2:1 ratio instead of ethyl alcohol in preparation of potassium hydroxide solution. (4) Ultraviolet absorbance limits specified in paragraph (a)(4) of this section, as determined by the analytical method described therein. (c) The polyhydric alcohol esters of oxidatively refined (Gersthofen process) montan wax acids, identified in paragraph (a) or (b) of this section, may also be used as a component of an aqueous dispersion of vinylidene chloride copolymers, subject to the conditions described in paragraphs (c)(1) and (2) of this section. (1) The aqueous dispersion of the additive contains not more that 18 percent polyhydric alcohol esters of oxidatively refined (Gersthofen process) montan wax acids, not more than 2 percent poly(oxyethylene) (minimum 20 moles of ethylene oxide) oleyl ether (CAS Reg. No. 9004-98-2), and not more than 1 percent poly(oxyethylene) (minimum 3 moles ethylene oxide) cetyl alcohols (CAS Reg. No. 9004-95-9). (2) The aqueous dispersion described in paragraph (c)(1) of this section is used as an additive to aqueous dispersions of vinylidene chloride copolymers, regulated in §§ 175.300, 175.320, 175.360, 176.170, 176,180, and 177.1630 of this chapter, at levels not to exceed 1.5 percent (solids basis) in the finished coating. (d) The polyhydric alcohol esters identified in this paragraph may be used as lubricants in the fabrication of vinyl chloride plastic food contact articles prepared from vinyl chloride polymers. Such esters meet the following specifications and are produced by partial esterification of oxidatively refined (Gersthofen process) montan wax acids with glycerol followed by neutralization: (1) Dropping point 79 to 85 °C, as determined by the American Society for Testing and Materials (ASTM), Method D-566-76 (Reapproved 1982), “Standard Test Method for Dropping Point of Lubricating Grease,” which is incorporated by reference in accordance with 5 U.S.C. 552(a). The availability of this incorporation by reference is given in paragraph (a)(1) of this section. (2) Acid value 20-30, as determined by ASTM Method D-1386-78 “Standard Test Method for Acid Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978) (which is incorporated by reference in accordance with 5 U.S.C. 552(a); the availability of this incorporation by reference is given in paragraph (a)(2) of this section), using as a solvent xylene-ethyl alcohol in a 2:1 ratio instead of toluene-ethyl alcohol in a 2:1 ratio. (3) Saponification value 130-160, as determined by ASTM Method D-1387-78 “Standard Test Method for Saponification Number (Empirical) of Synthetic and Natural Waxes” (Revised 1978), (which is incorporated by reference in accordance with 5 U.S.C. 552(a); the availability of this incorporation by reference is given in paragraph (a)(3) of this section), using xylene-ethyl alcohol in a 2:1 ratio instead of ethyl alcohol in the preparation of potassium hydroxide solution. (4) Ultraviolet absorbance limits specified in paragraph (a)(4) of this section, as determined by the analytical method described therein." 21:21:3.0.1.1.9.4.1.32,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3780 Polyhydric alcohol esters of long chain monobasic acids.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11849, Mar. 19, 1982; 54 FR 24899, June 12, 1989; 61 FR 14481, Apr. 2, 1996]","Polyhydric alcohol esters of long chain monobasic acids identified in this section may be safely used as lubricants in the fabrication of polyvinyl chloride and/or polyvinyl chloride copolymer articles complying with § 177.1980 of this chapter that contact food of Types I, II, IV-B, VI-B, VII-B, and VIII identified in table 1 in § 176.170(c) of this chapter under conditions of use E, F, and G described in table 2 in § 176.170(c) of this chapter, subject to the provisions of this section. (a) Identity. For the purpose of this section, polyhydric alcohol esters of long chain monobasic acids consist of polyhydric alcohol esters having number average molecular weights in the range of 1,050 to 1,700. The esters are produced by the reaction of either ethylene glycol or glycerol with long chain monobasic acids containing from 9 to 49 carbon atoms obtained by the ozonization of long chain alpha -olefins, the unreacted carboxylic acids in the formation of the glycerol esters being neutralized with calcium hydroxide to produce a composition having up to 2 percent by weight calcium. The alpha -olefins, obtained from the polymerization of ethylene, have 20 to 50 carbon atoms and contain a minimum of 75 percent by weight straight chain alpha -olefins and not more than 25 percent vinylidene compounds. (b) Specifications. The polyhydric alcohol esters have the following specifications: (1) Melting point of 60-80 °C for the ethylene glycol ester and 90-105 °C for the glycerol ester as determined by the Fisher Johns method as described in “Semimicro Qualitative Organic Analysis—The Systematic Identification of Organic Compounds,” by Cheronis and Entrikin, 2d Ed., Interscience Publishers, NY, which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (2) Acid value 15-25 for each ester as determined by the A.O.C.S. method Trla-64T “Titer Test,” which is incorporated by reference. Copies are available from American Association of Oil Chemists, 36 East Wacker Drive, Chicago, IL 60601, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. The method is modified to use as the acid solvent a 1:1 volume mixture of anhydrous isopropyl alcohol and toluene. The solution is titrated with 0.1 N methanolic sodium hydroxide. (3) Saponification value 120-160 for the ethylene glycol ester and 90-130 for the glycerol ester as determined the A.O.C.S. method Trla-64T “Saponification Value,” which is incorporated by reference. Copies are available from American Association of Oil Chemists, 36 East Wacker Drive, Chicago, IL 60601, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (4) Ultraviolet absorbance as specified in § 178.3770(a)(4) of this chapter when tested by the analytical method described therein." 21:21:3.0.1.1.9.4.1.33,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3790 Polymer modifiers in semirigid and rigid vinyl chloride plastics.,FDA,,,,"The polymers identified in paragraph (a) of this section may be safely admixed, alone or in mixture with other permitted polymers, as modifiers in semirigid and rigid vinyl chloride plastic food-contact articles prepared from vinyl chloride homopolymers and/or from vinyl chloride copolymers complying with § 177.1950, § 177.1970, and/or § 177.1980 of this chapter, in accordance with the following prescribed conditions: (a) For the purpose of this section, the polymer modifiers are identified as follows: (1) Acrylic polymers identified in this subparagraph provided that such polymers contain at least 50 weight-percent of polymer units derived from one or more of the monomers listed in paragraph (a)(1)(i) of this section. (i) Homopolymers and copolymers of the following monomers: n -Butyl acrylate. n -Butyl methacrylate. Ethyl acrylate. Methyl methacrylate. n -Butyl acrylate. n -Butyl methacrylate. Ethyl acrylate. Methyl methacrylate. (ii) Copolymers produced by copolymerizing one or more of the monomers listed in paragraph (a)(1)(i) of this section with one or more of the following monomers: Acrylonitrile. Butadiene. a -Methylstyrene. Styrene. Vinylidene chloride. Acrylonitrile. Butadiene. a -Methylstyrene. Styrene. Vinylidene chloride. (iii) Polymers identified in paragraphs (a)(1)(i) and (ii) of this section containing no more than 5 weight-percent of total polymer units derived by copolymerization with one or more of the following monomers: Acrylic acid. 1,3-Butylene glycol dimethacrylate. Divinylbenzene. Methacrylic acid. Acrylic acid. 1,3-Butylene glycol dimethacrylate. Divinylbenzene. Methacrylic acid. (iv) Mixtures of polymers identified in paragraph (a)(1)(i), (ii), and (iii) of this section; provided that no chemical reactions, other than addition reactions, occur when they are mixed. (2) Polymers identified in paragraph (a)(1) of this section combined during their polymerization with butadiene-styrene copolymers; provided that no chemical reactions, other than addition reactions, occur when they are combined. Such combined polymers may contain 50 weight-percent or more of total polymer units derived from the butadiene-styrene copolymers. (b) The polymer content of the finished plastic food-contact article consists of: (1) Not less than 80 weight-percent of polymer units derived from the vinyl chloride polymers identified in the introduction to this section and not more than 5 weight-percent of polymer units derived from polymers identified in paragraph (a)(1) of this section and may optionally contain up to 15 weight-percent of polymer units derived from butadiene-styrene copolymers; or (2) Not less than 50 weight-percent of polymer units derived from the vinyl chloride polymers identified in the introduction to this section, not more than 50 weight-percent of polymer units derived from homopolymers and/or copolymers of ethyl acrylate and methyl methacrylate, and not more than 30 weight-percent of polymer units derived from copolymers of methyl methacrylate, a -methylstyrene and acrylonitrile and may optionally contain up to 15 weight-percent of polymer units derived from butadiene-styrene copolymers. (c) No chemical reactions, other than addition reactions, occur among the vinyl chloride polymers and the modifying polymers present in the polymer mixture used in the manufacture of the finished plastic food-contact article. (d) The finished plastic food-contact article, when extracted with the solvent or solvents characterizing the type of food and under the conditions of time and temperature characterizing the conditions of its intended use as determined from tables 1 and 2 of § 176.170(c) of this chapter, yields extractives not to exceed the limits prescribed in § 177.1010 (b)(1), (2), (3), and (4) of this chapter when tested by the methods prescribed in § 177.1010 (c) of this chapter. (e) Acrylonitrile copolymers identified in this section shall comply with the provisions of § 180.22 of this chapter." 21:21:3.0.1.1.9.4.1.34,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3800 Preservatives for wood.,FDA,,,,"Preservatives may be safely used on wooden articles that are used or intended for use in packaging, transporting, or holding raw agricultural products subject to the provisions of this section: (a) The preservatives are prepared from substances identified in paragraph (b) of this section and applied in amounts not to exceed those necessary to accomplish the technical effect of protecting the wood from decay, mildew, and water absorption. (b) The substances permitted are as follows:" 21:21:3.0.1.1.9.4.1.35,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3850 Reinforced wax.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 1288, Jan. 12, 1982]","Reinforced wax may be safely used as an article or component of articles intended for use in producing, manufacturing, packing, processing, transporting, or holding food subject to the provisions of this section. (a) Reinforced wax consists of petroleum wax to which have been added certain optional substances required in its production, or added to impart desired physical or technical properties. (b) The quantity of any optional adjuvant substance employed in the production of or added to reinforced wax does not exceed the amount reasonably required to accomplish the intended physical or technical effect or any limitation provided in this section. (c) Any substance employed in the production of reinforced wax, including any optional substance, that is the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter, conforms with any specification in such regulation. (d) The substances and optional adjuvant substances employed in the production of or added to reinforced wax include: (1) Substances generally recognized as safe in food. (2) Substances subject to prior sanction for use in reinforced wax and used in accordance with such sanction or approval. (3) Substances identified in this subparagraph and subject to any limitations provided therein: (e) Reinforced wax conforming with the specifications in this paragraph is used as provided in paragraph (e)(2) of this section. (1) The chloroform-soluble portion of the water extract obtained by exposing reinforced wax to demineralized water at 70 °F for 48 hours shall not exceed 0.5 milligram per square inch of food-contact surface. (2) It is used as a packaging material or component of packaging materials for cheese and cheese products." 21:21:3.0.1.1.9.4.1.36,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3860 Release agents.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 44 FR 69649, Dec. 4, 1979; 46 FR 51902, Oct. 23, 1981; 61 FR 25396, May 21, 1996; 61 FR 42381, Aug. 15, 1996]","Substances listed in paragraph (b) of this section may be safely used as release agents in petroleum wax complying with § 178.3710 and in polymeric resins that contact food, subject to the provisions of this section. (a) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect or any limitations prescribed in this section. (b) Release agents:" 21:21:3.0.1.1.9.4.1.37,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3870 Rosins and rosin derivatives.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 47 FR 11849, Mar. 19, 1982; 49 FR 10113, Mar. 19, 1984; 54 FR 24899, June 12, 1989]","The rosins and rosin derivatives identified in paragraph (a) of this section may safely be used in the manufacture of articles or components of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section. (a) The rosins and rosin derivatives are identified as follows: (1) Rosins: (i) Gum rosin, refined to color grade of K or paler. (ii) Wood rosin, refined to color grade of K or paler. (iii) Tall oil rosin, refined to color grade of K or paler. (iv) Dark tall oil rosin, a fraction resulting from the refining of tall oil rosin produced by multicolumnar distillation of crude tall oil to effect removal of fatty acids and pitch components and having a saponification number of from 110-135 and 32 percent-44 percent rosin acids. (v) Dark wood rosin, all or part of the residue after the volatile terpene oils are distilled from the oleoresin extracted from pine wood. (2) Modified rosins manufactured from rosins identified in paragraph (a)(1) of this section: (i) Partially hydrogenated rosin, catalytically hydrogenated to a maximum refractive index of 1.5012 at 100 °C, and a color of WG or paler. (ii) Fully hydrogenated rosin, catalytically hydrogenated to a maximum dehydroabietic acid content of 2 percent, a minimum drop-softening point of 79 °C, and a color of X or paler. (iii) Partially dimerized rosin, dimerized by sulfuric acid catalyst to a drop-softening point of 95°-105 °C and a color of WG or paler. (iv) Fully dimerized rosin, dimerized by sulfuric acid catalyst, and from which sufficient nondimerized rosin has been removed by distillation to achieve a minimum drop-softening point of 143 °C, and a color of H or paler. (v) Disproportionated rosin, catalytically disproportionated to a minimum dehydroabietic acid content of 35 percent, a maximum abietic acid content of 1 percent, a maximum content of substituted phenanthrenes (as retene) of 0.25 percent, and a color of WG or paler. (3) Rosin esters manufactured from rosins and modified rosins identified in paragraphs (a)(1) and (2) of this section: (i) Glycerol ester of wood rosin purified by steam stripping to have an acid number of 3 to 9, a drop-softening point of 88°-96 °C, and a color of N or paler. (ii) Glycerol ester of partially hydrogenated wood rosin, having an acid number of 3 to 10, a drop-softening point of 79°-88 °C, and a color of N or paler. (iii) Glycerol ester of partially dimerized rosin, having an acid number of 3 to 8, a drop-softening point of 109°-119 °C, and a color of M or paler. (iv) Glycerol ester of fully dimerized rosin, having an acid number of 5 to 16, a drop-softening point of 165°-175 °C, and a color of H or paler. (v) Glycerol ester of maleic anhydride-modified wood rosin, having an acid number of 30 to 40, a drop-softening point of 138°-146 °C, a color of M or paler, and a saponification number less than 280. (vi) Methyl ester of rosin, partially hydrogenated, purified by steam stripping to have an acid number of 4 to 8, a refractive index of 1.5170 to 1.5205 at 20 °C, and a viscosity of 23 to 66 poises at 25 °C. (vii) Pentaerythritol ester of wood rosin, having an acid number of 6 to 16, a drop-softening point of 109°-116 °C, and a color of M or paler. (viii) Pentaerythritol ester of partially hydrogenated wood rosin, having an acid number of 7 to 18, a drop-softening point of 102°-110 °C, and a color of K or paler. (ix) Pentaerythritol ester of maleic anhydride-modified wood rosin, having an acid number of 8 to 16, a drop-softening point of 154°-162 °C, a color of M or paler, and having a saponification number less than 280. (x) Pentaerythritol ester of maleic anhydride-modified wood rosin, having an acid number of 9 to 16, a drop-softening point of 130°-140 °C, a color of N or paler, and having a saponification number less than 280. (xi) Pentaerythritol ester of maleic anhydride-modified wood rosin, having an acid number of 134 to 145, a drop-softening point of 127°-137 °C, a color of M or paler, and having a saponification number less than 280. (xii) Pentaerythritol ester of maleic anhydride-modified wood rosin, having an acid number of 30 to 40, a drop-softening point of 131°-137 °C, a color of N or paler, and having a saponification number less than 280. (xiii) Pentaerythritol ester of maleic anhydride-modified wood rosin, further modified by reaction with 4,4′-isopropyl-idenediphenol-formaldehyde condensate, having an acid number of 10 to 22, a drop-softening point of 162°-172 °C, a color of K or paler, a saponification number less than 280, and a maximum ultraviolet absorbance of 0.14 at 296 mµ (using a 1-centimeter cell and 200 milligrams of the rosin ester per liter of solvent consisting of ethyl alcohol made alkaline by addition of 0.1 percent of potassium hydroxide). (xiv) Mixed methyl and pentaerythritol ester of maleic anhydride-modified wood rosin, having an acid number of 73 to 83, a drop-softening point of 113°-123 °C, a color of M or paler, and a saponification number less than 280. (xv) Triethylene glycol ester of partially hydrogenated wood rosin, having an acid number of 2 to 10, a color of K or paler, and a viscosity of 350 to 425 seconds Saybolt at 100 °C. (xvi) Glycerol ester of maleic anhydride-modified wood rosin, having an acid number of 17 to 23, a drop-softening point of 136°-140 °C, a color of M or paler, and a saponification number less than 280. For use only in cellophane complying with § 177.1200 of this chapter. (xvii) Citric acid-modified glycerol ester of rosin, having an acid number less than 20, a drop-softening point of 105°-115 °C, and a color of K or paler. For use only as a blending agent in coatings for cellophane complying with § 177.1200 of this chapter. (xviii) Glycerol ester of tall oil rosin, purified by steam stripping to have an acid number of 5-12, a softening point of 80°-88 °C, and a color of N or paler. (xix) Glycerol ester of maleic anhydride-modified tall oil rosin, having an acid number of 30 to 40, a drop-softening point of 141°-146 °C, a color of N or paler, and a saponification number less than 280. (xx) Glycerol ester of disproportionated tall oil rosin, having an acid number of 5 to 10, a drop-softening point of 84°-93 °C, a color of WG or paler, and a saponification number less than 180. (4) Rosin salts and sizes—Ammonium, calcium, potassium, sodium, or zinc salts of rosin manufactured by the partial or complete saponification of any one of the rosins or modified rosins identified in paragraph (a)(1) and (2) of this section, or blends thereof, and with or without modification by reaction with one or more of the following: (i) Formaldehyde. (ii) Fumaric acid. (iii) Maleic anhydride. (iv) Saligenin. (b) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect. (c) The use in any substance or article that is the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter shall conform with any specifications and limitations prescribed by such regulation for the finished form of the substance or article. (d) The provisions of this section are not applicable to rosins and rosin derivatives identified in § 175.300(b)(3)(v) of this chapter and used in resinous and polymeric coatings complying with § 175.300 of this chapter. (e) The provisions of this section are not applicable to rosins and rosin derivatives identified in § 175.105(c)(5) of this chapter and used in defoaming agents complying with § 176.210 of this chapter, food-packaging adhesives complying with § 175.105 of this chapter, and rubber articles complying with § 177.2600 of this chapter. (f) The analytical methods for determining whether rosins and rosin derivatives conform to the specifications prescribed in paragraph (a) of this section are as follows: (1) Color: Color shall be as determined by ASTM method D509-70 (Reapproved 1981), “Standard Methods of Sampling and Grading Rosin,” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (2) Refractive index: Refractive index shall be as determined by ASTM method D1747-62 (Reapproved 1978), “Standard Test Method for Refractive Index of Viscous Materials,” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (f)(1) of this section. (3) Acid number: Acid number shall be as determined by ASTM method D465-82, “Standard Test Methods for Acid Number of Rosin,” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (f)(1) of this section. (4) Viscosity: Viscosity in poises shall be as determined by ASTM method D1824-66 (Reapproved 1980), “Standard Test Method for Apparent Viscosity of Plastisols and Organosols at Low Shear Rates by Brookfield Viscometer,” and in Saybolt seconds by ASTM method D88-81, “Standard Test Method for Saybolt Viscosity,” which are incorporated by reference. The availability of this incorporation by reference is given in paragraph (f)(1) of this section. (5) Softening point: Softening point shall be as determined by ASTM method E28-67, “Standard Test Method for Softening Point by Ring and Ball Apparatus” (Reapproved 1977), which is incorporated by reference. Copies are available from American Society for Testing and Materials (ASTM), 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. (6) Analytical methods for determining drop-softening point, saponification number, and any other specifications not listed under paragraphs (f)(1) through (5) of this section, titled: (i) “Determination of Abeitic Acid and Dehydroabietic Acid in Rosins”; (ii) “Determination of Softening Point of Solid Resins”; (iii) “Determination of Saponification Number of Rosin Esters,” and (iv) “Determination of Phenolic Modification of Rosin Derivatives,” which are incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html." 21:21:3.0.1.1.9.4.1.38,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3900 Sodium pentachlorophenate.,FDA,,,,Sodium pentachlorophenate may be safely used as a preservative for ammonium alginate employed as a processing aid in the manufacture of polyvinyl chloride emulsion polymers intended for use as articles or components of articles that contact food at temperatures not to exceed room temperature. The quantity of sodium pentachlorophenate used shall not exceed 0.5 percent by weight of ammonium alginate solids. 21:21:3.0.1.1.9.4.1.39,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3910 Surface lubricants used in the manufacture of metallic articles.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 48 FR 238, Jan. 4, 1983; 49 FR 10113, Mar. 19, 1984; 49 FR 29579, July 23, 1984; 50 FR 36874, Sept. 10, 1985; 52 FR 10223, Mar. 31, 1987; 54 FR 6124, Feb. 8, 1989; 54 FR 24899, June 12, 1989; 56 FR 55456, Oct. 28, 1991; 57 FR 23953, June 5, 1992; 58 FR 17513, Apr. 5, 1993; 64 FR 47110, Aug. 30, 1999; 69 FR 24512, May 4, 2004; 87 FR 31089, May 20, 2022]","The substances listed in this section may be safely used in surface lubricants employed in the manufacture of metallic articles that contact food, subject to the provisions of this section. (a) The following substances may be used in surface lubricants used in the rolling of metallic foil or sheet stock provided that total residual lubricant remaining on the metallic article in the form in which it contacts food does not exceed 0.015 milligram per square inch of metallic food-contact surface: (1) Substances identified in paragraphs (b)(1) and (2) of this section. (2) Substances identified in this paragraph. (3) Mineral oil conforming to the identity prescribed in § 178.3620(c). (4) Light petroleum hydrocarbons identified in paragraph (a)(4)(i) of this section: Provided, That the total residual lubricant on the metallic article in the form in which it contacts food meets the ultraviolet absorbance limits prescribed in paragraph (a)(4)(ii) of this section as determined by the analytical method described in paragraph (a)(4)(iii) of this section. (i) Light petroleum hydrocarbons are derived by distillation from virgin petroleum stocks or are synthesized from petroleum gases. They are chiefly paraffinic, isoparaffinic, napthenic, or aromatic in nature, and meet the following specifications: ( a ) Initial boiling point is 24 °C minimum and final boiling point is 288 °C maximum, as determined by ASTM method D86-82, “Standard Method for Distillation of Petroleum Products,” which is incorporated by reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. ( b ) Nonvolatile residue is 0.005 gram per 100 milliliters, maximum, as determined by ASTM method D381-80, “Standard Test Method for Existent Gum in Fuels by Jet Evaporation,” when the final boiling point is 121 °C or above and by ASTM method D1353-78, “Standard Test Method for Nonvolatile Matter in Volatile Solvents for Use in Paint, Varnish, Lacquer, and Related Products,” when the final boiling point is below 121 °C. These ASTM methods are incorporated by reference. The availability of these incorporations by reference is given in paragraph (a)(4)(i)( a ) of this section. ( c ) Saybolt color 20 minimum as determined by ASTM method D156-82, “Standard Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method),” which is incorporated by reference. The availability of this incorporation by reference is given in paragraph (a)(4)(i)( a ) of this section. ( d ) Aromatic component content shall not exceed 32 percent. ( e ) Conforms with ultraviolet absorbance limits prescribed in § 178.3620(c) as determined by the analytical method described therein. (ii) Ultraviolet absorbance limits on residual lubricants are as follows: (iii) The analytical method for determining ultraviolet absorbance limits on residual lubricants is as follows: general instructions Because of the sensitivity of the test, the possibility of errors arising from contamination is great. It is of the greatest importance that all glassware be scrupulously cleaned to remove all organic matter such as oil, grease, detergent, residues, etc. Examine all glassware including stoppers and stopcocks, under ultraviolet light to detect any residual fluorescent contamination. As a precautionary measure it is recommended practice to rinse all glassware with purified isooctane immediately before use. No grease is to be used on stopcocks or joints. Great care to avoid contamination of oil samples in handling and to assure absence of any extraneous material arising from inadequate packaging is essential. Because some of the polynuclear hydrocarbons sought in this test are very susceptible to photo-oxidation, the entire procedure is to be carried out under subdued light. apparatus Separatory funnels. 250-milliliter, 500-milliliter, 1,000-milliliter, and preferably 2,000-milliliter capacity, equipped with tetrafluoroethylene polymer stopcocks. Evaporation flask ( optional ). 250-milliliter or 500-milliliter capacity all-glass flask equipped with standard-taper stopper having inlet and outlet tubes to permit passage of nitrogen across the surface of contained liquid to be evaporated. Spectrophotometric cells. Fused quartz cells, optical path length in the range of 5,000 centimeters ±0.005 centimeter; also for checking spectrophotometer performance only, optical path length in the range 1.000 centimeter ±0.005 centimeter. With distilled water in the cells, determine any absorbance differences. Spectrophotometer. Special range 250 millicrons-400 millimicrons with spectral slit width of 2 millimicrons or less; under instrument operating conditions for these absorbance measurements, the spectrophotometer shall also meet the following performance requirements: Absorbance repeatability, ±0.01 at 0.4 absorbance. Absorbance accuracy, 1 ±0.05 at 0.4 absorbance. 1 As determined by procedure using potassium chromate for reference standard and described in National Bureau of Standards Circular 484, Spectrometry, U.S. Department of Commerce (1949), which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. The accuracy is to be determined by comparison with the standard values at 210, 345, and 400 millimicrons. Wavelength repeatability, ±0.2 millimicron. Wavelength accuracy, ±1.0 millimicron. Soxhlet apparatus. 60-millimeter diameter body tubes fitted with condenser and 500-milliliter round-bottom boiling flask. A supply of paper thimbles to fit is required. Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in cylinder equipped with regulator and valve to control flow at 5 p.s.i.g. reagents and materials Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this specification. The isooctane (2,2,4-trimethylpentane) shall pass the following test: Place 180 milliliters of solvent in a 250-milliliter Erlenmeyer flask, add 1 milliliter of purified n -hexadecane and evaporate on the steam bath under a stream of nitrogen (a loose aluminum foil jacket around the flask will speed evaporation). Discontinue evaporation when not over 1 milliliter of residue remains. Alternatively, the evaporation time can be reduced by using the optional evaporation flask. In this case the solvent and n -hexadecane are placed in the flask on the steam bath, the tube assembly is inserted, and a stream of nitrogen is fed through the inlet tube while the outlet tube is connected to a solvent trap and vacuum line in such a way as to prevent any flow-back of condensate into the flask. Dissolve the 1 milliliter of hexadecane residue in isooctane and make to 25 milliliters volume. Determine the absorbance in the 5-centimeter path length cells compared to isooctane as reference. The absorbance of the solution of the solvent residue shall not exceed 0.01 per centimeter path length between 280 and 400 mµ. Purify, if necessary, by passage through a column of activated silica gel (Grade 12, Davison Chemical Co., Baltimore, Maryland, or equivalent) about 90 centimeters in length and 5 centimeters to 8 centimeters in diameter. n-Hexadecane, 99-percent olefin-free. Dilute 1.0 milliliter of n -hexadecane to 25 milliliters with isooctane and determine the absorbance in a 5-centimeter cell compared to isooctane as reference point between 280 mµ-400 mµ. The absorbance per centimeter path length shall not exceed 0.00 in this range. Purify, if necessary, by percolation through activated silica gel or by distillation. Dimethyl sulfoxide. Spectrophotometric grade (Crown Zellerbach Corp., Camas, Washington, or equivalent). Absorbance (1-centimeter cell, distilled water reference, sample completely saturated with nitrogen). Wavelength Absorbance (maximum) 261.5 1.00 270 .20 275 .09 280 .06 300 .015 There shall be no irregularities in the absorbance curve within these wavelengths. Phosphoric acid. 85 percent A.C.S. reagent grade. Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in granular form. For each bottle of sodium sulfate reagent used, establish as follows the necessary sodium sulfate prewash to provide such filters required in the method: Place approximately 35 grams of anhydrous sodium sulfate in a 30-milliliter coarse, fritted-glass funnel or in a 65-milliliter filter funnel with glass wool plug; wash with successive 15-milliliter portions of the indicated solvent until a 15-milliliter portion of the wash shows 0.00 absorbance per centimeter path length between 280 mµ and 400 mµ when tested as prescribed under “Organic solvents.” Usually three portions of wash solvent are sufficient. Before proceeding with analysis of a sample, determine the absorbance in a 5-centimeter path cell between 250 millimicrons and 400 millimicrons for the reagent blank by carrying out the procedure, without a metal sample. The absorbance per centimeter path length should not exceed 0.02 in the wavelength range from 280 mµ to 400 mµ. Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory funnel and add 75 milliliters of phosphoric acid. Mix the contents of the funnel and allow to stand for 10 minutes. (The reaction between the sulfoxide and the acid is exothermic. Release pressure after mixing, then keep funnel stoppered.) Add 150 milliliters of isooctane and shake to pre-equilibrate the solvents. Draw off the individual layers and store in glass-stoppered flasks. procedure Sample. Select metal foil or sheet stock for the test which has not been previously contaminated by careless handling or exposure to atmospheric dust and fumes. A commercial coil in the form supplied for spindle mounting in a packaging line or wrapping machine is most suitable. Strip off the outside turn of metal and discard. Carefully avoid contamination or damage from handling the metal (wear gloves). Remove a 16-18-foot length from the coil and place it on a flat surface protected by a length of new kraft paper. Cut four 15-foot strips from the sample, each 3 inches wide (avoid tearing the edges of the strips). Using a piece of suitable glass rod, roll the strips of metal into loose coils and insert each into a Soxhlet thimble. Each turn of coil should be visibly separated from the adjacent turn. Extraction. Fill each of the four Soxhlet tubes with purified isooctane (see under heading “Reagents and Materials,” above) until siphon action occurs and then refill the tube body. Supply heat to the boiling flask and allow extraction to continue for at least 8 hours or until repeated weighings of the dried and cooled coil show no further weight loss. Combine the isooctane extracts from the four Soxhlet units in a suitable beaker, rinsing each tube and flask into the beaker with fresh purified solvent. Evaporate the solvent under an atmosphere of inert gas (nitrogen) to residual volume of 50-60 milliliters and transfer this solution to a 500-milliliter separatory funnel containing 100 milliliters of pre-equilibrated sulfoxide-phosphoric acid mixture. Complete the transfer of the sample with small portions of pre-equilibrated isooctane to give a total volume of the residue and solvent of 75 milliliters. Shake the funnel vigorously for 2 minutes. Set up three 250-milliliter separatory funnels with each containing 30 milliliters of pre-equilibrated isooctane. After separation of liquid phases, carefully draw off lower layer into the first 250-milliliter separatory funnel and wash in tandem with the 30-milliliter portion of isooctane contained in the 250-milliliter separatory funnels. Shaking time for each wash is 1 minute. Repeat the extraction operation with two additional portions of the sulfoxide-acid mixture and wash each extractive in tandem through the same three portions of isooctane. Collect the successive extractives (300 milliliters total) in a separatory funnel (preferably 2-liter) containing 480 milliliters of distilled water; mix, and allow to cool for a few minutes after the last extractive has been added. Add 80 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second separatory funnel (preferably 2-liter) and repeat the extraction with 80 milliliter of isooctane. Draw off and discard the aqueous layer. Wash each of the 80 milliliter extractives three times with 100-milliliter portions distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate pre-washed with isooctane (see sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the first separatory funnel with the second 80-milliliter isooctane extractive and pass through the sodium sulfate. Then wash the second and first separatory funnels successively with a 20-milliliter portion of isooctane and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane on the steam bath under nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane, reevaporate to 1 milliliter of hexadecane, and repeat this operation once. Quantitatively transfer the residue with isooctane to a 25-milliliter volumetric flask, make to volume, and mix. Determine the absorbance of the solution in 5-centimeter pathlength cells compared to isooctane as reference between 280mµ-400mµ (take care to lose none of the solution in filling the sample cell). Correct the absorbance values for any absorbance derived from reagents as determined by carrying out the procedure without a metal sample. If the corrected absorbance does not exceed the limits prescribed in this paragraph, the residue meets the ultraviolet absorbance specifications. Because of the sensitivity of the test, the possibility of errors arising from contamination is great. It is of the greatest importance that all glassware be scrupulously cleaned to remove all organic matter such as oil, grease, detergent, residues, etc. Examine all glassware including stoppers and stopcocks, under ultraviolet light to detect any residual fluorescent contamination. As a precautionary measure it is recommended practice to rinse all glassware with purified isooctane immediately before use. No grease is to be used on stopcocks or joints. Great care to avoid contamination of oil samples in handling and to assure absence of any extraneous material arising from inadequate packaging is essential. Because some of the polynuclear hydrocarbons sought in this test are very susceptible to photo-oxidation, the entire procedure is to be carried out under subdued light. Separatory funnels. 250-milliliter, 500-milliliter, 1,000-milliliter, and preferably 2,000-milliliter capacity, equipped with tetrafluoroethylene polymer stopcocks. Evaporation flask ( optional ). 250-milliliter or 500-milliliter capacity all-glass flask equipped with standard-taper stopper having inlet and outlet tubes to permit passage of nitrogen across the surface of contained liquid to be evaporated. Spectrophotometric cells. Fused quartz cells, optical path length in the range of 5,000 centimeters ±0.005 centimeter; also for checking spectrophotometer performance only, optical path length in the range 1.000 centimeter ±0.005 centimeter. With distilled water in the cells, determine any absorbance differences. Spectrophotometer. Special range 250 millicrons-400 millimicrons with spectral slit width of 2 millimicrons or less; under instrument operating conditions for these absorbance measurements, the spectrophotometer shall also meet the following performance requirements: Absorbance repeatability, ±0.01 at 0.4 absorbance. Absorbance accuracy, 1 ±0.05 at 0.4 absorbance. 1 As determined by procedure using potassium chromate for reference standard and described in National Bureau of Standards Circular 484, Spectrometry, U.S. Department of Commerce (1949), which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS-200), Food and Drug Administration, 5001 Campus Dr., College Park, MD 20740, or available for inspection at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. The accuracy is to be determined by comparison with the standard values at 210, 345, and 400 millimicrons. Wavelength repeatability, ±0.2 millimicron. Wavelength accuracy, ±1.0 millimicron. Soxhlet apparatus. 60-millimeter diameter body tubes fitted with condenser and 500-milliliter round-bottom boiling flask. A supply of paper thimbles to fit is required. Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in cylinder equipped with regulator and valve to control flow at 5 p.s.i.g. Organic solvents. All solvents used throughout the procedure shall meet the specifications and tests described in this specification. The isooctane (2,2,4-trimethylpentane) shall pass the following test: Place 180 milliliters of solvent in a 250-milliliter Erlenmeyer flask, add 1 milliliter of purified n -hexadecane and evaporate on the steam bath under a stream of nitrogen (a loose aluminum foil jacket around the flask will speed evaporation). Discontinue evaporation when not over 1 milliliter of residue remains. Alternatively, the evaporation time can be reduced by using the optional evaporation flask. In this case the solvent and n -hexadecane are placed in the flask on the steam bath, the tube assembly is inserted, and a stream of nitrogen is fed through the inlet tube while the outlet tube is connected to a solvent trap and vacuum line in such a way as to prevent any flow-back of condensate into the flask. Dissolve the 1 milliliter of hexadecane residue in isooctane and make to 25 milliliters volume. Determine the absorbance in the 5-centimeter path length cells compared to isooctane as reference. The absorbance of the solution of the solvent residue shall not exceed 0.01 per centimeter path length between 280 and 400 mµ. Purify, if necessary, by passage through a column of activated silica gel (Grade 12, Davison Chemical Co., Baltimore, Maryland, or equivalent) about 90 centimeters in length and 5 centimeters to 8 centimeters in diameter. n-Hexadecane, 99-percent olefin-free. Dilute 1.0 milliliter of n -hexadecane to 25 milliliters with isooctane and determine the absorbance in a 5-centimeter cell compared to isooctane as reference point between 280 mµ-400 mµ. The absorbance per centimeter path length shall not exceed 0.00 in this range. Purify, if necessary, by percolation through activated silica gel or by distillation. Dimethyl sulfoxide. Spectrophotometric grade (Crown Zellerbach Corp., Camas, Washington, or equivalent). Absorbance (1-centimeter cell, distilled water reference, sample completely saturated with nitrogen). There shall be no irregularities in the absorbance curve within these wavelengths. Phosphoric acid. 85 percent A.C.S. reagent grade. Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in granular form. For each bottle of sodium sulfate reagent used, establish as follows the necessary sodium sulfate prewash to provide such filters required in the method: Place approximately 35 grams of anhydrous sodium sulfate in a 30-milliliter coarse, fritted-glass funnel or in a 65-milliliter filter funnel with glass wool plug; wash with successive 15-milliliter portions of the indicated solvent until a 15-milliliter portion of the wash shows 0.00 absorbance per centimeter path length between 280 mµ and 400 mµ when tested as prescribed under “Organic solvents.” Usually three portions of wash solvent are sufficient. Before proceeding with analysis of a sample, determine the absorbance in a 5-centimeter path cell between 250 millimicrons and 400 millimicrons for the reagent blank by carrying out the procedure, without a metal sample. The absorbance per centimeter path length should not exceed 0.02 in the wavelength range from 280 mµ to 400 mµ. Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory funnel and add 75 milliliters of phosphoric acid. Mix the contents of the funnel and allow to stand for 10 minutes. (The reaction between the sulfoxide and the acid is exothermic. Release pressure after mixing, then keep funnel stoppered.) Add 150 milliliters of isooctane and shake to pre-equilibrate the solvents. Draw off the individual layers and store in glass-stoppered flasks. Sample. Select metal foil or sheet stock for the test which has not been previously contaminated by careless handling or exposure to atmospheric dust and fumes. A commercial coil in the form supplied for spindle mounting in a packaging line or wrapping machine is most suitable. Strip off the outside turn of metal and discard. Carefully avoid contamination or damage from handling the metal (wear gloves). Remove a 16-18-foot length from the coil and place it on a flat surface protected by a length of new kraft paper. Cut four 15-foot strips from the sample, each 3 inches wide (avoid tearing the edges of the strips). Using a piece of suitable glass rod, roll the strips of metal into loose coils and insert each into a Soxhlet thimble. Each turn of coil should be visibly separated from the adjacent turn. Extraction. Fill each of the four Soxhlet tubes with purified isooctane (see under heading “Reagents and Materials,” above) until siphon action occurs and then refill the tube body. Supply heat to the boiling flask and allow extraction to continue for at least 8 hours or until repeated weighings of the dried and cooled coil show no further weight loss. Combine the isooctane extracts from the four Soxhlet units in a suitable beaker, rinsing each tube and flask into the beaker with fresh purified solvent. Evaporate the solvent under an atmosphere of inert gas (nitrogen) to residual volume of 50-60 milliliters and transfer this solution to a 500-milliliter separatory funnel containing 100 milliliters of pre-equilibrated sulfoxide-phosphoric acid mixture. Complete the transfer of the sample with small portions of pre-equilibrated isooctane to give a total volume of the residue and solvent of 75 milliliters. Shake the funnel vigorously for 2 minutes. Set up three 250-milliliter separatory funnels with each containing 30 milliliters of pre-equilibrated isooctane. After separation of liquid phases, carefully draw off lower layer into the first 250-milliliter separatory funnel and wash in tandem with the 30-milliliter portion of isooctane contained in the 250-milliliter separatory funnels. Shaking time for each wash is 1 minute. Repeat the extraction operation with two additional portions of the sulfoxide-acid mixture and wash each extractive in tandem through the same three portions of isooctane. Collect the successive extractives (300 milliliters total) in a separatory funnel (preferably 2-liter) containing 480 milliliters of distilled water; mix, and allow to cool for a few minutes after the last extractive has been added. Add 80 milliliters of isooctane to the solution and extract by shaking the funnel vigorously for 2 minutes. Draw off the lower aqueous layer into a second separatory funnel (preferably 2-liter) and repeat the extraction with 80 milliliter of isooctane. Draw off and discard the aqueous layer. Wash each of the 80 milliliter extractives three times with 100-milliliter portions distilled water. Shaking time for each wash is 1 minute. Discard the aqueous layers. Filter the first extractive through anhydrous sodium sulfate pre-washed with isooctane (see sodium sulfate under “Reagents and Materials” for preparation of filter) into a 250-milliliter Erlenmeyer flask (or optionally into the evaporation flask). Wash the first separatory funnel with the second 80-milliliter isooctane extractive and pass through the sodium sulfate. Then wash the second and first separatory funnels successively with a 20-milliliter portion of isooctane and pass the solvent through the sodium sulfate into the flask. Add 1 milliliter of n -hexadecane and evaporate the isooctane on the steam bath under nitrogen. Discontinue evaporation when not over 1 milliliter of residue remains. To the residue, add a 10-milliliter portion of isooctane, reevaporate to 1 milliliter of hexadecane, and repeat this operation once. Quantitatively transfer the residue with isooctane to a 25-milliliter volumetric flask, make to volume, and mix. Determine the absorbance of the solution in 5-centimeter pathlength cells compared to isooctane as reference between 280mµ-400mµ (take care to lose none of the solution in filling the sample cell). Correct the absorbance values for any absorbance derived from reagents as determined by carrying out the procedure without a metal sample. If the corrected absorbance does not exceed the limits prescribed in this paragraph, the residue meets the ultraviolet absorbance specifications. (b) The following substances may be used in surface lubricants used to facilitate the drawing, stamping, or forming of metallic articles from rolled foil or sheet stock by further processing provided that the total residual lubricant remaining on the metallic article in the form in which it contacts food does not exceed 0.2 milligram per square inch of food-contact surface: (1) Antioxidants used in compliance with regulations in parts 170 through 189 of this chapter. (2) Substances identified in this subparagraph. (c) The substances identified in paragraph (a)(2) of this section may be used in surface lubricants used to facilitate the drawing, stamping, and forming of metallic articles from rolled foil and sheet stock provided that total residual lubricant remaining on the metallic article in the form in which it contacts food does not exceed 0.015 milligram per square inch of food-contact surface. (d) Subject to any prescribed limitations, the quantity of surface lubricant used in the manufacture of metallic articles shall not exceed the least amount reasonably required to accomplish the intended technical effect and shall not be intended to nor, in fact, accomplish any technical effect in the food itself. (e) The use of the surface lubricants in the manufacture of any article that is the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter must comply with any specifications prescribed by such regulation for the finished form of the article. (f) Any substance that is listed in this section and the subject of a regulation in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter shall comply with any applicable specifications prescribed by such regulation." 21:21:3.0.1.1.9.4.1.4,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3130 Antistatic and/or antifogging agents in food-packaging materials.,FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 45 FR 56797, Aug. 26, 1980; 45 FR 85727, Dec. 30, 1980; 46 FR 13688, Feb. 24, 1981; 47 FR 26824, June 22, 1982; 51 FR 28932, Aug. 13, 1986; 56 FR 41457, Aug. 21, 1991; 58 FR 57556, Oct. 26, 1993; 60 FR 54430, Oct. 24, 1995; 60 FR 18351, Apr. 11, 1995; 62 FR 31511, June 10, 1997; 63 FR 38748, July 20, 1998; 64 FR 62585, Nov. 17, 1999; 76 FR 59249, Sept. 26, 2011]","The substances listed in paragraph (b) of this section may be safely used as antistatic and/or antifogging agents in food-packaging materials, subject to the provisions of this section: (a) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect. (b) List of substances:" 21:21:3.0.1.1.9.4.1.40,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3930 Terpene resins.,FDA,,,,"The terpene resins identified in paragraph (a) of this section may be safely used as components of polypropylene film intended for use in contact with food, and the terpene resins identified in paragraph (b) of this section may be safely used as components of polyolefin film intended for use in contact with food; (a) Terpene resins consisting of the hydrogenated polymers of terpene hydrocarbons obtainable from sulfate turpentine and meeting the following specifications: Drop-softening point of 118°-138 °C; iodine value less than 20. (b) Terpene resins consisting of polymers of beta-pinene and meeting the following specifications: Acid value less than 1; saponification number less than 1; color less than 4 on the Gardner scale as measured in 50 percent mineral spirits solution." 21:21:3.0.1.1.9.4.1.41,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3940 Tetraethylene glycol di-(2-ethylhexoate).,FDA,,,,Tetraethylene glycol di-(2-ethylhexoate) containing not more than 22 parts per million ethylene and/or diethylene glycols may be used at a level not to exceed 0.7 percent by weight of twine as a finish on twine to be used for tying meat provided the twine fibers are produced from nylon resins complying with § 177.1500 of this chapter. 21:21:3.0.1.1.9.4.1.42,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3950 Tetrahydrofuran.,FDA,,,,"Tetrahydrofuran may be safely used in the fabrication of articles intended for packaging, transporting, or storing foods, subject to the provisions of this section. (a) It is used as a solvent in the casting of film from a solution of polymeric resins of vinyl chloride, vinyl acetate, or vinylidene chloride that have been polymerized singly or copolymerized with one another in any combination, or it may be used as a solvent in the casting of film prepared from vinyl chloride copolymers complying with § 177.1980 of this chapter. (b) The residual amount of tetrahydrofuran in the film does not exceed 1.5 percent by weight of film." 21:21:3.0.1.1.9.4.1.5,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,"§ 178.3280 Castor oil, hydrogenated.",FDA,,,"[42 FR 14609, Mar. 15, 1977, as amended at 55 FR 8914, Mar. 9, 1990]","Hydrogenated castor oil may be safely used in the manufacture of articles or components of articles intended for use in contact with food subject to the provisions of this section. (a) The quantity used shall not exceed the amount reasonably required to accomplish the intended technical effect. (b) The additive is used as follows:" 21:21:3.0.1.1.9.4.1.6,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3290 Chromic chloride complexes.,FDA,,,,"Myristo chromic chloride complex and stearato chromic chloride complex may be safely used as release agents in the closure area of packaging containers intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions of this section: (a) The quantity used shall not exceed that reasonably required to accomplish the intended technical effect nor exceed 7 micrograms of chromium per square inch of closure area. (b) The packaging container which has its closure area treated with the release agent shall have a capacity of not less than 120 grams of food per square inch of such treated closure area." 21:21:3.0.1.1.9.4.1.7,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3295 Clarifying agents for polymers.,FDA,,,"[46 FR 59236, Dec. 4, 1981, as amended at 52 FR 30920, Aug. 18, 1987; 53 FR 30049, Aug. 10, 1988; 54 FR 12432, Mar. 27, 1989; 54 FR 14734, Apr. 12, 1989; 55 FR 52990, Dec. 26, 1990; 56 FR 1085, Jan. 11, 1991; 59 FR 13650, Mar. 23, 1994; 59 FR 25323, May 16, 1994; 61 FR 33847, July 1, 1996; 61 FR 51588, Oct. 3, 1996; 61 FR 65943, Dec. 16, 1996; 63 FR 56789, Oct. 23, 1998; 63 FR 68392, Dec. 11, 1998; 64 FR 26843, May 18, 1999; 65 FR 16316, Mar. 28, 2000]","Clarifying agents may be safely used in polymers that are articles or components of articles intended for use in contact with food, subject to the provisions of this section:" 21:21:3.0.1.1.9.4.1.8,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3297 Colorants for polymers.,FDA,,,"[48 FR 46775, Oct. 14, 1983]","The substances listed in paragraph (e) of this section may be safely used as colorants in the manufacture of articles or components of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, subject to the provisions and definitions set forth in this section: (a) The term colorant means a dye, pigment, or other substance that is used to impart color to or to alter the color of a food-contact material, but that does not migrate to food in amounts that will contribute to that food any color apparent to the naked eye. For the purpose of this section, the term “colorant” includes substances such as optical brighteners and fluorescent whiteners, which may not themselves be colored, but whose use is intended to affect the color of a food-contact material. (b) The colorant must be used in accordance with current good manufacturing practice, including use levels which are not in excess of those reasonably required to accomplish the intended coloring effect. (c) Colorants in this section must conform to the description and specifications indicated. If a polymer described in this section is itself the subject of a regulation promulgated under section 409 of the Federal Food, Drug, and Cosmetic Act, it shall also comply with any specifications and limitations prescribed by that regulation. Extraction testing guidelines to conduct studies for additional uses of colorants under this section are available from the Food and Drug Administration free of charge from the Food and Drug Administration, Center for Food Safety and Applied Nutrition, 5001 Campus Dr., College Park, MD 20740, 240-402-1200 (d) Color additives and their lakes listed for direct use in foods, under the provisions of the color additive regulations in parts 73, 74, 81, and 82 of this chapter, may also be used as colorants for food-contact polymers. (e) List of substances:" 21:21:3.0.1.1.9.4.1.9,21,Food and Drugs,I,B,178,"PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS",D,Subpart D—Certain Adjuvants and Production Aids,,§ 178.3300 Corrosion inhibitors used for steel or tinplate.,FDA,,,,"Corrosion inhibitors may be safely used for steel or tinplate intended for use in, or to be fabricated as, food containers or food-processing or handling equipment, subject to the provisions of this section. (a) The corrosion inhibitors are prepared from substances identified in this section and used subject to the limitations prescribed. (b) The following corrosion inhibitors or adjuvants are used in amounts not to exceed those reasonably required to accomplish the intended physical or technical effect: (1) Corrosion inhibitors (active ingredients) used in packaging materials for the packaging of steel or tinplate or articles fabricated therefrom: (2) Adjuvants employed in the application and use of corrosion inhibitors:" 40:40:26.0.1.1.25.1.19.1,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,A,Subpart A—General Provisions,,§ 178.3 Definitions.,EPA,,,"[55 FR 50291, Dec. 5, 1990, as amended at 57 FR 28087, June 24, 1992; 77 FR 46292, Aug. 3, 2012]","For the purposes of this part: Administrator means the Administrator of the Agency, or any officer or employee of the Agency to whom the Administrator delegates the authority to perform functions under this part. Agency means the United States Environmental Protection Agency. Assistant Administrator means the Agency's Assistant Administrator for Chemical Safety and Pollution Prevention, or any officer or employee of the Agency's Office of Chemical Safety and Pollution Prevention to whom the Assistant Administrator delegates the authority to perform functions under this part. FFDCA means the Federal Food, Drug, and Cosmetic Act, as amended, 21 U.S.C. 301-392." 40:40:26.0.1.1.25.2.19.1,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.20 Right to submit objections and requests for a hearing.,EPA,,,"[55 FR 50291, Dec. 5, 1990, as amended at 70 FR 33359, June 8, 2005]","(a) On or before the 60th day after the date of publication in the Federal Register of an order under part 180 of this chapter establishing, modifying, or revoking a regulation, or denying all or any portion of a petition, a person adversely affected by such order or petition denial may submit, in accordance with § 178.25, one or more written objections to the order (or to the action that is the subject of the order). (b) A person may include with any such objection a written request for an evidentiary hearing on such objection in accordance with § 178.27 (c) A person who submits objections need not request a hearing. For instance, if the person's objections are of a purely legal or policy nature, a hearing request would be inappropriate; the purpose of an evidentiary hearing is to resolve factual disputes. The Administrator will rule on the objections, whether or not a hearing is requested. (d) As a matter of discretion, the Administrator may order a hearing on an objection even though no person has requested a hearing." 40:40:26.0.1.1.25.2.19.2,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.25 Form and manner of submission of objections.,EPA,,,"[55 FR 50291, Dec. 5, 1990, as amended at 69 FR 39864, July 1, 2004; 70 FR 33359, June 8, 2005; 71 FR 35546, June 21, 2006]","(a) To be considered by the Administrator, an objection must: (1) Be in writing. (2) Specify with particularity the provision(s) of the order, regulation, or denial objected to, the basis for the objection(s), and the relief sought. (3) Be signed by the objector. (4) State the objector's name and mailing address. (5) Be accompanied by the fee prescribed by § 180.33(i) of this chapter, if the objection is to an order or regulation issued under part 180 of this chapter. (6) Be submitted to the hearing clerk. (7) Be received by the Hearing Clerk not later than the close of business of the 60th day following the date of the publication in the Federal Register of the order to which the objection is taken (or, if such 60th day is a Saturday, Sunday, or Federal holiday, not later than the close of business of the next government business day after such 60th day). (b) Submissions to the hearing clerk shall be made as follows: (1) Mailed submissions should be addressed to: Office of the Hearing Clerk (1900L), Environmental Protection Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460-0001. (2) For hand/courier delivery the Office of the Hearing Clerk is located at Suite 350, 1099 14 th St., NW., Washington, DC 20005." 40:40:26.0.1.1.25.2.19.3,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.27 Form and manner of submission of request for evidentiary hearing.,EPA,,,,"To be considered by the Administrator, a request for an evidentiary hearing must meet the criteria in § 178.32, and must: (a) Be submitted as a part of, and specifically request an evidentiary hearing on an objection that complies with the requirements of § 178.25. (b) Include a statement of the factual issue(s) on which a hearing is requested and the requestor's contentions on each such issue. (c) Include a copy of any report, article, survey, or other written document (or the pertinent pages thereof) upon which the objector relies to justify an evidentiary hearing, unless the document is an EPA document that is routinely available to any member of the public. (d) Include a summary of any evidence not described in paragraph (a)(3) of this section upon which the objector relies to justify an evidentiary hearing. (e) Include a discussion of the relationship between the factual issues and the relief requested by the objection." 40:40:26.0.1.1.25.2.19.4,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.30 Response by Administrator to objections and to requests for hearing.,EPA,,,,"The Administrator will respond to objections, and to requests for a hearing on such objections, as set forth in this section. (a) Denial of objections that are improperly submitted or that seek an unavailable form of relief. The Administrator will by order issued under § 178.37 deny each objection and each request for a hearing that is included with such an objection, if: (1) The objection is found not to conform to § 178.25. (2) The action requested by the objection is inconsistent with any provision of FFDCA. (3) The action requested by the objection is inconsistent with any generic, e.g., non-chemical specific, interpretation of a provision of FFDCA in any regulation in this chapter (the proper procedure in such a case is for the person to petition for an amendment of the regulation involved). (b) Denial of improperly submitted requests for hearing. The Administrator will then determine whether any objection that has not been denied under paragraph (a) of this section was accompanied by a request for an evidentiary hearing that conforms to § 178.27. The Administrator will deny under § 178.37 each request that does not conform to § 178.27. (c) Grouping of certain related objections. If the Administrator then finds (1) That two or more undenied objections are substantially similar, or are related in such a way that any judicial review of the Administrator's action on those objections should occur at the same time, and (2) that one or more of those objections was accompanied by an undenied request for an evidentiary hearing on that objection, the Administrator will treat those objections as a group and will rule on them only after ruling under § 178.32 on the associated request for hearing. (d) Rulings on objections for which a request for hearing has been granted. If the Administrator rules under § 178.32 that an evidentiary hearing should be held on an objection, the Administrator will resolve the issues raised by any other objection grouped with it under paragraph (c) of this section in conjunction with the evidentiary hearing upon which the hearing request was granted, unless the Administrator for good cause determines otherwise. (e) Rulings on objections for which no request for hearing was received, or for which each request for hearing was denied. Except as provided in paragraphs (c) and (d) of this section, if no hearing was requested on an objection, or if each such request that was made is denied under the criteria of paragraphs (a) or (b) of this section or § 178.32(b), the Administrator will rule on the objection under § 178.37." 40:40:26.0.1.1.25.2.19.5,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.32 Rulings on requests for hearing.,EPA,,,,"(a) In the case of each request for an evidentiary hearing that was not denied under § 178.30(a) or (b), the Administrator will determine whether such a hearing on one or more of the objections is justified, and will publish in the Federal Register the determination in an order issued under § 178.37 or a Notice of Hearing issued under § 179.20 of this chapter. If some requests for a hearing are denied and others pertaining to the same order or regulation are granted, the denial order and the hearing notice may be combined into a single document and shall be issued at the same time unless the Administrator for good cause determines otherwise. (b) A request for an evidentiary hearing will be granted if the Administrator determines that the material submitted shows the following: (1) There is a genuine and substantial issue of fact for resolution at a hearing. An evidentiary hearing will not be granted on issues of policy or law. (2) There is a reasonable possibility that available evidence identified by the requestor would, if established, resolve one or more of such issues in favor of the requestor, taking into account uncontested claims or facts to the contrary. An evidentiary hearing will not be granted on the basis of mere allegations, denials, or general descriptions of positions and contentions, nor if the Administrator concludes that the data and information submitted, even if accurate, would be insufficient to justify the factual determination urged. (3) Resolution of the factual issue(s) in the manner sought by the person requesting the hearing would be adequate to justify the action requested. An evidentiary hearing will not be granted on factual issues that are not determinative with respect to the action requested. For example, a hearing will not be granted if the Administrator concludes that the action would be the same even if the factual issue were resolved in the manner sought. (c) Where appropriate, the Administrator will make rulings on any issues raised by an objection which are necessary for resolution prior to determining whether a request for an evidentiary hearing should be granted." 40:40:26.0.1.1.25.2.19.6,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.35 Modification or revocation of regulation or prior order.,EPA,,,"[55 FR 50291, Dec. 5, 1990, as amended at 70 FR 33359, June 8, 2005]","(a) If the Administrator determines upon review of an objection or request for hearing that the regulation or prior order in question should be modified or revoked, the Administrator will publish an order setting forth any revision to the regulation or prior order that the Administrator has found to be warranted. (b) The Administrator will provide an opportunity for objections and requests for hearing on such order to the extent required by law. Such objections to the modification or revocation of the regulation, and requests for a hearing on such objections, may be submitted under §§ 178.20 through 178.27. (c) Objections and requests for hearing that are not affected by the modification or revocation will remain on file and be acted upon in accordance with this part." 40:40:26.0.1.1.25.2.19.7,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,B,Subpart B—Procedures for Filing Objections and Requests for Hearing,,§ 178.37 Order responding to objections on which a hearing was not requested or was denied.,EPA,,,"[55 FR 50291, Dec. 5, 1990, as amended at 70 FR 33359, June 8, 2005]","(a) The Administrator will publish in the Federal Register an order under FFDCA section 408(g)(2)(B) or section 408(g)(2)(C) setting forth the Administrator's determination on each denial of a request for a hearing, and on each objection submitted under § 178.20 on which: (1) A hearing was not requested. (2) A hearing was requested, but denied. (b) Each order published under paragraph (a) of this section must state the reasons for the Administrator's determination. If the order denies a request for a hearing on the objection, the order also must state the reason for that denial (e.g., why the request for a hearing did not conform to § 178.27, or why the request was denied under § 178.32). (c) Each order published under paragraph (a) of this section must state its effective date." 40:40:26.0.1.1.25.4.19.1,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,D,Subpart D—Judicial Review,,§ 178.65 Judicial review.,EPA,,,"[70 FR 33359, June 8, 2005]","An order issued under § 178.37 is final agency action reviewable in the courts as provided by FFDCA section 408(h), as of the date of publication of the order in the Federal Register. The failure to file a petition for judicial review within the period ending on the 60th day after the date of the publication of the order constitutes a waiver under FFDCA section 408(h) of the right to judicial review of the order and of any regulation promulgated by the order." 40:40:26.0.1.1.25.4.19.2,40,Protection of Environment,I,E,178,PART 178—OBJECTIONS AND REQUESTS FOR HEARINGS,D,Subpart D—Judicial Review,,§ 178.70 Administrative record.,EPA,,,"[55 FR 50291, Dec. 5, 1990, as amended at 70 FR 33359, June 8, 2005]","(a) For purposes of judicial review, the record of an administrative proceeding that culminates in an order under § 178.37 consists of: (1) The objection ruled on (and any request for hearing that was included with the objection). (2) Any order issued under § 180.7(g) of this chapter to which the objection related, and: (i) Any regulation or petition denial that was the subject of that order. (ii) The petition to which such order responded. (iii) Any amendment or supplement of the petition. (iv) The data and information submitted in support of the petition. (v) The notice of filing of the petition. (3) Any order issued under § 180.29(f) of this chapter to which the objection related, the regulation that was the subject of that order, and each related Notice of Proposed Rulemaking. (4) Any comments submitted by members of the public in response to the Notice of Filing or Notice of Proposed Rulemaking, any data or information submitted as part of the comments, the Administrator's response to comments and the documents or information relied on by the Administrator in issuing the regulation or order. (5) All other documents or information submitted to the docket for the rulemaking in question. (6) The order issued under § 178.37. (b) The record will be closed as of the date of the Administrator's decision unless another date for closing of the record is specified in the order issued under § 178.37." 46:46:7.0.1.3.13.1.63.1,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,A,Subpart A—General Provisions,,§ 178.115 Applicability to existing vessels.,USCG,,,"[CGD 85-080, 61 FR 966, Jan. 10, 1996, as amended by USCG-2007-0030, 75 FR 78087, Dec. 14, 2010]","Except where specifically stated otherwise, an existing vessel must comply with the intact stability and seaworthiness regulations which were applicable to the vessel on March 10, 1996, or, as an alternative, the vessel may comply with the regulations in this part." 46:46:7.0.1.3.13.2.63.1,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,B,Subpart B—Stability Instructions for Operating Personnel,,§ 178.210 Stability information.,USCG,,,"[CGD 85-080, 61 FR 966, Jan. 10, 1996, as amended by USCG-2007-0030, 75 FR 78087, Dec. 14, 2010]","(a) Stability information (stability details indicated on the Certificate of Inspection, a stability letter, or a stability booklet), is required on certain vessels by paragraphs (b), (c), or (d) of this section. Enough stability information, including stability calculations and assumptions made to use them, must be provided to allow the master to be able to determine operating guidelines, loading restrictions, and ensure compliance with the applicable intact and damage stability regulations of this chapter. (b) A vessel which, under § 178.310 of this part, complies with requirements in subchapter S of this chapter, must have stability details on the vessel's Certificate of Inspection, a stability letter issued by the cognizant Officer in Charge, Marine Inspection (OCMI) or the Commanding Officer, Marine Safety Center, or an approved stability booklet. The form in which the stability information must be contained ( i.e. , stability details on the Certificate of Inspection, a stability letter, or a stability booklet) will be determined by the Commanding Officer, Marine Safety Center. (c) When necessary for safe operation, the cognizant OCMI may place specific stability restrictions in a stability letter or on the Certificate of Inspection of a vessel not more than 65 feet (19.8 meters) in length, which, under § 178.310 of this part, complies with the requirements of § 178.320 of this part. (d) Each pontoon vessel must have a stability letter and each stability letter issued after March 14, 2011 must be issued by the Commanding Officer, Marine Safety Center." 46:46:7.0.1.3.13.2.63.2,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,B,Subpart B—Stability Instructions for Operating Personnel,,§ 178.215 Weight of passengers and crew.,USCG,,,"[USCG-2007-0030, 75 FR 78087, Dec. 14, 2010]","(a) This section applies to each vessel, regardless of when constructed, for which stability information is based on the results of a simplified stability proof test. (b) Except as provided in paragraph (c) of this section, and if not provided in the stability information required, the owner of each vessel must provide the master with the total test weight used in the simplified stability proof test and the number of passengers and crew included in the total test weight. Owners and masters must use a total weight of passengers and crew carried that is based upon an assumed weight per person, which is determined in accordance with § 170.090 of this chapter. (c) The information specified in paragraph (b) of this section need not be provided if the owner attests that the vessel complies with applicable intact stability requirements when carrying the number of passengers and crew permitted by the Certificate of Inspection with an assumed weight per person determined in accordance with § 170.090 of this chapter." 46:46:7.0.1.3.13.2.63.3,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,B,Subpart B—Stability Instructions for Operating Personnel,,§ 178.220 Stability booklet.,USCG,,,,"When the Commanding Officer, Marine Safety Center determines, in accordance with § 178.210(b), that a vessel must have a stability booklet, the owner or operator must prepare the booklet in accordance with subchapter S of this chapter, and submit it to the Commanding Officer, Marine Safety Center." 46:46:7.0.1.3.13.2.63.4,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,B,Subpart B—Stability Instructions for Operating Personnel,,§ 178.230 Stability letter or Certificate of Inspection stability details.,USCG,,,"[CGD 85-080, 61 FR 966, Jan. 10, 1996, as amended by USCG-2007-0030, 75 FR 78087, Dec. 14, 2010]","(a) When the cognizant OCMI or the Commanding Officer, Marine Safety Center determines, in accordance with § 178.210, that a vessel must have stability details indicated on its Certificate of Inspection or a stability letter, the owner or operator must submit the information listed in paragraph (b) of this section: (1) If § 178.210(c) is applicable, to the OCMI for approval; or (2) If § 178.210(b) is applicable, to the Commanding Officer, Marine Safety Center for approval. (b) If § 178.210(b) of this part applies, the applicable information described in subpart C of part 170 of this title, and the calculations used to determine that information, must be submitted in addition to the applicable information listed in paragraph (b) of this section. (1) Allowable weight and number of passengers and crew on each deck; (2) Deepest waterline drafts or freeboard; (3) Location of watertight bulkheads and openings in watertight bulkheads; (4) Explanation of the vessel's subdivision and specific identification of the vessel's subdivision bulkheads; (5) Location of openings through watertight bulkheads, such as watertight doors, which must be closed to limit flooding in an emergency; (6) Location, type and amount of fixed ballast; (7) Location and details of foam flotation material; and (8) Maximum weight of portable equipment permitted on the vessel including diving equipment. (c) If § 178.210(c) of this part applies, the allowable weight and number of passengers and crew on each deck, and the necessary calculations used to determine that information, must be submitted in accordance with paragraph (a) of this section." 46:46:7.0.1.3.13.3.63.1,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,C,Subpart C—Intact Stability Standards,,§ 178.310 Intact stability requirements—general.,USCG,,,"[USCG-2007-0030, 75 FR 78088, Dec. 14, 2010]","(a) Except as provided in paragraph (c) of this section, each vessel must, in each condition of loading and operation, comply with the applicable requirements of— (1) Part 170 of this chapter, except subparts G and H; and (2) Part 171 of this chapter, subparts A and B. (b) Sailing vessels must meet the appropriate requirements of § 171.055 or § 171.057 in subchapter S in this chapter while under sail, as well as the requirements of § 170.170 in subchapter S in this chapter while under bare poles (if an auxiliary sailing vessel as defined in § 170.055(a) of this chapter) and with storm sails set and trimmed flat (if a sailing vessel as defined in § 170.055(n) of this chapter). (c) As an alternative to meeting the requirements of paragraphs (a) and (b) of this section, a vessel may demonstrate compliance with an appropriate standard set forth in either § 178.320 of this part for non-sailing vessels or § 178.325 of this part for monohull sailing vessels if all of the following criteria are satisfied: (1) The length is not more than 19.8 meters (65 feet) in length; (2) The vessel does not carry more than 12 passengers on an international voyage; (3) The vessel either does not have more than one deck above the bulkhead deck or, if without a bulkhead deck, does not have more than one deck above the deck from which freeboard is measured excluding a pilot house; and (4) The vessel's stability has not been questioned by the cognizant Officer in Charge, Marine Inspection (OCMI). (d) In lieu of the requirements in paragraphs (a) through (c) of this section, a vessel may meet another stability standard approved by the Commanding Officer, Marine Safety Center." 46:46:7.0.1.3.13.3.63.2,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,C,Subpart C—Intact Stability Standards,,§ 178.320 Intact stability requirements—non-sailing vessels.,USCG,,,"[USCG-2007-0030, 75 FR 78088, Dec. 14, 2010]","(a) As permitted by § 178.310(c) of this part, the following vessels may undergo the simplified stability proof test detailed in § 178.330 of this part, in the presence of a Coast Guard marine inspector, if they do not have tumblehome at the deck, measured amidships, that exceeds 2 percent of the beam: (1) Monohull vessels; and (2) Flush deck catamaran vessels which are not pontoon vessels and carry not more than 49 passengers. (b) As permitted by § 178.310(c) of this part, a self-propelled pontoon vessel may undergo the pontoon simplified stability proof test detailed in § 178.340 of this part, in the presence of a Coast Guard marine inspector, if it satisfies all of the following requirements: (1) The vessel carries not more than 49 passengers and does not make international voyages; (2) The vessel operates on Protected Waters only; (3) The vessel is constructed with only one deck; (4) The buoyant hull volume consists of two symmetric, fully enclosed hulls; (5) The cross section of each hull is circular or of wall-sided construction without tumblehome, and constant for at least 90 percent of the length of the hull; (6) The hulls contain no machinery or tanks; (7) The portion of the deck accessible to passengers does not extend beyond— (i) The outboard edge of the hulls, and (ii) The forward or the aft end of the hulls; (8) There is no deck more than 0.15 meters (6 inches) above any point on any of the buoyant hulls; (9) The distance between the centerlines of the hulls is not less than 1.83 meters (6 feet); and (10) Each hull has a beam or diameter, as applicable, of not less than 0.61 meters (2 feet). (c) For a vessel that carries not more than 49 passengers, carries no deck cargo, and is otherwise eligible to undergo the simplified stability proof test detailed in § 178.330 or § 178.340 of this part, the authority issuing the stability letter may— (1) Dispense with the requirements of the simplified stability proof test in § 178.330 or § 178.340 of this part when the vessel's stability can be adequately assessed by alternate means giving due consideration to each item that impacts a vessel's stability characteristics which include, but are not limited to, the form, arrangement, construction, number of decks, route, and operating restrictions of the vessel; or (2) Authorize a change in the requirements of the simplified stability proof test in either § 178.330 or § 178.340 of this part, when necessary to adequately assess the vessel's stability." 46:46:7.0.1.3.13.3.63.3,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,C,Subpart C—Intact Stability Standards,,§ 178.325 Intact stability requirements—monohull sailing vessels.,USCG,,,"[USCG-2007-0030, 75 FR 78088, Dec. 14, 2010]","(a) As permitted by § 178.310(c) of this part, a monohull sailing vessel may demonstrate compliance with paragraphs (b) or (c) of this section if it satisfies all of the following requirements: (1) It does not operate on exposed waters; (2) It only operates during the daylight hours; (3) It is of the usual type, rig, and hull form, excluding vessels without a weathertight deck, such as open boats; (4) It carries not more than 49 passengers; (5) It is not a sailing school vessel that carries a combined total of six or more sailing school students and instructors; (6) Its minimum downflooding angle is greater than 60 degrees; (7) It does not have a cockpit greater than 20 percent of the Length Over Deck; and (8) If equipped with a cockpit and operating on Partially Protected Waters, the cockpit must be self-bailing. (b) The vessel may undergo the simplified stability proof test detailed in § 178.330 of this part, in the presence of a Coast Guard marine inspector, if it does not have tumblehome at the deck, measured amidships, that exceeds 2 percent of the beam. (c) The cognizant Officer in Charge, Marine Inspection (OCMI) may perform operational tests to determine whether the vessel has adequate stability and satisfactory handling characteristics under sail for protected waters or partially protected waters. (d) The Commanding Officer, Marine Safety Center, may prescribe additional or different stability requirements for a broad, shallow draft vessel with little or no ballast outside the hull." 46:46:7.0.1.3.13.3.63.4,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,C,Subpart C—Intact Stability Standards,,§ 178.330 Simplified stability proof test (SST).,USCG,,,"[CGD 85-080, 61 FR 966, Jan. 10, 1996; 61 FR 20557, May 7, 1996, as amended at 62 FR 51356, Sept. 30, 1997; 62 FR 64306, Dec. 5, 1997; USCG-2007-0030, 75 FR 78088, Dec. 14, 2010]","(a) A vessel must be in the condition specified in this paragraph when a simplified stability proof test is performed. (1) The construction of the vessel is complete in all respects. (2) Ballast, if necessary, is in compliance with § 178.510 of this part and is on board and in place. (3) Each fuel and water tank is approximately three-quarters full. Any sewage tank should be either empty or full. (4) A weight equal to the total weight of all passengers, crew, and variable loads permitted on the vessel is on board and distributed so as to provide normal operating trim and to simulate the vertical center of gravity, causing the least stable condition that is likely to occur in service. The assumed weight per person of passengers and crew must be representative of the passengers and crew on board the vessel while engaged in the service intended. Unless the cognizant Officer in Charge, Marine Inspection (OCMI) permits or requires the use of other values in writing, weight and vertical center of gravity are to be assumed as follows: (i) The weight of primary lifesaving equipment should be simulated at its normal location, if not on board at the time of the test. (ii) The assumed weight per person is determined as provided by § 170.090 of this chapter. (iii) The weight and associated vertical center of gravity of variable loads must be included as appropriate for the service intended and documented in the stability information required by subpart B of this part. (iv) The vertical center for the total test weight must be at least 30 inches (760 millimeters) above the deck for seated passengers, and at least 39 inches (1.0 meter) above the deck for standing passengers. (v) If the vessel carries passengers on diving excursions, the total weight of diving gear must be included in the loaded condition and placed in its stowed position. Not less than 80 pounds (36.3 kilograms) should be assumed for each person for whom diving gear is provided. (vi) On vessels having one upper deck available to passengers above the main deck, the weight distribution must not be less severe than the following: Total Test Weight (W) = ________ Passenger Capacity of Upper Deck: Weight on Upper Deck = (Number of Passengers on Upper Deck) * (Wt per Passenger) * 1.33 Weight on Main Deck = Total Test Weight−Weight on Upper Deck. Total Test Weight (W) = ________ Passenger Capacity of Upper Deck: Weight on Upper Deck = (Number of Passengers on Upper Deck) * (Wt per Passenger) * 1.33 Weight on Main Deck = Total Test Weight−Weight on Upper Deck. (5) All non-return closures on cockpit scuppers or on weather deck drains must be kept open during the test. (b) A vessel must not exceed the limitations in paragraph (d) of this section, when subjected to the greater of the following heeling moments: M p = (W) (B p )/6; or M w = (P) (A) (H) Where: M p = passenger heeling moment in foot-pounds (kilogram-meters); M w = Wind heeling moment in foot-pounds (kilogram-meters) W = the total weight of persons other than required crew, plus the personal effects of those persons expected to be carried while aboard the vessel (total test weight) in pounds (meters); B p = the maximum transverse distance in feet (meters) of a deck that is accessible to passengers; A = Area, in square feet (square meters), of the projected lateral surface of the vessel above the waterline (including each projected area of the hull, superstructure, cargo, masts, area bounded by railings and canopies, but not protruding fixed objects such as antennas or running rigging). Where: M p = passenger heeling moment in foot-pounds (kilogram-meters); M w = Wind heeling moment in foot-pounds (kilogram-meters) W = the total weight of persons other than required crew, plus the personal effects of those persons expected to be carried while aboard the vessel (total test weight) in pounds (meters); B p = the maximum transverse distance in feet (meters) of a deck that is accessible to passengers; A = Area, in square feet (square meters), of the projected lateral surface of the vessel above the waterline (including each projected area of the hull, superstructure, cargo, masts, area bounded by railings and canopies, but not protruding fixed objects such as antennas or running rigging). (c) For sailing vessels the heeling moment used for this test must be the greater of the following: (1) Passenger heeling moment from paragraph (b) of this section. (2) Wind heeling moment from paragraph (b) of this section. (3) Wind heeling moment calculated from the wind heeling moment equation in paragraph (b) of this section, where: M w = wind heeling moment in kilogram-meters (foot-pounds); P = 4.9 kilograms/square meter (1.0 pounds/square foot) for both protected and partially protected waters. A = the windage area of the vessel in square meters (square feet) with all sails set and trimmed flat; H = height, in meters (feet), of the center of effort of area (A) above the waterline, measured up from the waterline; and M w = wind heeling moment in kilogram-meters (foot-pounds); P = 4.9 kilograms/square meter (1.0 pounds/square foot) for both protected and partially protected waters. A = the windage area of the vessel in square meters (square feet) with all sails set and trimmed flat; H = height, in meters (feet), of the center of effort of area (A) above the waterline, measured up from the waterline; and (d) A vessel must not exceed the following limits of heel: (1) On a flush deck vessel, not more than one-half of the freeboard may be immersed. (2) On a well deck vessel, not more than one-half of the freeboard may be immersed, except that, on a well deck vessel that operates on protected waters and has non-return scuppers or freeing ports, the full freeboard may be immersed if the full freeboard is not more than one-quarter of the distance from the waterline to the gunwale. (3) On a cockpit vessel, the maximum allowable immersion is calculated from the following equation: (i) On exposed waters— i = f(2L-1.5L′)/4L (ii) On protected or partially protected waters— i = f(2L−L′)/4L where: i = maximum allowable immersion in meters (feet); f = freeboard in meters (feet); L = length of the weather deck, in meters (feet); and L′ = length of cockpit in meters (feet). where: i = maximum allowable immersion in meters (feet); f = freeboard in meters (feet); L = length of the weather deck, in meters (feet); and L′ = length of cockpit in meters (feet). (4) On an open boat, not more than one quarter of the freeboard may be immersed. (5) On a flush deck sailing vessel, the full freeboard may be immersed. (6) On a non-sailing flush deck catamaran that is propelled by mechanical means, not more than one-third of the freeboard or one-third of the draft, whichever is less, may be immersed. (7) In no case may the angle of heel exceed 14 degrees. (e) The limits of heel must be measured at: (1) The point of minimum freeboard; or (2) At a point three-quarters of the vessel's length from the bow if the point of minimum freeboard is aft of this point. (f) When demonstrating compliance with paragraph (d) of this section, the freeboard must be measured as follows: (1) For a flush deck or well deck vessel, the freeboard must be measured to the top of the weatherdeck at the side of the vessel; and (2) For a cockpit vessel or for an open boat, the freeboard must be measured to the top of the gunwale. (g) A ferry must also be tested in a manner acceptable to the cognizant OCMI to determine whether the trim or heel during loading or unloading will submerge the deck edge. A ferry passes this test if, with the total number of passengers and the maximum vehicle weight permitted on board, the deck edge is not submerged during loading or unloading of the vessel." 46:46:7.0.1.3.13.3.63.5,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,C,Subpart C—Intact Stability Standards,,§ 178.340 Stability standards for pontoon vessels on protected waters.,USCG,,,"[USCG-2007-0030, 75 FR 78089, Dec. 14, 2010]","(a) A pontoon vessel meeting the applicability requirements of § 178.320 of this part must be in the condition described in § 178.330(a) of this part when the PSST is performed, except that fuel, water and sewage tanks should either be empty or filled to 100 percent capacity, whichever is more conservative. (b) A pontoon vessel must not exceed the limitations in paragraph (c) of this section when subjected to the greater of the following heeling moments: M pc = [(W)(B p −K)]/2; or M w = (P) (A) (H) Where: M pc = passenger and crew heeling moment in foot-pounds (kilogram-meters); W = the total weight of passengers and crew aboard (total test weight) in pounds (kilograms); B p = the maximum transverse distance of the deck accessible to passengers in feet (meters); K = 2.0 feet (0.61 meters); M w = Wind heeling moment in foot-pounds (kilogram-meters) P = Wind pressure of 7.5 pounds/square foot (36.6 kilograms/square meter); A = Area, in square feet (square meters), of the projected lateral surface of the vessel above the waterline (including each projected area of the pontoons, superstructure and area bounded by railings and structural canopies); and H = Height, in feet (meters), of the center of area (A) above the waterline, measured up from the waterline. Where: M pc = passenger and crew heeling moment in foot-pounds (kilogram-meters); W = the total weight of passengers and crew aboard (total test weight) in pounds (kilograms); B p = the maximum transverse distance of the deck accessible to passengers in feet (meters); K = 2.0 feet (0.61 meters); M w = Wind heeling moment in foot-pounds (kilogram-meters) P = Wind pressure of 7.5 pounds/square foot (36.6 kilograms/square meter); A = Area, in square feet (square meters), of the projected lateral surface of the vessel above the waterline (including each projected area of the pontoons, superstructure and area bounded by railings and structural canopies); and H = Height, in feet (meters), of the center of area (A) above the waterline, measured up from the waterline. (c) With the appropriate heeling moment applied to the most adversely affected side of the vessel, the remaining exposed cross-sectional area of the pontoon must be equal to or greater than both— (1) The cross-sectional area submerged due to the load shift (for an example, see Figure 178.340(c)(1) of this section); and (2) One-quarter of the cross-sectional area on one pontoon. (d) A pontoon vessel must also be tested to determine whether trimming moments will submerge the bow or stern of the buoyant hull. The top of any pontoon must not be submerged at any location, as indicated in Figure 178.340(d) of this section, with the total test weight (W) located on the centerline and positioned as far forward or aft on the deck as practicable, whichever position results in the least freeboard." 46:46:7.0.1.3.13.4.63.1,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,D,Subpart D—Drainage of Weather Decks,,§ 178.410 Drainage of flush deck vessels.,USCG,,,"[CGD 85-080, 61 FR 966, Jan. 10, 1996, as amended at 62 FR 51357, Sept. 30, 1997]","(a) Except as provided in paragraph (b) of this section, the weather deck on a flush deck vessel must be watertight and have no obstruction to overboard drainage. (b) Each flush deck vessel may have solid bulwarks in the forward one-third length of the vessel if: (1) The bulwarks do not form a well enclosed on all sides; and (2) The foredeck of the vessel has sufficient sheer to ensure drainage aft." 46:46:7.0.1.3.13.4.63.2,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,D,Subpart D—Drainage of Weather Decks,,§ 178.420 Drainage of cockpit vessels.,USCG,,,,"(a) Except as follows, the cockpit on a cockpit vessel may be watertight: (1) A cockpit may have companionways if the companionway openings have watertight doors, or weathertight doors and coamings which meet § 179.360 of this subchapter. (2) A cockpit may have ventilation openings along its inner periphery if the vessel operates only on protected or partially protected waters. (b) The cockpit deck of a cockpit vessel that operates on exposed or partially protected waters must be at least 255 millimeters (10 inches) above the deepest load waterline unless the vessel complies with: (1) The intact stability requirements of §§ 170.170, 170.173, 171.050, 171.055, and 171.057 in subchapter S of this chapter; (2) The Type II subdivision requirements in §§ 171.070, 171.072, and 171.073 in subchapter S of this chapter; and (3) The damage stability requirements in § 171.080 in subchapter S of this chapter. (c) The cockpit deck of a cockpit vessel that does not operate on exposed or partially protected waters must be located as high above the deepest load waterline as practicable. (d) The cockpit must be self-bailing. Scuppers or freeing ports for the cockpit deck of a cockpit vessel must: (1) Be located to allow rapid clearing of water in all probable conditions of list and trim; (2) Have a combined drainage area of at least the area required by § 178.450 of this part; and (3) If the deck is less than 255 millimeters (10 inches) above the deepest load waterline of the vessel, be fitted with non-return devices." 46:46:7.0.1.3.13.4.63.3,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,D,Subpart D—Drainage of Weather Decks,,§ 178.430 Drainage of well deck vessels.,USCG,,,,"(a) The weather deck on a well deck vessel must be watertight. (b) The area required on a well deck vessel for drainage of well formed by the bulwarks shall be determined by § 178.450. (c) The freeing ports or scuppers on a well deck vessel must be located to allow rapid clearing of water in all probable conditions of list and trim. (d) The deck of well deck vessel that operates on exposed or partially protected waters must be at least 255 millimeters (10 inches) above the deepest load waterline unless the vessel complies with: (1) The intact stability requirements of §§ 170.170, 170.173, 171.050, 171.055, and 171.057 in subchapter S of this chapter; (2) The Type II subdivision requirements in §§ 171.070, 171.072, and 171.073 in subchapter S of this chapter; and (3) The damage stability requirements in § 171.080 in subchapter S of this chapter." 46:46:7.0.1.3.13.4.63.4,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,D,Subpart D—Drainage of Weather Decks,,§ 178.440 Drainage of open boats.,USCG,,,,The deck within the hull of an open boat must drain to the bilge. Overboard drainage of the deck is not permitted. 46:46:7.0.1.3.13.4.63.5,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,D,Subpart D—Drainage of Weather Decks,,§ 178.450 Calculation of drainage area for cockpit and well deck vessels.,USCG,,,"[CGD 85-080, 61 FR 966, Jan. 10, 1996; 61 FR 20557, May 7, 1996; USCG-2022-0323, 88 FR 10032, Feb. 16, 2023 ]","(a) The drainage area required on a vessel must be computed using the following formula: For protected waters required drainage = .1 × Basic Drainage For partially protected waters required drainage = .5 × Basic Drainage For exposed waters required drainage = Basic Drainage where: Basic Drainage area in centimeters 2 = 4389.12 × [(Recess Volume × Recess Ratio) + (Weather Deck Volume × Weather Deck Ratio)]; or Basic Drainage area in inch 2 = (Recess Volume × Recess Ratio) + (Weather Deck Volume × Weather Deck Ratio) Recess Volume = (B R × D R ) − V R B R = average height in centimeters (feet) of the bulwark above the well deck or cockpit deck; D R = total deck area of the cockpit or well deck in the after 2/3 of the vessel length (LOD) measured in centimeters 2 (feet 2 ). V R = volume of any weather tight structure below the bulwark of the well deck or cockpit deck. B R = average height in centimeters (feet) of the bulwark above the well deck or cockpit deck; D R = total deck area of the cockpit or well deck in the after 2/3 of the vessel length (LOD) measured in centimeters 2 (feet 2 ). V R = volume of any weather tight structure below the bulwark of the well deck or cockpit deck. Recess Ratio = L R / L C L R = the length of the recess in the after 2/3 vessel length (LOD). L C = 2/3 vessel length (LOD). L R = the length of the recess in the after 2/3 vessel length (LOD). L C = 2/3 vessel length (LOD). Weather Deck Volume = (B D × D D ) − V S B D = average height in centimeters (feet) of the bulwark above the weather deck; D D = total deck area of the weather deck adjacent to bulwarks but not in way of the cockpit or well deck in the after 2/3 of the vessel length (LOD) measured in centimenters 2 (feet 2 ). V S = volume of any weather tight superstructure below the bulwark on the weather deck located within D D . B D = average height in centimeters (feet) of the bulwark above the weather deck; D D = total deck area of the weather deck adjacent to bulwarks but not in way of the cockpit or well deck in the after 2/3 of the vessel length (LOD) measured in centimenters 2 (feet 2 ). V S = volume of any weather tight superstructure below the bulwark on the weather deck located within D D . Weather Deck Ratio = L D / L C L D = the length of the weather deck bulwark in the after 2/3 of the vessel length (LOD). L C = 2/3 vessel length (LOD). L D = the length of the weather deck bulwark in the after 2/3 of the vessel length (LOD). L C = 2/3 vessel length (LOD). (b) Vessels with bulwarks in the forward part of the vessel shall not form a well with the deckhouse which retains water." 46:46:7.0.1.3.13.5.63.1,46,Shipping,I,T,178,PART 178—INTACT STABILITY AND SEAWORTHINESS,E,Subpart E—Special Installations,,§ 178.510 Ballast.,USCG,,,,"(a) Any solid fixed ballast used to comply with the requirements of parts 170, 171, 178, and 179 of this chapter must be: (1) Stowed in a manner that prevents shifting of the ballast; and (2) Installed to the satisfaction of the cognizant OCMI. (b) Solid fixed ballast may not be located forward of the collision bulkhead unless the installation and arrangement of the ballast and the collision bulkhead minimizes the risk of the ballast penetrating the bulkhead in a collision. (c) Solid fixed ballast may not be removed from a vessel or relocated unless approved by the cognizant OCMI except that ballast may be temporarily moved for a vessel examination or repair if it is replaced to the satisfaction of the OCMI. (d) Water ballast, either as an active system or permanent, must be approved by the Commanding Officer, Marine Safety Center." 49:49:3.1.1.1.1.0.1.1,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,,,,§ 178.1 Purpose and scope.,PHMSA,,,"[Amdt. 178-40, 42 FR 2689, Jan. 13, 1977. Redesignated by Amdt. 178-97, 55 FR 52715, Dec. 21, 1990]",This part prescribes the manufacturing and testing specifications for packaging and containers used for the transportation of hazardous materials in commerce. 49:49:3.1.1.1.1.0.1.2,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,,,,§ 178.2 Applicability and responsibility.,PHMSA,,,"[Amdt. 178-97, 55 FR 52715, Dec. 21, 1990; 56 FR 66284, Dec. 20, 1991, as amended by Amdt. 178-106, 59 FR 67519, Dec. 29, 1994; Amdt. 178-117, 62 FR 14338, Mar. 26, 1997; 68 FR 45041, July 31, 2003; 69 FR 34612, June 22, 2004; 75 FR 5395, Feb. 2, 2010; 75 FR 60339, Sept. 30, 2010; 78 FR 1118, Jan. 7, 2013; 78 FR 15328, Mar. 11, 2013]","(a) Applicability. (1) The requirements of this part apply to packagings manufactured— (i) To a DOT specification, regardless of country of manufacture; or (ii) To a UN standard, for packagings manufactured within the United States. For UN standard packagings manufactured outside the United States, see § 173.24(d)(2) of this subchapter. For UN standard packagings for which standards are not prescribed in this part, see § 178.3(b). (2) A manufacturer of a packaging subject to the requirements of this part is primarily responsible for compliance with the requirements of this part. However, any person who performs a function prescribed in this part shall perform that function in accordance with this part. (b) Specification markings. When this part requires that a packaging be marked with a DOT specification or UN standard marking, marking of the packaging with the appropriate DOT or UN markings is the certification that— (1) Except as otherwise provided in this section, all requirements of the DOT specification or UN standard, including performance tests, are met; and (2) All functions performed by, or on behalf of, the person whose name or symbol appears as part of the marking conform to requirements specified in this part. (c) Notification. (1) Except as specifically provided in §§ 178.337-18, 178.338-19, and 178.345-15 of this part, the manufacturer or other person certifying compliance with the requirements of this part, and each subsequent distributor of that packaging must: (i) Notify each person to whom that packaging is transferred— (A) Of all requirements in this part not met at the time of transfer, and (B) With information specifying the type(s) and dimensions of the closures, including gaskets and any other components needed to ensure that the packaging is capable of successfully passing the applicable performance tests. This information must include any procedures to be followed, including closure instructions for inner packagings and receptacles, to effectively assemble and close the packaging for the purpose of preventing leakage in transportation. Closure instructions must provide for a consistent and repeatable means of closure that is sufficient to ensure the packaging is closed in the same manner as it was tested. For packagings sold or represented as being in conformance with the requirements of this subchapter applicable to transportation by aircraft, this information must include relevant guidance to ensure that the packaging, as prepared for transportation, will withstand the pressure differential requirements in § 173.27 of this subchapter. (ii) Retain copies of each written notification for at least one year from date of issuance; and (iii) Make copies of all written notifications available for inspection by a representative of the Department. (2) The notification required in accordance with this paragraph (c) may be in writing or by electronic means, including e-mailed transmission or transmission on a CD or similar device. If a manufacturer or subsequent distributor of the packaging utilizes electronic means to make the required notifications, the notification must be specific to the packaging in question and must be in a form that can be printed in hard copy by the person receiving the notification. (d) Except as provided in paragraph (c) of this section, a packaging not conforming to the applicable specifications or standards in this part may not be marked to indicate such conformance. (e) Definitions. For the purpose of this part— Manufacturer means the person whose name and address or symbol appears as part of the specification markings required by this part or, for a packaging marked with the symbol of an approval agency, the person on whose behalf the approval agency certifies the packaging. Specification markings mean the packaging identification markings required by this part including, where applicable, the name and address or symbol of the packaging manufacturer or approval agency. (f) No packaging may be manufactured or marked to a packaging specification that was in effect on September 30, 1991, and that was removed from this part 178 by a rule published in the Federal Register on December 21, 1990 and effective October 1, 1991." 49:49:3.1.1.1.1.0.1.3,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,,,,§ 178.3 Marking of packagings.,PHMSA,,,"[Amdt. 178-97, 55 FR 52716, Dec. 21, 1990; 56 FR 66284, Dec. 20, 1991, as amended by Amdt. 178-106, 59 FR 67519, Dec. 29, 1994; Amdt. 178-113, 61 FR 21102, May 9, 1996; 65 FR 50462, Aug. 18, 2000; 66 FR 45386, Aug. 28, 2001; 67 FR 61015, Sept. 27, 2002; 68 FR 75748, Dec. 31, 2003; 70 FR 73166, Dec. 9, 2005; 78 FR 14714, Mar. 7, 2013; 87 FR 44999, July 26, 2022]","(a) Each packaging represented as manufactured to a DOT specification or a UN standard must be marked on a non-removable component of the packaging with specification markings conforming to the applicable specification, and with the following: (1) In an unobstructed area, with letters, and numerals identifying the standards or specification (e.g. UN 1A1, DOT 4B240ET, etc.). (2) Unless otherwise specified in this part, the name and address or symbol of the packaging manufacturer or the person certifying compliance with a UN standard. Symbols, if used, must be registered with the Associate Administrator. Unless authorized in writing by the holder of the symbol, symbols must represent either the packaging manufacturer or the approval agency responsible for providing the most recent certification for the packaging through design certification testing or periodic retesting, as applicable. Duplicative symbols are not authorized. (3) The markings must be stamped, embossed, burned, printed or otherwise marked on the packaging to provide adequate accessibility, permanency, contrast, and legibility so as to be readily apparent and understood. (4) Unless otherwise specified, letters and numerals must be at least 12.0 mm (0.47 inches) in height except for packagings of less than or equal to 30 L (7.9 gallons) capacity for liquids or 30 kg (66 pounds) maximum net mass for solids the height must be at least 6.0 mm (0.2 inches). For packagings having a capacity of 5 L (1.3 gallons) or less or of 5 kg (11 pounds) maximum net mass, letters and numerals must be of an appropriate size. (5) For packages with a gross mass of more than 30 kg (66 pounds), the markings or a duplicate thereof must appear on the top or on a side of the packaging. (b) A UN standard packaging for which the UN standard is set forth in this part may be marked with the United Nations symbol and other specification markings only if it fully conforms to the requirements of this part. A UN standard packaging for which the UN standard is not set forth in this part may be marked with the United Nations symbol and other specification markings for that standard as provided in the ICAO Technical Instructions or the IMDG Code subject to the following conditions: (1) The U.S. manufacturer must establish that the packaging conforms to the applicable provisions of the ICAO Technical Instructions (IBR, see § 171.7 of this subchapter) or the IMDG Code (IBR, see § 171.7 of this subchapter), respectively. (2) If an indication of the name of the manufacturer or other identification of the packaging as specified by the competent authority is required, the name and address or symbol of the manufacturer or the approval agency certifying compliance with the UN standard must be entered. Symbols, if used, must be registered with the Associate Administrator. (3) The letters “USA” must be used to indicate the State authorizing the allocation of the specification marks if the packaging is manufactured in the United States. (c) Where a packaging conforms to more than one UN standard or DOT specification, the packaging may bear more than one marking, provided the packaging meets all the requirements of each standard or specification. Where more than one marking appears on a packaging, each marking must appear in its entirety. (d) No person may mark or otherwise certify a packaging or container as meeting the requirements of a manufacturing special permit unless that person is the holder of or a party to that special permit, an agent of the holder or party for the purpose of marking or certification, or a third party tester." 49:49:3.1.1.1.1.10.1.1,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.600 Purpose and scope.,PHMSA,,,"[Amdt. 178-97, 55 FR 52717, Dec. 21, 1990, as amended by Amdt. 178-99, 58 FR 51534, Oct. 1, 1993]",This subpart prescribes certain testing requirements for performance-oriented packagings identified in subpart L of this part. 49:49:3.1.1.1.1.10.1.10,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.609 Test requirements for packagings for infectious substances.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended by Amdt. 178-111, 60 FR 48787, Sept. 20, 1995; 67 FR 53143, Aug. 14, 2002; 69 FR 54046, Sept. 7, 2004; 87 FR 45000, July 26, 2022; 89 FR 25490, Apr. 10, 2024]","(a) Samples of each packaging must be prepared for testing as described in paragraph (b) of this section and then subjected to the tests in paragraphs (d) through (i) of this section. (b) Samples of each packaging must be prepared as for transport except that a liquid or solid infectious substance should be replaced by water or, where conditioning at −18 °C (0 °F) is specified, by water/antifreeze. Each primary receptacle must be filled to 98 percent capacity. Packagings for live animals should be tested with the live animal being replaced by an appropriate dummy of similar mass. (c) Packagings prepared as for transport must be subjected to the tests in Table I of this paragraph (c), which, for test purposes, categorizes packagings according to their material characteristics. For outer packagings, the headings in Table I relate to fiberboard or similar materials whose performance may be rapidly affected by moisture; plastics that may embrittle at low temperature; and other materials, such as metal, for which performance is not significantly affected by moisture or temperature. Where a primary receptacle and a secondary packaging of an inner packaging are made of different materials, the material of the primary receptacle determines the appropriate test. In instances where a primary receptacle is made of more than one material, the material most likely to be damaged determines the appropriate test. Table I—Tests Required (d) Samples must be subjected to free-fall drops onto a rigid, nonresilient, flat, horizontal surface from a height of 9 m (30 feet). The drops must be performed as follows: (1) Where the samples are in the shape of a box, five samples must be dropped, one in each of the following orientation: (i) Flat on the base; (ii) Flat on the top; (iii) Flat on the longest side; (iv) Flat on the shortest side; and (v) On a corner. (2) Where the samples are in the shape of a drum or jerrican, three samples must be dropped, one in each of the following orientations: (i) Diagonally on the top edge, with the center of gravity directly above the point of impact; (ii) Diagonally on the base edge; and (iii) Flat on the body or side. (3) While the sample should be released in the required orientation, it is accepted that for aerodynamic reasons the impact may not take place in that orientation. (4) Following the appropriate drop sequence, there must be no leakage from the primary receptacle(s) which should remain protected by absorbent material in the secondary packaging. (e) The samples must be subjected to a water spray to simulate exposure to rainfall of approximately 50 mm (2 inches) per hour for at least one hour. They must then be subjected to the test described in paragraph (d) of this section. (f) The sample must be conditioned in an atmosphere of −18 °C (0 °F) or less for a period of at least 24 hours and within 15 minutes of removal from that atmosphere be subjected to the test described in paragraph (d) of this section. Where the sample contains dry ice, the conditioning period may be reduced to 4 hours. (g) Where packaging is intended to contain dry ice, an additional drop test to that specified in paragraph (d), and when appropriate, paragraph (e) or (f) of this section must be performed on one sample in one of the orientations described in paragraph (d)(1) or (2) of this section, as appropriate, which is most likely to result in failure of the packaging. The sample must be stored so that all the dry ice dissipates prior to being subjected to the drop test. (h) Packagings with a gross mass of 7 kg (15 pounds) or less should be subjected to the tests described in paragraph (h)(1) of this section and packagings with a gross mass exceeding 7 kg (15 pounds) to the tests in paragraph (h)(2) of this section. (1) Samples must be placed on a level, hard surface. A cylindrical steel rod with a mass of at least 7 kg (15 pounds), a diameter not exceeding 38 mm (1.5 inches), and, at the impact end edges, a radius not exceeding 6 mm (0.2 inches), must be dropped in a vertical free fall from a height of 1 m (3 feet), measured from the impact end of the sample's impact surface. One sample must be placed on its base. A second sample must be placed in an orientation perpendicular to that used for the first. In each instance, the steel rod must be aimed to impact the primary receptacle(s). For a successful test, there must be no leakage from the primary receptacle(s) following each impact. (2) Samples must be dropped onto the end of a cylindrical steel rod. The rod must be set vertically in a level, hard surface. It must have a diameter of 38 mm (1.5 inches) and a radius not exceeding 6 mm (0.2 inches) at the edges of the upper end. The rod must protrude from the surface a distance at least equal to that between the primary receptacle(s) and the outer surface of the outer packaging with a minimum of 200 mm (7.9 inches). One sample must be dropped in a vertical free fall from a height of 1 m (3 feet), measured from the top of the steel rod. A second sample must be dropped from the same height in an orientation perpendicular to that used for the first. In each instance, the packaging must be oriented so the steel rod will impact the primary receptacle(s). For a successful test, there must be no leakage from the primary receptacle(s) following each impact. (i) Variations. The following variations in the primary receptacles placed within the secondary packaging are allowed without additional testing of the completed package. An equivalent level of performance must be maintained. (1) Variation 1. Primary receptacles of equivalent or smaller size as compared to the tested primary receptacles may be used provided they meet all of the following conditions: (i) The primary receptacles are of similar design to the tested primary receptacle (e.g., shape: round, rectangular, etc.). (ii) The material of construction of the primary receptacle (glass, plastics, metal, etc.) offers resistance to impact and a stacking force equal to or greater than that of the originally tested primary receptacle. (iii) The primary receptacles have the same or smaller openings and the closure is of similar design (e.g., screw cap, friction lid, etc.). (iv) Sufficient additional cushioning material is used to fill void spaces and to prevent significant movement of the primary receptacles. (v) Primary receptacles are oriented within the intermediate packaging in the same manner as in the tested package. (2) Variation 2. A lesser number of the tested primary receptacles, or of the alternative types of primary receptacles identified in paragraph (i)(1) of this section, may be used provided sufficient cushioning is added to fill the void space(s) and to prevent significant movement of the primary receptacles. (3) Variation 3. Primary receptacles of any type may be placed within a secondary packaging and shipped without testing in the outer packaging provided all of the following conditions are met: (i) The secondary and outer packaging combination must be successfully tested in accordance with paragraphs (a) through (h) of this section with fragile (e.g., glass) inner receptacles. (ii) The total combined gross weight of inner receptacles may not exceed one-half the gross weight of inner receptacles used for the drop test in paragraph (d) of this section. (iii) The thickness of cushioning material between inner receptacles and between inner receptacles and the outside of the secondary packaging may not be reduced below the corresponding thicknesses in the originally tested packaging. If a single inner receptacle was used in the original test, the thickness of cushioning between the inner receptacles must be no less than the thickness of cushioning between the outside of the secondary packaging and the inner receptacle in the original test. When either fewer or smaller inner receptacles are used (as compared to the inner receptacles used in the drop test), sufficient additional cushioning material must be used to fill the void. (iv) The outer packaging must pass the stacking test in § 178.606 while empty. The total weight of identical packages must be based on the combined mass of inner receptacles used in the drop test in paragraph (d) of this section. (v) For inner receptacles containing liquids, an adequate quantity of absorbent material must be present to absorb the entire liquid contents of the inner receptacles. (vi) If the outer packaging is intended to contain inner receptacles for liquids and is not leakproof, or is intended to contain inner receptacles for solids and is not sift proof, a means of containing any liquid or solid contents in the event of leakage must be provided. This can be a leakproof liner, plastic bag, or other equally effective means of containment. (vii) In addition, the marking required in § 178.503(f) of this subchapter must be followed by the letter “U”." 49:49:3.1.1.1.1.10.1.2,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.601 General requirements.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66285, Dec. 20, 1991; 57 FR 45465, Oct. 1, 1992; Amdt. 178-102, 59 FR 28494, June 2, 1994; Amdt. 178-106, 59 FR 67521, 67522, Dec. 29, 1994; Amdt. 178-117, 61 FR 50628, Sept. 26, 1996; 66 FR 45386, Aug. 28, 2001; 67 FR 53143, Aug. 14, 2002; 68 FR 75758, Dec. 31, 2003; 68 FR 61942, Oct. 30, 2003; 75 FR 5396, Feb. 2, 2010; 75 FR 60339, Sept. 30, 2010; 77 FR 60944, Oct. 5, 2012; 78 FR 1118, Jan. 7, 2013; 78 FR 14715, Mar. 7, 2013; 78 FR 65487, Oct. 31, 2013; 85 FR 27901, May 11, 2020; 87 FR 79784, Dec. 27, 2022; 89 FR 15666, Mar. 4, 2024 ]","(a) General. The test procedures prescribed in this subpart are intended to ensure that packages containing hazardous materials can withstand normal conditions of transportation and are considered minimum requirements. Each packaging must be manufactured and assembled so as to be capable of successfully passing the prescribed tests and of conforming to the requirements of § 173.24 of this subchapter at all times while in transportation. (b) Responsibility. It is the responsibility of the packaging manufacturer to assure that each package is capable of passing the prescribed tests. To the extent that a package assembly function, including final closure, is performed by the person who offers a hazardous material for transportation, that person is responsible for performing the function in accordance with §§ 173.22 and 178.2 of this subchapter. (c) Definitions. For the purpose of this subpart: (1) Design qualification testing is the performance of the tests prescribed in § 178.603, § 178.604, § 178.605, § 178.606, § 178.607, § 178.608, or § 178.609, as applicable, for each new or different packaging, at the start of production of that packaging. (2) Periodic retesting is the performance of the drop, leakproofness, hydrostatic pressure, and stacking tests, as applicable, as prescribed in § 178.603, § 178.604, § 178.605, or § 178.606, respectively, at the frequency specified in paragraph (e) of this section. For infectious substances packagings required to meet the requirements of § 178.609, periodic retesting is the performance of the tests specified in § 178.609 at the frequency specified in paragraph (e) of this section. (3) Production testing is the performance of the leakproofness test prescribed in § 178.604 of this subpart on each single or composite packaging intended to contain a liquid. (4) A different packaging is one that differs ( i.e. , is not identical) from a previously produced packaging in structural design, size, material of construction, wall thickness or manner of construction but does not include: (i) A packaging which differs only in surface treatment; (ii) A combination packaging which differs only in that the outer packaging has been successfully tested with different inner packagings. A variety of such inner packagings may be assembled in this outer packaging without further testing; (iii) A plastic packaging which differs only with regard to additives which conform to § 178.509(b)(3) or § 178.517(b) (4) or (5) of this part; (iv) A combination packaging with inner packagings conforming to the provisions of paragraph (g) of this section; (v) Packagings which differ from the design type only in their lesser design height; or (vi) For a steel drum, variations in design elements which do not constitute a different design type under the provisions of paragraph (g)(8) of this section. (d) Design qualification testing. The packaging manufacturer shall achieve successful test results for the design qualification testing at the start of production of each new or different packaging. (e) Periodic retesting. The packaging manufacturer must achieve successful test results for the periodic retesting at intervals established by the manufacturer of sufficient frequency to ensure that each packaging produced by the manufacturer is capable of passing the design qualification tests. Changes in retest frequency are subject to the approval of the Associate Administrator for Hazardous Materials Safety. For single or composite packagings, the periodic retests must be conducted at least once every 12 months. For combination packagings, the periodic retests must be conducted at least once every 24 months. For infectious substances packagings, the periodic retests must be conducted at least once every 24 months. (f) Test samples. The manufacturer shall conduct the design qualification and periodic tests prescribed in this subpart using random samples of packagings, in the numbers specified in the appropriate test section. In addition, the leakproofness test, when required, shall be performed on each packaging produced by the manufacturer, and each packaging prior to reuse under § 173.28 of this subchapter, by the reconditioner. (g) Selective testing. The selective testing of packagings that differ only in minor respects from a tested type is permitted as described in this section. For air transport, packagings must comply with § 173.27(c)(1) and (c)(2) of this subchapter. (1) Selective testing of combination packagings. Variation 1. Variations are permitted in inner packagings of a tested combination package, without further testing of the package, provided an equivalent level of performance is maintained and, when a package is altered under Variation 1 after October 1, 2010, the methodology used to determine that the inner packaging, including closure, maintains an equivalent level of performance is documented in writing by the person certifying compliance with this paragraph and retained in accordance with paragraph (l) of this section. Permitted variations are as follows: (i) Inner packagings of equivalent or smaller size may be used provided— (A) The inner packagings are of similar design to the tested inner packagings ( i.e. , shape—round, rectangular, etc.); (B) The material of construction of the inner packagings (glass, plastic, metal, etc.) offers resistance to impact and stacking forces equal to or greater than that of the originally tested inner packaging; (C) The inner packagings have the same or smaller openings and the closure is of similar design (e.g., screw cap, friction lid, etc.); (D) Sufficient additional cushioning material is used to take up void spaces and to prevent significant moving of the inner packagings; (E) Inner packagings are oriented within the outer packaging in the same manner as in the tested package; and, (F) The gross mass of the package does not exceed that originally tested. (ii) A lesser number of the tested inner packagings, or of the alternative types of inner packagings identified in paragraph (g)(1)(i) of this section, may be used provided sufficient cushioning is added to fill void space(s) and to prevent significant moving of the inner packagings. (2) Selective testing of combination packagings. Variation 2. Articles or inner packagings of any type, for solids or liquids, may be assembled and transported without testing in an outer packaging under the following conditions: (i) The outer packaging must have been successfully tested in accordance with § 178.603 with fragile (e.g. glass) inner packagings containing liquids at the Packing Group I drop height; (ii) The total combined gross mass of inner packagings may not exceed one-half the gross mass of inner packagings used for the drop test; (iii) The thickness of cushioning material between inner packagings and between inner packagings and the outside of the packaging may not be reduced below the corresponding thickness in the originally tested packaging; and when a single inner packaging was used in the original test, the thickness of cushioning between inner packagings may not be less than the thickness of cushioning between the outside of the packaging and the inner packaging in the original test. When either fewer or smaller inner packagings are used (as compared to the inner packagings used in the drop test), sufficient additional cushioning material must be used to take up void spaces. (iv) The outer packaging must have successfully passed the stacking test set forth in § 178.606 of this subpart when empty, i.e., without either inner packagings or cushioning materials. The total mass of identical packages must be based on the combined mass of inner packagings used for the drop test; (v) Inner packagings containing liquids must be completely surrounded with a sufficient quantity of absorbent material to absorb the entire liquid contents of the inner packagings; (vi) When the outer packaging is intended to contain inner packagings for liquids and is not leakproof or is intended to contain inner packagings for solids and is not siftproof, a means of containing any liquid or solid contents in the event of leakage must be provided in the form of a leakproof liner, plastic bag, or other equally efficient means of containment. For packagings containing liquids, the absorbent material required in paragraph (g)(2)(v) of this section must be placed inside as the means of containing liquid contents; and (vii) Packagings must be marked in accordance with § 178.503 of this part as having been tested to Packing Group I performance for combination packagings. The marked maximum gross mass may not exceed the sum of the mass of the outer packaging plus one half the mass of the filled inner packagings of the tested combination packaging. In addition, the marking required by § 178.503(a)(2) of this part must include the letter “V”. (3) Variation 3. Packagings other than combination packagings which are produced with reductions in external dimensions ( i.e. , length, width or diameter) of up to 25 percent of the dimensions of a tested packaging may be used without further testing provided an equivalent level of performance is maintained. The packagings must, in all other respects (including wall thicknesses), be identical to the tested design-type. The marked gross mass (when required) must be reduced in proportion to the reduction in volume. (4) Variation 4. Variations are permitted in outer packagings of a tested design-type combination packaging, without further testing, provided an equivalent level of performance is maintained, as follows: (i) Each external dimension (length, width and height) is less than or equal to the corresponding dimension of the tested design-type; (ii) The structural design of the tested outer packaging ( i.e. , methods of construction, materials of construction, strength characteristics of materials of construction, method of closure and material thicknesses) is maintained; (iii) The inner packagings are identical to the inner packagings used in the tested design type except that their size and mass may be less; and they are oriented within the outer packaging in the same manner as in the tested packaging; (iv) The same type or design of absorbent materials, cushioning materials and any other components necessary to contain and protect inner packagings, as used in the tested design type, are maintained. The thickness of cushioning material between inner packagings and between inner packagings and the outside of the packaging may not be less than the thicknesses in the tested design type packaging; and (v) Sufficient additional cushioning material is used to take up void spaces and to prevent significant moving of the inner packagings. An outer packaging qualifying for use in transport in accordance with all of the above conditions may also be used without testing to transport inner packagings substituted for the originally tested inner packagings in accordance with the conditions set out in Variation 1 in paragraph (g)(1) of this section. (5) Variation 5. Single packagings ( i.e. , non-bulk packagings other than combination packagings), that differ from a tested design type only to the extent that the closure device or gasketing differs from that used in the originally tested design type, may be used without further testing, provided an equivalent level of performance is maintained, subject to the following conditions (the qualifying tests): (i) A packaging with the replacement closure devices or gasketing must successfully pass the drop test specified in § 178.603 in the orientation which most severely tests the integrity of the closure or gasket; (ii) When intended to contain liquids, a packaging with the replacement closure devices or gasketing must successfully pass the leakproofness test specified in § 178.604, the hydrostatic pressure test specified in § 178.605, and the stacking test specified in § 178.606. Replacement closures and gasketings qualified under the above test requirements are authorized without additional testing for packagings described in paragraph (g)(3) of this section. Replacement closures and gasketings qualified under the above test requirements also are authorized without additional testing for different tested design types packagings of the same type as the originally tested packaging, provided the original design type tests are more severe or comparable to tests which would otherwise be conducted on the packaging with the replacement closures or gasketings. (For example: The packaging used in the qualifying tests has a lesser packaging wall thickness than the packaging with replacement closure devices or gasketing; the gross mass of the packaging used in the qualifying drop test equals or exceeds the mass for which the packaging with replacement closure devices or gasketing was tested; the packaging used in the qualifying drop test was dropped from the same or greater height than the height from which the packaging with replacement closure devices or gasketing was dropped in design type tests; and the specific gravity of the substance used in the qualifying drop test was the same or greater than the specific gravity of the liquid used in the design type tests of the packaging with replacement closure devices or gasketing.) (6) Selective testing of combination packagings for articles containing small arms ammunition: Variation 6. Variations in inner and intermediate packagings are permitted in packages for articles containing Cartridges, small arms (UN0012); Cartridges for tools, blank (UN0014); Primers, cap type (UN0044); and Cases, cartridge empty with primer (UN0055) packed in inner packages without further testing of the package under the following conditions: (i) The package has been tested containing only the articles to be transported without intermediate containment; (ii) The outer packaging must have passed the stacking test set forth in § 178.606 when empty, i.e., without cushioning or inner or intermediate packagings, with the test mass of identical packages being the mass of the package filled with the articles; (iii) Only articles tested without intermediate containment may be transported; however, a variety of articles tested in this fashion may be assembled in a package with intermediate containment; (iv) No articles demonstrate a loss of material in testing; and (v) The completed package does not exceed the marked maximum gross mass of the package. (7) The provisions in Variations 1, 2, and 4 in paragraphs (g)(1), (2) and (4) of this section for combination packagings may be applied to packagings containing articles, where the provisions for inner packagings are applied analogously to the articles. In this case, inner packagings need not comply with § 173.27(c)(1) and (c)(2) of this subchapter. (8) Approval of selective testing. In addition to the provisions of paragraphs (g)(1) through (7) of this section, the Associate Administrator may approve the selective testing of packagings that differ only in minor respects from a tested type. (9) For a steel drum with a capacity greater than 12 L (3 gallons) manufactured from low carbon, cold-rolled sheet steel meeting ASTM designations A 366/A 366M or A 568/A 568M, variations in elements other than the following design elements are considered minor and do not constitute a different drum design type, or “different packaging” as defined in paragraph (c) of this section for which design qualification testing and periodic retesting are required. Minor variations authorized without further testing include changes in the identity of the supplier of component material made to the same specifications, or the original manufacturer of a DOT specification or UN standard drum to be remanufactured. A change in any one or more of the following design elements constitutes a different drum design type: (i) The packaging type and category of the original drum and the remanufactured drum, i.e., 1A1 or 1A2; (ii) The style, ( i.e., straight-sided or tapered); (iii) Except as provided in paragraph (g)(3) of this section, the rated (marked) capacity and outside dimensions; (iv) The physical state for which the packaging was originally approved (e.g., tested for solids or liquids); (v) An increase in the marked level of performance of the original drum ( i.e., to a higher packing group, hydrostatic test pressure, or specific gravity to which the packaging has been tested); (vi) Type of side seam welding; (vii) Type of steel; (viii) An increase greater than 10% or any decrease in the steel thickness of the head, body, or bottom; (ix) End seam type, (e.g., triple or double seam); (x) A reduction in the number of rolling hoops (beads) which equal or exceed the diameter over the chimes; (xi) The location, type or size, and material of closures (other than the cover of UN 1A2 drums); (xii) The location (e.g., from the head to the body), type (e.g., mechanically seamed or welded flange), and materials of closure (other than the cover of UN 1A2 drums); and (xiii) For UN 1A2 drums: (A) Gasket material (e.g., plastic), or properties affecting the performance of the gasket; (B) Configuration or dimensions of the gasket; (C) Closure ring style including bolt size (e.g., square or round back, 0.625 inches bolt); and (D) Closure ring thickness, (E) Width of lugs or extensions in crimp/lug cover. (h) Approval of equivalent packagings. A packaging having specifications different from those in §§ 178.504-178.523 of this part, or which is tested using methods or test intervals, other than those specified in subpart M of this part, may be used if approved by the Associate Administrator. Such packagings must be shown to be equally effective, and testing methods used must be equivalent. (i) Proof of compliance. Notwithstanding the periodic retest intervals specified in paragraph (e) of this section, the Associate Administrator may at any time require demonstration of compliance by a manufacturer, through testing in accordance with this subpart, that packagings meet the requirements of this subpart. As required by the Associate Administrator, the manufacturer shall either— (1) Conduct performance tests, or have tests conducted by an independent testing facility, in accordance with this subpart; or (2) Supply packagings, in quantities sufficient to conduct tests in accordance with this subpart, to the Associate Administrator or a designated representative of the Associate Administrator. (j) Coatings. If an inner treatment or coating of a packaging is required for safety reasons, the manufacturer shall design the packaging so that the treatment or coating retains its protective properties even after withstanding the tests prescribed by this subpart. (k) Number of test samples. Except as provided in this section, one test sample must be used for each test performed under this subpart. (1) Stainless steel drums. Provided the validity of the test results is not affected, a person may perform the design qualification testing of stainless steel drums using three (3) samples rather than the specified eighteen (18) samples under the following provisions: (i) The packaging must be tested in accordance with this subpart by subjecting each of the three containers to the following sequence of tests: (A) The stacking test in § 178.606, (B) The leakproofness test in § 178.604, (C) The hydrostatic pressure test in § 178.608, and (D) Diagonal top chime and flat on the side drop tests in § 178.603. Both drop tests may be conducted on the same sample. (ii) For periodic retesting of stainless steel drums, a reduced sample size of one container is authorized. (2) Packagings other than stainless steel drums. Provided the validity of the test results is not affected, several tests may be performed on one sample with the approval of the Associate Administrator. (l) Record retention. Following each design qualification test and each periodic retest on a packaging, a test report must be prepared. (1) The test report must be maintained at each location where the packaging is manufactured, certified, and a design qualification test or periodic retest is conducted as follows: (2) The test report must be made available to a user of a packaging or a representative of the Department upon request. The test report, at a minimum, must contain the following information: (i) Name and address of test facility; (ii) Name and address of applicant (where appropriate); (iii) A unique test report identification; (iv) Date of the test report; (v) Manufacturer of the packaging; (vi) Description of the packaging design type (e.g., dimensions, materials, closures, thickness, etc. ), including methods of manufacture (e.g., blow molding) and which may include drawing(s) and/or photograph(s); (vii) Maximum capacity; (viii) Characteristics of test contents, including for plastic packagings subject to the hydrostatic pressure test in § 178.605 of this subpart, the temperature of the water used; (ix) Test descriptions and results; and (x) Signed with the name and title of signatory." 49:49:3.1.1.1.1.10.1.3,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.602 Preparation of packagings and packages for testing.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66286, Dec. 20, 1991; Amdt. 178-106, 59 FR 67522, Dec. 29, 1994; 69 FR 76186, Dec. 20, 2004; 71 FR 78635, Dec. 29, 2006]","(a) Except as otherwise provided in this subchapter, each packaging and package must be closed in preparation for testing and tests must be carried out in the same manner as if prepared for transportation, including inner packagings in the case of combination packagings. (b) For the drop and stacking test, inner and single-unit receptacles other than bags must be filled to not less than 95% of maximum capacity (see § 171.8 of this subchapter) in the case of solids and not less than 98% of maximum in the case of liquids. Bags containing solids shall be filled to the maximum mass at which they may be used. The material to be transported in the packagings may be replaced by a non-hazardous material, except for chemical compatibility testing or where this would invalidate the results of the tests. (c) If the material to be transported is replaced for test purposes by a non-hazardous material, the material used must be of the same or higher specific gravity as the material to be carried, and its other physical properties (grain, size, viscosity) which might influence the results of the required tests must correspond as closely as possible to those of the hazardous material to be transported. Water may also be used for the liquid drop test under the conditions specified in § 178.603(e) of this subpart. It is permissible to use additives, such as bags of lead shot, to achieve the requisite total package mass, so long as they are placed so that the test results are not affected. (d) Paper or fiberboard packagings must be conditioned for at least 24 hours immediately prior to testing in an atmosphere maintained— (1) At 50 percent ±2 percent relative humidity, and at a temperature of 23 °C±2 °C (73 °F±4 °F). Average values should fall within these limits. Short-term fluctuations and measurement limitations may cause individual measurements to vary by up to ±5 percent relative humidity without significant impairment of test reproducibility; (2) At 65 percent ±2 percent relative humidity, and at a temperature of 20 °C±2 °C (68 °F±4 °F), or 27 °C±2 °C (81 °F±4 °F). Average values should fall within these limits. Short-term fluctuations and measurement limitations may cause individual measurements to vary by up to ±5 percent relative humidity without significant impairment of test reproducibility; or (3) For testing at periodic intervals only ( i.e. , other than initial design qualification testing), at ambient conditions. (e) Except as otherwise provided, each packaging must be closed in preparation for testing in the same manner as if prepared for actual shipment. All closures must be installed using proper techniques and torques. (f) Bung-type barrels made of natural wood must be left filled with water for at least 24 hours before the tests." 49:49:3.1.1.1.1.10.1.4,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.603 Drop test.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66286, Dec. 20, 1991; 57 FR 45465, Oct. 1, 1992; Amdt. 178-99, 58 FR 51534, Oct. 1, 1993; Amdt. 178-106, 59 FR 67522, Dec. 29, 1994; 65 FR 50462, Aug. 18, 2000; 66 FR 45386, Aug. 28, 2001; 67 FR 61016, Sept. 27, 2002; 69 FR 76186, Dec. 20, 2004; 76 FR 3389, Jan. 19, 2011; 78 FR 1097, Jan. 7, 2013]","(a) General. The drop test must be conducted for the qualification of all packaging design types and performed periodically as specified in § 178.601(e). For other than flat drops, the center of gravity of the test packaging must be vertically over the point of impact. Where more than one orientation is possible for a given drop test, the orientation most likely to result in failure of the packaging must be used. The number of drops required and the packages' orientations are as follows: (b) Exceptions. For testing of single or composite packagings constructed of stainless steel, nickel, or monel at periodic intervals only ( i.e. , other than design qualification testing), the drop test may be conducted with two samples, one sample each for the two drop orientations. These samples may have been previously used for the hydrostatic pressure or stacking test. Exceptions for the number of steel, aluminum and other metal packaging samples used for conducting the drop test are subject to the approval of the Associate Administrator. (c) Special preparation of test samples for the drop test. (1) Testing of plastic drums, plastic jerricans, plastic boxes other than expanded polystyrene boxes, composite packagings (plastic material), and combination packagings with plastic inner packagings other than plastic bags intended to contain solids or articles must be carried out when the temperature of the test sample and its contents has been reduced to −18 °C (0 °F) or lower. Test liquids must be kept in the liquid state, if necessary, by the addition of anti-freeze. Water/anti-freeze solutions with a minimum specific gravity of 0.95 for testing at −18 °C (0 °F) or lower are considered acceptable test liquids. Test samples prepared in this way are not required to be conditioned in accordance with § 178.602(d). (d) Target. The target must be a rigid, non-resilient, flat and horizontal surface. (e) Drop height. Drop heights, measured as the vertical distance from the target to the lowest point on the package, must be equal to or greater than the drop height determined as follows: (1) For solids and liquids, if the test is performed with the solid or liquid to be transported or with a non-hazardous material having essentially the same physical characteristic, the drop height must be determined according to packing group, as follows: (i) Packing Group I: 1.8 m (5.9 feet). (ii) Packing Group II: 1.2 m (3.9 feet). (iii) Packing Group III: 0.8 m (2.6 feet). (2) For liquids in single packagings and for inner packagings of combination packagings, if the test is performed with water: (i) Where the materials to be carried have a specific gravity not exceeding 1.2, drop height must be determined according to packing group, as follows: (A) Packing Group I: 1.8 m (5.9 feet). (B) Packing Group II: 1.2 m (3.9 feet). (C) Packing Group III: 0.8 m (2.6 feet). (ii) Where the materials to be transported have a specific gravity exceeding 1.2, the drop height must be calculated on the basis of the specific gravity (SG) of the material to be carried, rounded up to the first decimal, as follows: (A) Packing Group I: SG × 1.5 m (4.9 feet). (B) Packing Group II: SG × 1.0 m (3.3 feet). (C) Packing Group III: SG × 0.67 m (2.2 feet). (f) Criteria for passing the test. A package is considered to successfully pass the drop tests if for each sample tested— (1) For packagings containing liquid, each packaging does not leak when equilibrium has been reached between the internal and external pressures, except for inner packagings of combination packagings when it is not necessary that the pressures be equalized; (2) For removable head drums for solids, the entire contents are retained by an inner packaging (e.g., a plastic bag) even if the closure on the top head of the drum is no longer sift-proof; (3) For a bag, neither the outermost ply nor an outer packaging exhibits any damage likely to adversely affect safety during transport; (4) The packaging or outer packaging of a composite or combination packaging must not exhibit any damage likely to affect safety during transport. Inner receptacles, inner packagings, or articles must remain completely within the outer packaging and there must be no leakage of the filling substance from the inner receptacles or inner packagings; (5) Any discharge from a closure is slight and ceases immediately after impact with no further leakage; and (6) No rupture is permitted in packagings for materials in Class 1 which would permit spillage of loose explosive substances or articles from the outer packaging." 49:49:3.1.1.1.1.10.1.5,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.604 Leakproofness test.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66286, Dec. 20, 1991; Amdt. 178-106, 59 FR 67522, Dec. 29, 1994; 66 FR 45386, Aug. 28, 2001]","(a) General. The leakproofness test must be performed with compressed air or other suitable gases on all packagings intended to contain liquids, except that: (1) The inner receptacle of a composite packaging may be tested without the outer packaging provided the test results are not affected; and (2) This test is not required for inner packagings of combination packagings. (b) Number of packagings to be tested —(1) Production testing. All packagings subject to the provisions of this section must be tested and must pass the leakproofness test: (i) Before they are first used in transportation; and (ii) Prior to reuse, when authorized for reuse by § 173.28 of this subchapter. (2) Design qualification and periodic testing. Three samples of each different packaging must be tested and must pass the leakproofness test. Exceptions for the number of samples used in conducting the leakproofness test are subject to the approval of the Associate Administrator. (c) Special preparation —(1) For design qualification and periodic testing, packagings must be tested with closures in place. For production testing, packagings need not have their closures in place. Removable heads need not be installed during production testing. (2) For testing with closures in place, vented closures must either be replaced by similar non-vented closures or the vent must be sealed. (d) Test method. The packaging must be restrained under water while an internal air pressure is applied; the method of restraint must not affect the results of the test. The test must be conducted, for other than production testing, for a minimum time of five minutes. Other methods, at least equally effective, may be used in accordance with appendix B of this part. (e) Pressure applied. An internal air pressure (gauge) must be applied to the packaging as indicated for the following packing groups: (1) Packing Group I: Not less than 30 kPa (4 psi). (2) Packing Group II: Not less than 20 kPa (3 psi). (3) Packing Group III: Not less than 20 kPa (3 psi). (f) Criteria for passing the test. A packaging passes the test if there is no leakage of air from the packaging." 49:49:3.1.1.1.1.10.1.6,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.605 Hydrostatic pressure test.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66286, Dec. 20, 1991; Amdt. 178-99, 58 FR 51534, Oct. 1, 1993; Amdt. 178-102, 59 FR 28494, June 2, 1994; 65 FR 50462, Aug. 18, 2000; 66 FR 45386, 45390, Aug. 28, 2001; 73 FR 57007, Oct. 1, 2008; 78 FR 60755, Oct. 2, 2013]","(a) General. The hydrostatic pressure test must be conducted for the qualification of all metal, plastic, and composite packaging design types intended to contain liquids and be performed periodically as specified in § 178.601(e). This test is not required for inner packagings of combination packagings. For internal pressure requirements for inner packagings of combination packagings intended for transportation by aircraft, see § 173.27(c) of this subchapter. (b) Number of test samples. Three test samples are required for each different packaging. For packagings constructed of stainless steel, monel, or nickel, only one sample is required for periodic retesting of packagings. Exceptions for the number of aluminum and steel sample packagings used in conducting the hydrostatic pressure test are subject to the approval of the Associate Administrator. (c) Special preparation of receptacles for testings. Vented closures must either be replaced by similar non-vented closures or the vent must be sealed. (d) Test method and pressure to be applied. Metal packagings and composite packagings other than plastic (e.g., glass, porcelain or stoneware), including their closures, must be subjected to the test pressure for 5 minutes. Plastic packagings and composite packagings (plastic material), including their closures, must be subjected to the test pressure for 30 minutes. This pressure is the one to be marked as required in § 178.503(a)(5). The receptacles must be supported in a manner that does not invalidate the test. The test pressure must be applied continuously and evenly, and it must be kept constant throughout the test period. In addition, packagings intended to contain hazardous materials of Packing Group I must be tested to a minimum test pressure of 250 kPa (36 psig). The hydraulic pressure (gauge) applied, taken at the top of the receptacle, and determined by any one of the following methods must be: (1) Not less than the total gauge pressure measured in the packaging ( i.e. , the vapor pressure of the filling material and the partial pressure of the air or other inert gas minus 100 kPa (15 psi)) at 55 °C (131 °F), multiplied by a safety factor of 1.5. This total gauge pressure must be determined on the basis of a maximum degree of filling in accordance with § 173.24a(d) of this subchapter and a filling temperature of 15 °C (59 °F); (2) Not less than 1.75 times the vapor pressure at 50 °C (122 °F) of the material to be transported minus 100 kPa (15 psi), but with a minimum test pressure of 100 kPa (15 psig); or (3) Not less than 1.5 times the vapor pressure at 55 °C (131 °F) of the material to be transported minus 100 kPa (15 psi), but with a minimum test pressure of 100 kPa (15 psig). Packagings intended to contain hazardous materials of Packing Group I must be tested to a minimum test pressure of 250 kPa (36 psig). (e) Criteria for passing the test. A package passes the hydrostatic test if, for each test sample, there is no leakage of liquid from the package." 49:49:3.1.1.1.1.10.1.7,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.606 Stacking test.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66286, Dec. 20, 1991; 57 FR 45465, Oct. 1, 1992; Amdt. 178-102, 59 FR 28494, June 2, 1994; Amdt. 178-106, 59 FR 67522, Dec. 29, 1994; 65 FR 58632, Sept. 29, 2000; 66 FR 45386, Aug. 28, 2001; 70 FR 34076, June 13, 2005; 72 FR 55696, Oct. 1, 2007]","(a) General. All packaging design types other than bags must be subjected to a stacking test. (b) Number of test samples. Three test samples are required for each different packaging. For periodic retesting of packagings constructed of stainless steel, monel, or nickel, only one test sample is required. Exceptions for the number of aluminum and steel sample packagings used in conducting the stacking test are subject to the approval of the Associate Administrator. Notwithstanding the provisions of § 178.602(a) of this subpart, combination packagings may be subjected to the stacking test without their inner packagings, except where this would invalidate the results of the test. (c) Test method —(1) Design qualification testing. The test sample must be subjected to a force applied to the top surface of the test sample equivalent to the total weight of identical packages which might be stacked on it during transport; where the contents of the test sample are non-hazardous liquids with specific gravities different from that of the liquid to be transported, the force must be calculated based on the specific gravity that will be marked on the packaging. The minimum height of the stack, including the test sample, must be 3.0 m (10 feet). The duration of the test must be 24 hours, except that plastic drums, jerricans, and composite packagings 6HH intended for liquids shall be subjected to the stacking test for a period of 28 days at a temperature of not less than 40 °C (104 °F). Alternative test methods which yield equivalent results may be used if approved by the Associate Administrator. In guided load tests, stacking stability must be assessed after completion of the test by placing two filled packagings of the same type on the test sample. The stacked packages must maintain their position for one hour. Plastic packagings must be cooled to ambient temperature before this stacking stability assessment. (2) Periodic retesting. The test sample must be tested in accordance with: (i) Section 178.606(c)(1) of this subpart; or (ii) The packaging may be tested using a dynamic compression testing machine. The test must be conducted at room temperature on an empty, unsealed packaging. The test sample must be centered on the bottom platen of the testing machine. The top platen must be lowered until it comes in contact with the test sample. Compression must be applied end to end. The speed of the compression tester must be one-half inch plus or minus one-fourth inch per minute. An initial preload of 50 pounds must be applied to ensure a definite contact between the test sample and the platens. The distance between the platens at this time must be recorded as zero deformation. The force A to then be applied must be calculated using the formula: Liquids: A = (n−1) [w + (s × v × 8.3 × .98)] × 1.5; Solids: A = (n−1) (m × 2.2 × 1.5) Where: A = applied load in pounds m = the certified maximum gross mass for the container in kilograms. n = minimum number of containers that, when stacked, reach a height of 3 meters. s = specific gravity of lading. w = maximum weight of one empty container in pounds. v = actual capacity of container (rated capacity + outage) in gallons. And: 8.3 corresponds to the weight in pounds of 1.0 gallon of water. .98 corresponds to the minimum filling percentage of the maximum capacity for liquids. 1.5 is a compensation factor that converts the static load of the stacking test into a load suitable for dynamic compression testing. 2.2 is the conversion factor for kilograms to pounds. Where: A = applied load in pounds m = the certified maximum gross mass for the container in kilograms. n = minimum number of containers that, when stacked, reach a height of 3 meters. s = specific gravity of lading. w = maximum weight of one empty container in pounds. v = actual capacity of container (rated capacity + outage) in gallons. And: 8.3 corresponds to the weight in pounds of 1.0 gallon of water. .98 corresponds to the minimum filling percentage of the maximum capacity for liquids. 1.5 is a compensation factor that converts the static load of the stacking test into a load suitable for dynamic compression testing. 2.2 is the conversion factor for kilograms to pounds. (d) Criteria for passing the test. No test sample may leak. In composite packagings or combination packagings, there must be no leakage of the filling substance from the inner receptacle, or inner packaging. No test sample may show any deterioration which could adversely affect transportation safety or any distortion likely to reduce its strength, cause instability in stacks of packages, or cause damage to inner packagings likely to reduce safety in transportation. For the dynamic compression test, a container passes the test if, after application of the required load, there is no buckling of the sidewalls sufficient to cause damage to its expected contents; in no case may the maximum deflection exceed one inch." 49:49:3.1.1.1.1.10.1.8,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.607 Cooperage test for bung-type wooden barrels.,PHMSA,,,,"(a) Number of samples. One barrel is required for each different packaging. (b) Method of testing. Remove all hoops above the bilge of an empty barrel at least two days old. (c) Criteria for passing the test. A packaging passes the cooperage test only if the diameter of the cross-section of the upper part of the barrel does not increase by more than 10 percent." 49:49:3.1.1.1.1.10.1.9,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,M,Subpart M—Testing of Non-bulk Packagings and Packages,,§ 178.608 Vibration standard.,PHMSA,,,"[Amdt. 178-97, 55 FR 52723, Dec. 21, 1990, as amended at 56 FR 66286, Dec. 20, 1991; 66 FR 45386, Aug. 28, 2001]","(a) Each packaging must be capable of withstanding, without rupture or leakage, the vibration test procedure outlined in this section. (b) Test method. (1) Three sample packagings, selected at random, must be filled and closed as for shipment. (2) The three samples must be placed on a vibrating platform that has a vertical or rotary double-amplitude (peak-to-peak displacement) of one inch. The packages should be constrained horizontally to prevent them from falling off the platform, but must be left free to move vertically, bounce and rotate. (3) The test must be performed for one hour at a frequency that causes the package to be raised from the vibrating platform to such a degree that a piece of material of approximately 1.6 mm (0.063 inch) thickness (such as steel strapping or paperboard) can be passed between the bottom of any package and the platform. (4) Immediately following the period of vibration, each package must be removed from the platform, turned on its side and observed for any evidence of leakage. (5) Other methods, at least equally effective, may be used, if approved by the Associate Administrator. (c) Criteria for passing the test. A packaging passes the vibration test if there is no rupture or leakage from any of the packages. No test sample should show any deterioration which could adversely affect transportation safety or any distortion liable to reduce packaging strength." 49:49:3.1.1.1.1.11.1.1,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,"§ 178.700 Purpose, scope and definitions.",PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended by Amdt. 178-108, 60 FR 40038, Aug. 4, 1995; 66 FR 45386, 45387, Aug. 28, 2001; 73 FR 57008, Oct. 1, 2008; 75 FR 5396, Feb. 2, 2010]","(a) This subpart prescribes requirements applying to IBCs intended for the transportation of hazardous materials. Standards for these packagings are based on the UN Recommendations. (b) Terms used in this subpart are defined in § 171.8 of this subchapter and in paragraph (c) of this section. (c) The following definitions pertain to the IBC standards in this subpart. (1) Body means the receptacle proper (including openings and their closures, but not including service equipment) that has a volumetric capacity of not more than 3 cubic meters (3,000 L, 793 gallons, or 106 cubic feet). (2) Service equipment means filling and discharge, pressure relief, safety, heating and heat-insulating devices and measuring instruments. (3) Structural equipment means the reinforcing, fastening, handling, protective or stabilizing members of the body or stacking load bearing structural members (such as metal cages). (4) Maximum permissible gross mass means the mass of the body, its service equipment, structural equipment and the maximum net mass (see § 171.8 of this subchapter)." 49:49:3.1.1.1.1.11.1.10,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.710 Standards for flexible IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended by Amdt. 178-108, 60 FR 40038, Aug. 4, 1995; 66 FR 45386, Aug. 28, 2001; 75 FR 5397, Feb. 2, 2010]","(a) The provisions of this section apply to flexible IBCs intended to contain solid hazardous materials. Flexible IBC types are designated: (1) 13H1 woven plastic without coating or liner. (2) 13H2 woven plastic, coated. (3) 13H3 woven plastic with liner. (4) 13H4 woven plastic, coated and with liner. (5) 13H5 plastic film. (6) 13L1 textile without coating or liner. (7) 13L2 textile, coated. (8) 13L3 textile with liner. (9) 13L4 textile, coated and with liner. (10) 13M1 paper, multiwall. (11) 13M2 paper, multiwall, water resistant. (b) Definitions for flexible IBCs: (1) Flexible IBCs consist of a body constructed of film, woven plastic, woven fabric, paper, or combination thereof, together with any appropriate service equipment and handling devices, and if necessary, an inner coating or liner. (2) Woven plastic means a material made from stretched tapes or monofilaments. (3) Handling device means any sling, loop, eye, or frame attached to the body of the IBC or formed from a continuation of the IBC body material. (c) Construction requirements for flexible IBCs are as follows: (1) The strength of the material and the construction of the flexible IBC must be appropriate to its capacity and its intended use. (2) All materials used in the construction of flexible IBCs of types 13M1 and 13M2 must, after complete immersion in water for not less than 24 hours, retain at least 85 percent of the tensile strength as measured originally on the material conditioned to equilibrium at 67 percent relative humidity or less. (3) Seams must be stitched or formed by heat sealing, gluing or any equivalent method. All stitched seam-ends must be secured. (4) In addition to conformance with the requirements of § 173.24 of this subchapter, flexible IBCs must be resistant to aging and degradation caused by ultraviolet radiation. (5) For plastic flexible IBCs, if necessary, protection against ultraviolet radiation must be provided by the addition of pigments or inhibitors such as carbon black. These additives must be compatible with the contents and remain effective throughout the life of the container. Where use is made of carbon black, pigments, or inhibitors, other than those used in the manufacture of the tested design type, retesting may be omitted if the carbon black content, the pigment content or the inhibitor content does not adversely affect the physical properties of the material of construction. Additives may be included in the composition of the plastic material to improve resistance to aging, provided they do not adversely affect the physical or chemical properties of the material. (6) No used material other than production residues or regrind from the same manufacturing process may be used in the manufacture of plastic flexible IBCs. This does not preclude the re-use of component parts such as fittings and pallet bases, provided such components have not in any way been damaged in previous use. (7) When flexible IBCs are filled, the ratio of height to width may not be more than 2:1. (d) Flexible IBCs: (1) May not have a volumetric capacity greater than 3,000 L (793 gallons) or less than 56 L (15 gallons); and (2) Must be designed and tested to a capacity of no less than 50 kg (110 pounds)." 49:49:3.1.1.1.1.11.1.2,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.702 IBC codes.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended at 66 FR 45386, Aug. 28, 2001]","(a) Intermediate bulk container code designations consist of: two numerals specified in paragraph (a)(1) of this section; followed by the capital letter(s) specified in paragraph (a)(2) of this section; followed, when specified in an individual section, by a numeral indicating the category of intermediate bulk container. (1) IBC code number designations are as follows: (2) Intermediate bulk container code letter designations are as follows: “A” means steel (all types and surface treatments). “B” means aluminum. “C” means natural wood. “D” means plywood. “F” means reconstituted wood. “G” means fiberboard. “H” means plastic. “L” means textile. “M” means paper, multiwall. “N” means metal (other than steel or aluminum). “A” means steel (all types and surface treatments). “B” means aluminum. “C” means natural wood. “D” means plywood. “F” means reconstituted wood. “G” means fiberboard. “H” means plastic. “L” means textile. “M” means paper, multiwall. “N” means metal (other than steel or aluminum). (b) For composite IBCs, two capital letters are used in sequence following the numeral indicating IBC design type. The first letter indicates the material of the IBC inner receptacle. The second letter indicates the material of the outer IBC. For example, 31HA1 is a composite IBC with a plastic inner receptacle and a steel outer packaging." 49:49:3.1.1.1.1.11.1.3,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.703 Marking of IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended by Amdt. 178-119, 62 FR 24743, May 6, 1997; 64 FR 10782, Mar. 5, 1999; 65 FR 50462, Aug. 18, 2000; 65 FR 58632, Sept. 29, 2000; 66 FR 33451, June 21, 2001; 66 FR 45387, Aug. 28, 2001; 74 FR 2269, Jan. 14, 2009; 75 FR 74, Jan. 4, 2010; 75 FR 5396, Feb. 2, 2010; 76 FR 3389, Jan. 19, 2011; 80 FR 1168, Jan. 8, 2015; 83 FR 55810, Nov. 7, 2018; 87 FR 45000, July 26, 2022]","(a) The manufacturer shall: (1) Mark every IBC in a durable and clearly visible manner. The marking may be applied in a single line or in multiple lines provided the correct sequence is followed with the information required by this section in letters, numerals and symbols of at least 12 mm in height. This minimum marking size applies only to IBCs manufactured after October 1, 2001). The following information is required in the sequence presented: (i) Except as provided in § 178.503(e)(1)(ii), the United Nations symbol as illustrated in § 178.503(e)(1)(i). For metal IBCs on which the marking is stamped or embossed, the capital letters “UN” may be applied instead of the symbol. (ii) The code number designating IBC design type according to § 178.702(a). The letter “W” must follow the IBC design type identification code on an IBC when the IBC differs from the requirements in subpart N of this part, or is tested using methods other than those specified in this subpart, and is approved by the Associate Administrator in accordance with the provisions in § 178.801(i). (iii) A capital letter identifying the performance standard under which the design type has been successfully tested, as follows: (A) X—for IBCs meeting Packing Group I, II and III tests; (B) Y—for IBCs meeting Packing Group II and III tests; and (C) Z—for IBCs meeting only Packing Group III tests. (iv) The month (designated numerically) and year (last two digits) of manufacture. (v) The country authorizing the allocation of the mark. The letters ‘USA’ indicate that the IBC is manufactured and marked in the United States in compliance with the provisions of this subchapter. (vi) The name and address or symbol of the manufacturer or the approval agency certifying compliance with subparts N and O of this part. Symbols, if used, must be registered with the Associate Administrator. (vii) The stacking test load in kilograms (kg). For IBCs not designed for stacking, the figure “0” must be shown. (viii) The maximum permissible gross mass in kg. (2) The following are examples of symbols and required markings: (i) For a metal IBC containing solids discharged by gravity made from steel: (ii) For a flexible IBC containing solids discharged by gravity and made from woven plastic with a liner: (iii) For a rigid plastic IBC containing liquids, made from plastic with structural equipment withstanding the stack load and with a manufacturer's symbol in place of the manufacturer's name and address: (iv) For a composite IBC containing liquids, with a rigid plastic inner receptacle and an outer steel body and with the symbol of a DOT approved third-party test laboratory: (b) Additional marking. In addition to markings required in paragraph (a) of this section, each IBC must be marked as follows in a place near the markings required in paragraph (a) of this section that is readily accessible for inspection. Where units of measure are used, the metric unit indicated (e.g., 450 L) must also appear. (1) For each rigid plastic and composite IBC, the following markings must be included: (i) Rated capacity in L of water at 20 °C (68 °F); (ii) Tare mass in kilograms; (iii) Gauge test pressure in kPa; (iv) Date of last leakproofness test, if applicable (month and year); and (v) Date of last inspection (month and year). (2) For each metal IBC, the following markings must be included on a metal corrosion-resistant plate: (i) Rated capacity in L of water at 20 °C (68 °F); (ii) Tare mass in kilograms; (iii) Date of last leakproofness test, if applicable (month and year); (iv) Date of last inspection (month and year); (v) Maximum loading/discharge pressure, in kPa, if applicable; (vi) Body material and its minimum thickness in mm; and (vii) Serial number assigned by the manufacturer. (3) Markings required by paragraph (b)(1) or (b)(2) of this section may be preceded by the narrative description of the marking, e.g. “Tare Mass: * * *” where the “* * *” are replaced with the tare mass in kilograms of the IBC. (4) For each fiberboard and wooden IBC, the tare mass in kg must be shown. (5) Each flexible IBC may be marked with a pictogram displaying recommended lifting methods. (6) For each composite IBC, the inner receptacle must be marked with at least the following information as required by paragraphs (b)(6)(i) and (ii) of this section. Additionally, the marking must be visible while inside of the outer receptacle. If the marking is not visible from the outer receptacle, the marking must be duplicated on the outer receptacle and include an indication that the marking applies to the inner receptacle. (i) The code number designating the IBC design type, the name and address or symbol of the manufacturer, the date of manufacture and the country authorizing the allocation of the mark as specified in paragraph (a) of this section. The date of manufacture of the inner receptacle may be different from the marked date of manufacture required by § 178.703(a)(1)(iv) or by § 180.352(d)(1)(iv) of this subchapter; and (ii) When a composite IBC is designed in such a manner that the outer casing is intended to be dismantled for transport when empty (such as, for the return of the IBC for reuse to the original consignor), each of the parts intended to be detached when so dismantled must be marked with the month and year of manufacture and the name or symbol of the manufacturer. (7) The symbol applicable to an IBC designed for stacking or not designed for stacking, as appropriate, must be marked on all IBCs manufactured, repaired or remanufactured after January 1, 2011 as follows: (i) (ii) Display the symbol in a durable and visible manner. (iii) The symbol must be a square with each side being not less than 100 mm (3.9 inches) by 100 mm (3.9 inches) as measured from the corner printer marks shown on the figures in paragraph (b)(7)(i) of this section. Where dimensions are not specified, all features must be in approximate proportion to those shown. (A) Transitional exception. A marking in conformance with the requirements of this paragraph in effect on December 31, 2014, may continue to be applied to all IBCs manufactured, repaired or remanufactured between January 1, 2011 and December 31, 2016. (B) For domestic transportation, an IBC marked prior to January 1, 2017 and in conformance with the requirements of this paragraph in effect on December 31, 2014, may continue in service until the end of its useful life. (iv) For IBCs designed for stacking, the maximum permitted stacking load applicable when the IBC is in transportation must be displayed with the symbol. The mass in kilograms (kg) marked above the symbol must not exceed the load imposed during the design test, as indicated by the marking in paragraph (a)(1)(vii) of this section, divided by 1.8. The letters and numbers indicating the mass must be at least 12 mm (0.48 inches)." 49:49:3.1.1.1.1.11.1.4,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.704 General IBC standards.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended at 66 FR 45386, Aug. 28, 2001; 68 FR 61942, Oct. 30, 2003]","(a) Each IBC must be resistant to, or protected from, deterioration due to exposure to the external environment. IBCs intended for solid hazardous materials must be sift-proof and water-resistant. (b) All service equipment must be so positioned or protected as to minimize potential loss of contents resulting from damage during IBC handling and transportation. (c) Each IBC, including attachments, and service and structural equipment, must be designed to withstand, without loss of hazardous materials, the internal pressure of the contents and the stresses of normal handling and transport. An IBC intended for stacking must be designed for stacking. Any lifting or securing features of an IBC must be of sufficient strength to withstand the normal conditions of handling and transportation without gross distortion or failure and must be positioned so as to cause no undue stress in any part of the IBC. (d) An IBC consisting of a packaging within a framework must be so constructed that: (1) The body is not damaged by the framework; (2) The body is retained within the framework at all times; and (3) The service and structural equipment are fixed in such a way that they cannot be damaged if the connections between body and frame allow relative expansion or motion. (e) Bottom discharge valves must be secured in the closed position and the discharge system suitably protected from damage. Valves having lever closures must be secured against accidental opening. The open or closed position of each valve must be readily apparent. For each IBC containing a liquid, a secondary means of sealing the discharge aperture must also be provided, e.g., by a blank flange or equivalent device. (f) IBC design types must be constructed in such a way as to be bottom-lifted or top-lifted as specified in §§ 178.811 and 178.812." 49:49:3.1.1.1.1.11.1.5,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.705 Standards for metal IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended by Amdt. 178-108, 60 FR 40038, Aug. 4, 1995; Amdt. 178-117, 61 FR 50629, Sept. 26, 1996; 66 FR 33452, June 21, 2001; 66 FR 45386, 45387, Aug. 28, 2001; 68 FR 45041, July 31, 2003; 75 FR 5396, Feb. 2, 2010; 78 FR 1097, Jan. 7, 2013; 87 FR 45000, July 26, 2022]","(a) The provisions in this section apply to metal IBCs intended to contain liquids and solids. Metal IBC types are designated: (1) 11A, 11B, 11N for solids that are loaded or discharged by gravity. (2) 21A, 21B, 21N for solids that are loaded or discharged at a gauge pressure greater than 10 kPa (1.45 psig). (3) 31A, 31B, 31N for liquids. (b) Definitions for metal IBCs: (1) Metal IBC means an IBC with a metal body, together with appropriate service and structural equipment. (2) Protected means providing the IBC body with additional external protection against impact and abrasion. For example, a multi-layer (sandwich) or double wall construction or a frame with a metal lattice-work casing. (c) Construction requirements for metal IBCs are as follows: (1) Body. The body must be made of ductile metal materials. Welds must be made so as to maintain design type integrity of the receptacle under conditions normally incident to transportation. (i) The use of dissimilar metals must not result in deterioration that could affect the integrity of the body. (ii) Aluminum IBCs intended to contain flammable liquids must have no movable parts, such as covers and closures, made of unprotected steel liable to rust, which might cause a dangerous reaction from friction or percussive contact with the aluminum. (iii) Metals used in fabricating the body of a metal IBC must meet the following requirements: (A) For steel, the percentage elongation at fracture must not be less than 10,000/Rm with a minimum of 20 percent; where Rm = minimum tensile strength of the steel to be used, in N/mm 2 ; if U.S. Standard units of psi are used for tensile strength then the ratio becomes 10,000 × (145/Rm). (B) For aluminum, the percentage elongation at fracture must not be less than 10,000/(6Rm) with an absolute minimum of eight percent; if U.S. Standard units of psi are used for tensile strength then the ratio becomes 10,000 × 145 / (6Rm). (C) Specimens used to determine the elongation at fracture must be taken transversely to the direction of rolling and be so secured that: Lo = 5d or Lo = 5.65 √A where: Lo = gauge length of the specimen before the test d = diameter A = cross-sectional area of test specimen. where: Lo = gauge length of the specimen before the test d = diameter A = cross-sectional area of test specimen. (iv) Minimum wall thickness. For metal IBCs with a capacity of more than 1500 liters, the minimum wall thickness must be determined as follows: (A) For a reference steel having a product of Rm × Ao = 10,000, where Ao is the minimum elongation (as a percentage) of the reference steel to be used on fracture under tensile stress (Rm × Ao = 10,000 × 145; if tensile strength is in U.S. Standard units of pounds per square inch), the wall thickness must not be less than: Table 1 to Paragraph ( c )(1)( iv )(A)—Wall Thickness (T) in mm , Capacity (C) in Liters (B) For metals other than the reference steel described in paragraph (c)(1)(iii)(A) of this section, the minimum wall thickness is the greater of 1.5 mm (0.059 inches) or as determined by use of the following equivalence formula: where: e 1 = required equivalent wall thickness of the metal to be used (in mm or if e o is in inches, use formula for U.S. Standard units). e o = required minimum wall thickness for the reference steel (in mm or if e o is in inches, use formula for U.S. Standard units). Rm 1 = guaranteed minimum tensile strength of the metal to be used (in N/mm 2 or for U.S. Standard units, use psi). A 1 = minimum elongation (as a percentage) of the metal to be used on fracture under tensile stress (see paragraph (c)(1) of this section). where: e 1 = required equivalent wall thickness of the metal to be used (in mm or if e o is in inches, use formula for U.S. Standard units). e o = required minimum wall thickness for the reference steel (in mm or if e o is in inches, use formula for U.S. Standard units). Rm 1 = guaranteed minimum tensile strength of the metal to be used (in N/mm 2 or for U.S. Standard units, use psi). A 1 = minimum elongation (as a percentage) of the metal to be used on fracture under tensile stress (see paragraph (c)(1) of this section). (C) For purposes of the calculation described in paragraph (c)(1)(iv)(B) of this section, the guaranteed minimum tensile strength of the metal to be used (Rm 1 ) must be the minimum value according to material standards. However, for austenitic (stainless) steels, the specified minimum value for Rm, according to the material standards, may be increased by up to 15% when a greater value is provided in the material inspection certificate. When no material standard exists for the material in question, the value of Rm must be the minimum value indicated in the material inspection certificate. (2) Pressure relief. The following pressure relief requirements apply to IBCs intended for liquids: (i) IBCs must be capable of releasing a sufficient amount of vapor in the event of fire engulfment to ensure that no rupture of the body will occur due to pressure build-up. This can be achieved by spring-loaded or non-reclosing pressure relief devices or by other means of construction. (ii) The start-to-discharge pressure may not be higher than 65 kPa (9 psig) and no lower than the vapor pressure of the hazardous material plus the partial pressure of the air or other inert gases, measured in the IBC at 55 °C (131 °F), determined on the basis of a maximum degree of filling as specified in § 173.35(d) of this subchapter. This does not apply to fusible devices unless such devices are the only source of pressure relief for the IBC. Pressure relief devices must be fitted in the vapor space. (d) Metal IBCs may not have a volumetric capacity greater than 3,000 L (793 gallons) or less than 450 L (119 gallons)." 49:49:3.1.1.1.1.11.1.6,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.706 Standards for rigid plastic IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended at 66 FR 45386, 45387, Aug. 28, 2001; 75 FR 5396, Feb. 2, 2010; 89 FR 25490, Apr. 10, 2024]","(a) The provisions in this section apply to rigid plastic IBCs intended to contain solids or liquids. Rigid plastic IBC types are designated: (1) 11H1 fitted with structural equipment designed to withstand the whole load when IBCs are stacked, for solids which are loaded or discharged by gravity. (2) 11H2 freestanding, for solids which are loaded or discharged by gravity. (3) 21H1 fitted with structural equipment designed to withstand the whole load when IBCs are stacked, for solids which are loaded or discharged under pressure. (4) 21H2 freestanding, for solids which are loaded or discharged under pressure. (5) 31H1 fitted with structural equipment designed to withstand the whole load when IBCs are stacked, for liquids. (6) 31H2 freestanding, for liquids. (b) Rigid plastic IBCs consist of a rigid plastic body, which may have structural equipment, together with appropriate service equipment. (c) Rigid plastic IBCs must be manufactured from plastic material of known specifications and be of a strength relative to its capacity and to the service it is required to perform. In addition to conformance to § 173.24 of this subchapter, plastic materials must be resistant to aging and to degradation caused by ultraviolet radiation. (1) If protection against ultraviolet radiation is necessary, it must be provided by the addition of a pigment or inhibiter such as carbon black. These additives must be compatible with the contents and remain effective throughout the life of the IBC body. Where use is made of carbon black, pigments or inhibitors, other than those used in the manufacture of the tested design type, retesting may be omitted if changes in the carbon black content, the pigment content or the inhibitor content do not adversely affect the physical properties of the material of construction. (2) Additives may be included in the composition of the plastic material to improve the resistance to aging or to serve other purposes, provided they do not adversely affect the physical or chemical properties of the material of construction. (3) No used material other than production residues or regrind from the same manufacturing process may be used in the manufacture of rigid plastic IBCs unless approved by the Associate Administrator. (4) Rigid plastic IBCs intended for the transportation of liquids must be capable of releasing a sufficient amount of vapor to prevent the body of the IBC from rupturing if it is subjected to an internal pressure in excess of that for which it was hydraulically tested. This may be achieved by spring-loaded or non-reclosing pressure relief devices or by other means of construction. (d) Rigid plastic IBCs may not have a volumetric capacity greater than 3,000 L (793 gallons) or less than 450 L (119 gallons)." 49:49:3.1.1.1.1.11.1.7,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.707 Standards for composite IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended by Amdt. 178-119, 62 FR 24743, May 6, 1997; 66 FR 45387, Aug. 28, 2001; 67 FR 61016, Sept. 27, 2002; 68 FR 75758, Dec. 31, 2003; 69 FR 54046, Sept. 7, 2004; 75 FR 5396, Feb. 2, 2010; 89 FR 25490, Apr. 10, 2024]","(a) The provisions in this section apply to composite IBCs intended to contain solids and liquids. To complete the marking codes listed below, the letter “Z” must be replaced by a capital letter in accordance with § 178.702(a)(2) to indicate the material used for the outer packaging. Composite IBC types are designated: (1) 11HZ1 Composite IBCs with a rigid plastic inner receptacle for solids loaded or discharged by gravity. (2) 11HZ2 Composite IBCs with a flexible plastic inner receptacle for solids loaded or discharged by gravity. (3) 21HZ1 Composite IBCs with a rigid plastic inner receptacle for solids loaded or discharged under pressure. (4) 21HZ2 Composite IBCs with a flexible plastic inner receptacle for solids loaded or discharged under pressure. (5) 31HZ1 Composite IBCs with a rigid plastic inner receptacle for liquids. (6) 31HZ2 Composite IBCs with a flexible plastic inner receptacle for liquids. (b) Definitions for composite IBC types: (1) A composite IBC is an IBC which consists of a rigid outer packaging enclosing a plastic inner receptacle together with any service or other structural equipment. The outer packaging of a composite IBC is designed to bear the entire stacking load. The inner receptacle and outer packaging form an integral packaging and are filled, stored, transported, and emptied as a unit. (2) The term plastic means polymeric materials ( i.e. , plastic or rubber). (3) A “rigid” inner receptacle is an inner receptacle which retains its general shape when empty without closures in place and without benefit of the outer casing. Any inner receptacle that is not “rigid” is considered to be “flexible.” (c) Construction requirements for composite IBCs with plastic inner receptacles are as follows: (1) The outer packaging must consist of rigid material formed so as to protect the inner receptacle from physical damage during handling and transportation, but is not required to perform the secondary containment function. It includes the base pallet where appropriate. The inner receptacle is not intended to perform a containment function without the outer packaging. (2) A composite IBC with a fully enclosing outer packaging must be designed to permit assessment of the integrity of the inner container following the leakproofness and hydraulic tests. The outer packaging of 31HZ2 composite IBCs must enclose the inner receptacles on all sides. (3) The inner receptacle must be manufactured from plastic material of known specifications and be of a strength relative to its capacity and to the service it is required to perform. In addition to conformance with the requirements of § 173.24 of this subchapter, the material must be resistant to aging and to degradation caused by ultraviolet radiation. The inner receptacle of 31HZ2 composite IBCs must consist of at least three plies of film. (i) If necessary, protection against ultraviolet radiation must be provided by the addition of pigments or inhibitors such as carbon black. These additives must be compatible with the contents and remain effective throughout the life of the inner receptacle. Where use is made of carbon black, pigments, or inhibitors, other than those used in the manufacture of the tested design type, retesting may be omitted if the carbon black content, the pigment content, or the inhibitor content do not adversely affect the physical properties of the material of construction. (ii) Additives may be included in the composition of the plastic material of the inner receptacle to improve resistance to aging, provided they do not adversely affect the physical or chemical properties of the material. (iii) No used material, other than production residues or regrind from the same manufacturing process, may be used in the manufacture of inner receptacles unless approved by the Associate Administrator. (iv) Composite IBCs intended for the transportation of liquids must be capable of releasing a sufficient amount of vapor to prevent the body of the IBC from rupturing if it is subjected to an internal pressure in excess of that for which it was hydraulically tested. This may be achieved by spring-loaded or non-reclosing pressure relief devices or by other means of construction. (4) The strength of the construction material comprising the outer packaging and the manner of construction must be appropriate to the capacity of the composite IBC and its intended use. The outer packaging must be free of any projection that might damage the inner receptacle. (i) Outer packagings of natural wood must be constructed of well seasoned wood that is commercially dry and free from defects that would materially lessen the strength of any part of the outer packaging. The tops and bottoms may be made of water-resistant reconstituted wood such as hardboard or particle board. Materials other than natural wood may be used for construction of structural equipment of the outer packaging. (ii) Outer packagings of plywood must be made of well-seasoned, rotary cut, sliced, or sawn veneer, commercially dry and free from defects that would materially lessen the strength of the casing. All adjacent plies must be glued with water-resistant adhesive. Materials other than plywood may be used for construction of structural equipment of the outer packaging. Outer packagings must be firmly nailed or secured to corner posts or ends or be assembled by equally suitable devices. (iii) Outer packagings of reconstituted wood must be constructed of water-resistant reconstituted wood such as hardboard or particle board. Materials other than reconstituted wood may be used for the construction of structural equipment of reconstituted wood outer packaging. (iv) Fiberboard outer packagings must be constructed of strong, solid, or double-faced corrugated fiberboard (single or multiwall). (A) Water resistance of the outer surface must be such that the increase in mass, as determined in a test carried out over a period of 30 minutes by the Cobb method of determining water absorption, is not greater than 155 grams per square meter (0.0316 pounds per square foot)—see ISO 535 (E) (IBR, see § 171.7 of this subchapter). Fiberboard must have proper bending qualities. Fiberboard must be cut, creased without cutting through any thickness of fiberboard, and slotted so as to permit assembly without cracking, surface breaks, or undue bending. The fluting of corrugated fiberboard must be firmly glued to the facings. (B) The ends of fiberboard outer packagings may have a wooden frame or be constructed entirely of wood. Wooden battens may be used for reinforcements. (C) Manufacturers' joints in the bodies of outer packagings must be taped, lapped and glued, or lapped and stitched with metal staples. (D) Lapped joints must have an appropriate overlap. (E) Where closing is effected by gluing or taping, a water-resistant adhesive must be used. (F) All closures must be sift-proof. (v) Outer packagings of plastic materials must be constructed in accordance with the relevant provisions of paragraph (c)(3) of this section. (5) Any integral pallet base forming part of an IBC, or any detachable pallet, must be suitable for the mechanical handling of an IBC filled to its maximum permissible gross mass. (i) The pallet or integral base must be designed to avoid protrusions that may cause damage to the IBC in handling. (ii) The outer packaging must be secured to any detachable pallet to ensure stability in handling and transportation. Where a detachable pallet is used, its top surface must be free from sharp protrusions that might damage the IBC. (iii) Strengthening devices, such as timber supports to increase stacking performance, may be used but must be external to the inner receptacle. (iv) The load-bearing surfaces of IBCs intended for stacking must be designed to distribute loads in a stable manner. An IBC intended for stacking must be designed so that loads are not supported by the inner receptacle. (6) Intermediate IBCs of type 31HZ2 must be limited to a capacity of not more than 1,250 L. (d) Composite IBCs may not have a volumetric capacity greater than 3,000 L (793 gallons) or less than 450 L (119 gallons)." 49:49:3.1.1.1.1.11.1.8,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.708 Standards for fiberboard IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended at 66 FR 45386, Aug. 28, 2001; 68 FR 75758, Dec. 31, 2003; 75 FR 5396, Feb. 2, 2010]","(a) The provisions of this section apply to fiberboard IBCs intended to contain solids that are loaded or discharged by gravity. Fiberboard IBCs are designated: 11G. (b) Definitions for fiberboard IBC types: (1) Fiberboard IBCs consist of a fiberboard body with or without separate top and bottom caps, appropriate service and structural equipment, and if necessary an inner liner (but no inner packaging). (2) Liner means a separate tube or bag, including the closures of its openings, inserted in the body but not forming an integral part of it. (c) Construction requirements for fiberboard IBCs are as follows: (1) Top lifting devices are prohibited in fiberboard IBCs. (2) Fiberboard IBCs must be constructed of strong, solid or double-faced corrugated fiberboard (single or multiwall) that is appropriate to the capacity of the outer packaging and its intended use. Water resistance of the outer surface must be such that the increase in mass, as determined in a test carried out over a period of 30 minutes by the Cobb method of determining water absorption, is not greater than 155 grams per square meter (0.0316 pounds per square foot)—see ISO 535 (E) (IBR, see § 171.7 of this subchapter). Fiberboard must have proper bending qualities. Fiberboard must be cut, creased without cutting through any thickness of fiberboard, and slotted so as to permit assembly without cracking, surface breaks, or undue bending. The fluting of corrugated fiberboard must be firmly glued to the facings. (i) The walls, including top and bottom, must have a minimum puncture resistance of 15 Joules (11 foot-pounds of energy) measured according to ISO 3036 (IBR, see § 171.7 of this subchapter). (ii) Manufacturers' joints in the bodies of IBCs must be made with an appropriate overlap and be taped, glued, stitched with metal staples or fastened by other means at least equally effective. Where joints are made by gluing or taping, a water-resistant adhesive must be used. Metal staples must pass completely through all pieces to be fastened and be formed or protected so that any inner liner cannot be abraded or punctured by them. (3) The strength of the material used and the construction of the liner must be appropriate to the capacity of the IBC and the intended use. Joints and closures must be sift-proof and capable of withstanding pressures and impacts liable to occur under normal conditions of handling and transport. (4) Any integral pallet base forming part of an IBC, or any detachable pallet, must be suitable for the mechanical handling of an IBC filled to its maximum permissible gross mass. (i) The pallet or integral base must be designed to avoid protrusions that may cause damage to the IBC in handling. (ii) The outer packaging must be secured to any detachable pallet to ensure stability in handling and transport. Where a detachable pallet is used, its top surface must be free from sharp protrusions that might damage the IBC. (iii) Strengthening devices, such as timber supports to increase stacking performance, may be used but must be external to the inner liner. (iv) The load-bearing surfaces of IBCs intended for stacking must be designed to distribute loads in a stable manner. (d) Fiberboard IBCs may not have a volumetric capacity greater than 3,000 L (793 gallons) or less than 450 L (119 gallons)." 49:49:3.1.1.1.1.11.1.9,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,N,Subpart N—IBC Performance-Oriented Standards,,§ 178.709 Standards for wooden IBCs.,PHMSA,,,"[Amdt. 178-103, 59 FR 38068, July 26, 1994, as amended at 66 FR 45386, Aug. 28, 2001; 75 FR 5397, Feb. 2, 2010]","(a) The provisions in this section apply to wooden IBCs intended to contain solids that are loaded or discharged by gravity. Wooden IBC types are designated: (1) 11C Natural wood with inner liner. (2) 11D Plywood with inner liner. (3) 11F Reconstituted wood with inner liner. (b) Definitions for wooden IBCs: (1) Wooden IBCs consist of a rigid or collapsible wooden body together with an inner liner (but no inner packaging) and appropriate service and structural equipment. (2) Liner means a separate tube or bag, including the closures of its openings, inserted in the body but not forming an integral part of it. (c) Construction requirements for wooden IBCs are as follows: (1) Top lifting devices are prohibited in wooden IBCs. (2) The strength of the materials used and the method of construction must be appropriate to the capacity and intended use of the IBC. (i) Natural wood used in the construction of an IBC must be well-seasoned, commercially dry, and free from defects that would materially lessen the strength of any part of the IBC. Each IBC part must consist of uncut wood or a piece equivalent in strength and integrity. IBC parts are equivalent to one piece when a suitable method of glued assembly is used ( i.e. , a Lindermann joint, tongue and groove joint, ship lap or rabbet joint, or butt joint with at least two corrugated metal fasteners at each joint, or when other methods at least equally effective are used). Materials other than natural wood may be used for the construction of structural equipment of the outer packaging. (ii) Plywood used in construction of bodies must be at least 3-ply. Plywood must be made of well-seasoned, rotary-cut, sliced or sawn veneer, commercially dry, and free from defects that would materially lessen the strength of the body. All adjacent plies must be glued with water-resistant adhesive. Materials other than plywood may be used for the construction of structural equipment of the outer packaging. (iii) Reconstituted wood used in construction of bodies must be water resistant reconstituted wood such as hardboard or particle board. Materials other than reconstituted wood may be used for the construction of structural equipment of the outer packaging. (iv) Wooden IBCs must be firmly nailed or secured to corner posts or ends or be assembled by similar devices. (3) The strength of the material used and the construction of the liner must be appropriate to the capacity of the IBC and its intended use. Joints and closures must be sift-proof and capable of withstanding pressures and impacts liable to occur under normal conditions of handling and transportation. (4) Any integral pallet base forming part of an IBC, or any detachable pallet, must be suitable for the mechanical handling of an IBC filled to its maximum permissible gross mass. (i) The pallet or integral base must be designed to avoid protrusions that may cause damage to the IBC in handling. (ii) The outer packaging must be secured to any detachable pallet to ensure stability in handling and transportation. Where a detachable pallet is used, its top surface must be free from sharp protrusions that might damage the IBC. (iii) Strengthening devices, such as timber supports to increase stacking performance, may be used but must be external to the inner liner. (iv) The load-bearing surfaces of IBCs intended for stacking must be designed to distribute loads in a stable manner. (d) Wooden IBCs may not have a volumetric capacity greater than 3,000 L (793 gallons) or less than 450 L (119 gallons)." 49:49:3.1.1.1.1.12.1.1,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,O,Subpart O—Testing of IBCs,,§ 178.800 Purpose and scope.,PHMSA,,,"[Amdt. 178-103, 59 FR 38074, July 26, 1994, as amended by 66 FR 45386, Aug. 28, 2001]",This subpart prescribes certain testing requirements for IBCs identified in subpart N of this part. 49:49:3.1.1.1.1.12.1.10,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,O,Subpart O—Testing of IBCs,,§ 178.815 Stacking test.,PHMSA,,,"[75 FR 5397, Feb. 2, 2010]","(a) General. The stacking test must be conducted for the qualification of all IBC design types intended to be stacked. (b) Special preparation for the stacking test. (1) All IBCs except flexible IBC design types must be loaded to their maximum permissible gross mass. (2) The flexible IBC must be filled to not less than 95 percent of its capacity and to its maximum net mass, with the load being evenly distributed. (c) Test method. (1) Design Qualification Testing. All IBCs must be placed on their base on level, hard ground and subjected to a uniformly distributed superimposed test load for a period of at least five minutes (see paragraph (c)(5) of this section). (2) Fiberboard, wooden and composite IBCs with outer packagings constructed of other than plastic materials must be subject to the test for 24 hours. (3) Rigid plastic IBC types and composite IBC types with plastic outer packagings (11HH1, 11HH2, 21HH1, 21HH2, 31HH1 and 31HH2) which bear the stacking load must be subjected to the test for 28 days at 40 °C (104 °F). (4) For all IBCs, the load must be applied by one of the following methods: (i) One or more IBCs of the same type loaded to their maximum permissible gross mass and stacked on the test IBC; (ii) The calculated superimposed test load weight loaded on either a flat plate or a reproduction of the base of the IBC, which is stacked on the test IBC. (5) Calculation of superimposed test load. For all IBCs, the load to be placed on the IBC must be 1.8 times the combined maximum permissible gross mass of the number of similar IBCs that may be stacked on top of the IBC during transportation. (d) Periodic Retest. (1) The package must be tested in accordance with paragraph (c) of this section; or (2) The packaging may be tested using a dynamic compression testing machine. The test must be conducted at room temperature on an empty, unsealed packaging. The test sample must be centered on the bottom platen of the testing machine. The top platen must be lowered until it comes in contact with the test sample. Compression must be applied end to end. The speed of the compression tester must be one-half inch plus or minus one-fourth inch per minute. An initial preload of 50 pounds must be applied to ensure a definite contact between the test sample and the platens. The distance between the platens at this time must be recorded as zero deformation. The force “A” then to be applied must be calculated using the applicable formula: Liquids: A = (1.8)(n − 1) [w + (s × v × 8.3 × .98)] × 1.5; or Solids: A = (1.8)(n − 1) [w + (s × v × 8.3 × .95)] × 1.5 Where: A = applied load in pounds. n = maximum number of IBCs being stacked during transportation. w = maximum weight of one empty container in pounds. s = specific gravity (liquids) or density (solids) of the lading. v = actual capacity of container (rated capacity + outage) in gallons. and: 8.3 corresponds to the weight in pounds of 1.0 gallon of water. 1.5 is a compensation factor converting the static load of the stacking test into a load suitable for dynamic compression testing. Where: A = applied load in pounds. n = maximum number of IBCs being stacked during transportation. w = maximum weight of one empty container in pounds. s = specific gravity (liquids) or density (solids) of the lading. v = actual capacity of container (rated capacity + outage) in gallons. and: 8.3 corresponds to the weight in pounds of 1.0 gallon of water. 1.5 is a compensation factor converting the static load of the stacking test into a load suitable for dynamic compression testing. (e) Criteria for passing the test. (1) For metal, rigid plastic, and composite IBCs, there may be no permanent deformation, which renders the IBC unsafe for transportation, and no loss of contents. (2) For fiberboard and wooden IBCs, there may be no loss of contents and no permanent deformation, which renders the whole IBC, including the base pallet, unsafe for transportation. (3) For flexible IBCs, there may be no deterioration, which renders the IBC unsafe for transportation, and no loss of contents. (4) For the dynamic compression test, a container passes the test if, after application of the required load, there is no permanent deformation to the IBC, which renders the whole IBC, including the base pallet, unsafe for transportation; in no case may the maximum deflection exceed one inch." 49:49:3.1.1.1.1.12.1.11,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,O,Subpart O—Testing of IBCs,,§ 178.816 Topple test.,PHMSA,,,"[Amdt. 178-103, 59 FR 38074, July 26, 1994, as amended at 66 FR 45386, Aug. 28, 2001]","(a) General. The topple test must be conducted for the qualification of all flexible IBC design types. (b) Special preparation for the topple test. The flexible IBC must be filled to not less than 95 percent of its capacity and to its maximum net mass, with the load being evenly distributed. (c) Test method. A flexible IBC must be toppled onto any part of its top upon a rigid, non-resilient, smooth, flat, and horizontal surface. (d) Topple height. For all flexible IBCs, the topple height is specified as follows: (1) Packing Group I: 1.8 m (5.9 feet). (2) Packing Group II: 1.2 m (3.9 feet). (3) Packing Group III: 0.8 m (2.6 feet). (e) Criteria for passing the test. For all flexible IBCs, there may be no loss of contents. A slight discharge (e.g., from closures or stitch holes) upon impact is not considered to be a failure, provided no further leakage occurs." 49:49:3.1.1.1.1.12.1.12,49,Transportation,I,C,178,PART 178—SPECIFICATIONS FOR PACKAGINGS,O,Subpart O—Testing of IBCs,,§ 178.817 Righting test.,PHMSA,,,"[Amdt. 178-103, 59 FR 38074, July 26, 1994, as amended at 66 FR 45386, Aug. 28, 2001]","(a) General. The righting test must be conducted for the qualification of all flexible IBCs designed to be lifted from the top or side. (b) Special preparation for the righting test. The flexible IBC must be filled to not less than 95 percent of its capacity and to its maximum net mass, with the load being evenly distributed. (c) Test method. The flexible IBC, lying on its side, must be lifted at a speed of at least 0.1 m/second (0.33 ft/s) to an upright position, clear of the floor, by one lifting device, or by two lifting devices when four are provided. (d) Criterion for passing the test. For all flexible IBCs, there may be no damage to the IBC or its lifting devices which renders the IBC unsafe for transportation or handling."