Title 21—Food and Drugs--Volume 1
PART 178—INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND SANITIZERS
§ 178.1005   Hydrogen peroxide solution.
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.
§ 178.1010   Sanitizing solutions.
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.
§ 178.2010   Antioxidants and/or stabilizers for polymers.
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.
§ 178.2550   4-Hydroxymethyl-2,6-di-tert-butylphenol.
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.
§ 178.2650   Organotin stabilizers in vinyl chloride plastics.
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:
§ 178.3010   Adjuvant substances used in the manufacture of foamed plastics.
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:
§ 178.3120   Animal glue.
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.
§ 178.3125   Anticorrosive agents.
The substances listed in this section may be used as anticorrosive agents in food-contact materials subject to the provisions of this section:
§ 178.3130   Antistatic and/or antifogging agents in food-packaging materials.
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:
§ 178.3280   Castor oil, hydrogenated.
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:
§ 178.3290   Chromic chloride complexes.
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.
§ 178.3295   Clarifying agents for polymers.
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:
§ 178.3297   Colorants for polymers.
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:
§ 178.3300   Corrosion inhibitors used for steel or tinplate.
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:
§ 178.3400   Emulsifiers and/or surface-active agents.
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.
§ 178.3450   Esters of stearic and palmitic acids.
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.
§ 178.3480   Fatty alcohols, synthetic.
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.
§ 178.3500   Glycerin, synthetic.
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.
§ 178.3505   Glyceryl tri-(12-acetoxystearate).
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.
§ 178.3520   Industrial starch-modified.
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:
(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.
§ 178.3530   Isoparaffinic petroleum hydrocarbons, synthetic.
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:
(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.
§ 178.3570   Lubricants with incidental food contact.
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.
§ 178.3600   Methyl glucoside-coconut oil ester.
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.
§ 178.3610   α-Methylstyrene-vinyltoluene resins, hydrogenated.
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.
§ 178.3620   Mineral oil.
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:
(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:
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).
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:
Also calculate the pyrene content of the oil sample in parts per million as follows:
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.
§ 178.3650   Odorless light petroleum hydrocarbons.
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:
§ 178.3690   Pentaerythritol adipate-stearate.
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.
§ 178.3700   Petrolatum.
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.
§ 178.3710   Petroleum wax.
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.
§ 178.3720   Petroleum wax, synthetic.
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.
§ 178.3725   Pigment dispersants.
Subject to the provisions of this regulation, the substances listed in this section may be safely used as pigment dispersants in food-contact materials.
§ 178.3730   Piperonyl butoxide and pyrethrins as components of bags.
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.
§ 178.3740   Plasticizers in polymeric substances.
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.
§ 178.3750   Polyethylene glycol (mean molecular weight 200-9,500).
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.
§ 178.3760   Polyethylene glycol (400) monolaurate.
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.
§ 178.3770   Polyhydric alcohol esters of oxidatively refined (Gersthofen process) montan wax acids.
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.
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.
§ 178.3780   Polyhydric alcohol esters of long chain monobasic acids.
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.
§ 178.3790   Polymer modifiers in semirigid and rigid vinyl chloride plastics.
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:
(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:
(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:
(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.
§ 178.3800   Preservatives for wood.
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:
§ 178.3850   Reinforced wax.
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.
§ 178.3860   Release agents.
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:
§ 178.3870   Rosins and rosin derivatives.
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.
§ 178.3900   Sodium pentachlorophenate.
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.
§ 178.3910   Surface lubricants used in the manufacture of metallic articles.
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:
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.
§ 178.3930   Terpene resins.
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.
§ 178.3940   Tetraethylene glycol di-(2-ethylhexoate).
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.
§ 178.3950   Tetrahydrofuran.
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.