Title 21—Food and Drugs--Volume 1
PART 175—INDIRECT FOOD ADDITIVES: ADHESIVES AND COMPONENTS OF COATINGS
§ 175.105   Adhesives.
(a) Adhesives may be safely used as components of articles intended for use in packaging, transporting, or holding food in accordance with the following prescribed conditions:
(1) The adhesive is prepared from one or more of the optional substances named in paragraph (c) of this section, subject to any prescribed limitations.
(2) The adhesive is either separated from the food by a functional barrier or used subject to the following additional limitations:
(i) In dry foods. The quantity of adhesive that contacts packaged dry food shall not exceed the limits of good manufacturing practice.
(ii) In fatty and aqueous foods. ( a ) The quantity of adhesive that contacts packaged fatty and aqueous foods shall not exceed the trace amount at seams and at the edge exposure between packaging laminates that may occur within the limits of good manufacturing practice.
( b ) Under normal conditions of use the packaging seams or laminates will remain firmly bonded without visible separation.
(b) To assure safe usage of adhesives, the label of the finished adhesive container shall bear the statement “food-packaging adhesive”.
(c) Subject to any limitation prescribed in this section and in any other regulation promulgated under section 409 of the Act which prescribes safe conditions of use for substances that may be employed as constituents of adhesives, the optional substances used in the formulation of adhesives may include the following:
(1) Substances generally recognized as safe for use in food or food packaging.
(2) Substances permitted for use in adhesives by prior sanction or approval and employed under the specific conditions of use prescribed by such sanction or approval.
(3) Flavoring substances permitted for use in food by regulations in this part, provided that such flavoring substances are volatilized from the adhesives during the packaging fabrication process.
(4) Color additives approved for use in food.
(5) Substances permitted for use in adhesives by other regulations in this subchapter and substances named in this subparagraph: Provided, however, That any substance named in this paragraph and covered by a specific regulation in this subchapter, must meet any specifications in such regulation.
§ 175.125   Pressure-sensitive adhesives.
Pressure-sensitive adhesives may be safely used as the food-contact surface of labels and/or tapes applied to food, in accordance with the following prescribed conditions:
(a) Pressure-sensitive adhesives prepared from one or a mixture of two or more of the substances listed in this paragraph may be used as the food-contact surface of labels and/or tapes applied to poultry, dry food, and processed, frozen, dried, or partially dehydrated fruits or vegetables.
(1) Substances generally recognized as safe in food.
(2) Substances used in accordance with a prior sanction or approval.
(3) Color additives listed for use in or on food in parts 73 and 74 of this chapter.
(4) Substances identified in § 172.615 of this chapter other than substances used in accordance with paragraph (a)(2) of this section.
(5) Polyethylene, oxidized; complying with the identity prescribed in § 177.1620(a) of this chapter.
(6) 4-[[4, 6-Bis(octylthio)- s -triazin-2-yl]amino]-2,6-di- tert -butylphenol (CAS Reg. No. 991-84-4) as an antioxidant/stabilizer at a level not to exceed 1.5 percent by weight of the finished pressure-sensitive adhesive.
(7) 2,2′-(2,5-Thiophenediyl)-bis(5- tert -butylbenzoxazole) (CAS Reg. No. 7128-64-5) as an optical brightener at a level not to exceed 0.05 percent by weight of the finished pressure-sensitive adhesive.
(8) 2-Hydroxy-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-propanone (CAS Reg. No. 106797-53-9) as a photoinitiator at a level not to exceed 5 percent by weight of the pressure-sensitive adhesive.
(9) Butanedioic acid, sulfo-1,4-di-(C 9 -C 11 alkyl) ester, ammonium salt (also known as butanedioic acid sulfo-1, 4-diisodecyl ester, ammonium salt [CAS Reg. No. 144093-88-9]) as a surface active agent at a level not to exceed 3.0 percent by weight of the finished pressure-sensitive adhesive.
(b) Pressure-sensitive adhesives prepared from one or a mixture of two or more of the substances listed in this paragraph may be used as the food-contact surface of labels and/or tapes applied to raw fruit and raw vegetables.
(1) Substances listed in paragraphs (a)(1), (a)(2), (a)(3), (a)(5), (a)(6), (a)(7), (a)(8), and (a)(9) of this section, and those substances prescribed by paragraph (a)(4) of this section that are not identified in paragraph (b)(2) of this section.
(2) Substances identified in this subparagraph and subject to the limitations provided:
(c) Acrylonitrile copolymers identified in this section shall comply with the provisions of § 180.22 of this chapter.
§ 175.210   Acrylate ester copolymer coating.
Acrylate ester copolymer coating may safely be used as a food-contact surface of articles intended for packaging and holding food, including heating of prepared food, subject to the provisions of this section:
(a) The acrylate ester copolymer is a fully polymerized copolymer of ethyl acrylate, methyl methacrylate, and methacrylic acid applied in emulsion form to molded virgin fiber and heat-cured to an insoluble resin.
(b) Optional substances used in the preparation of the polymer and in the preparation and application of the emulsion may include substances named in this paragraph, in an amount not to exceed that required to accomplish the desired technical effect and subject to any limitation prescribed: Provided, however, That any substance named in this paragraph and covered by a specific regulation in subchapter B of this chapter must meet any specifications in such regulation.
(c) The coating in the form in which it contacts food meets the following tests:
(1) An appropriate sample when exposed to distilled water at 212 °F for 30 minutes shall yield total chloroform-soluble extractables not to exceed 0.5 milligram per square inch.
(2) An appropriate sample when exposed to n- heptane at 120 °F for 30 minutes shall yield total chloroform-soluble extractables not to exceed 0.5 milligram per square inch.
§ 175.230   Hot-melt strippable food coatings.
Hot-melt strippable food coatings may be safely applied to food, subject to the provisions of this section.
(a) The coatings are applied to and used as removable coatings for food.
(b) The coatings may be prepared, as mixtures, from the following substances:
(1) Substances generally recognized as safe in food.
(2) Substances identified in this subparagraph.
§ 175.250   Paraffin (synthetic).
Synthetic paraffin may be safely used as an impregnant in, coating on, or component of coatings on articles used in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food in accordance with the following prescribed conditions:
(a) The additive is synthesized by the Fischer-Tropsch process from carbon monoxide and hydrogen, which are catalytically converted to a mixture of paraffin hydrocarbons. Lower molecular-weight fractions are removed by distillation. The residue is hydrogenated and may be further treated by percolation through activated charcoal. This mixture can be fractionated into its components by a solvent separation method, using synthetic isoparaffinic petroleum hydrocarbons complying with § 178.3530 of this chapter.
(b) Synthetic paraffin shall conform to the following specifications:
(1) Congealing point. There is no specification for the congealing point of synthetic paraffin components, except those components that have a congealing point below 50 °C when used in contact with food Types III, IVA, V, VIIA, and IX identified in table 1 of § 176.170(c) of this chapter and under conditions of use E, F, and G described in table 2 of § 176.170(c) of this chapter shall be limited to a concentration not exceeding 15 percent by weight of the finished coating. The congealing point shall be determined by ASTM method D938-71 (Reapproved 1981), “Standard Test Method for Congealing Point of Petroleum Waxes, Including Petrolatum,” 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) Oil content. The substance has an oil content not exceeding 2.5 percent as determined by ASTM method D721-56T, “Tentative Method of Test for Oil Content of Petroleum Waxes” (Revised 1956), which is incorporated by reference. See paragraph (b)(1) of this section for availability of the incorporation by reference.
(3) Absorptivity. The substance has an absorptivity at 290 millimicrons in decahydronaphthalene at 88 °C not exceeding 0.01 as determined by ASTM method E131-81a, “Standard Definitions of Terms and Symbols Relating to Molecular-Spectroscopy,” which is incorporated by reference. See paragraph (b)(1) of this section for availability of the incorporation by reference.
(c) The provisions of this section are not applicable to synthetic paraffin used in food-packaging adhesives complying with § 175.105.
§ 175.260   Partial phosphoric acid esters of polyester resins.
Partial phosphoric acid esters of polyester resins identified in this section and applied on aluminum may be safely used as food-contact coatings, in accordance with the following prescribed conditions:
(a) For the purpose of this section, partial phosphoric acid esters of polyester resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an acid number of 81 to 98 and a phosphorus content of 4.05 to 4.65 percent by weight.
(b) The coating is chemically bonded to the metal and cured at temperatures exceeding 450 °F.
(c) The finished food-contact coating, 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 § 175.300(d), yields total extractives in each extracting solvent not to exceed 0.3 milligrams per square inch of food-contact surface, as determined by the methods described in § 175.300(e), and the coating yields 2,2-dimethyl-1,3-propanediol in each extracting solvent not to exceed 0.3 micrograms per square inch of food-contact surface. In testing the finished food-contact articles, a separate test sample is to be used for each required extracting solvent.
§ 175.270   Poly(vinyl fluoride) resins.
Poly(vinyl fluoride) resins identified in this section may be safely used as components of food-contact coatings for containers having a capacity of not less than 5 gallons, subject to the provisions of this section.
(a) For the purpose of this section, poly(vinyl fluoride) resins consist of basic resins produced by the polymerization of vinyl fluoride.
(b) The poly(vinyl fluoride) basic resins have an intrinsic viscosity of not less than 0.75 deciliter per gram as determined by ASTM method D1243-79, “Standard Test Method for Dilute Solution Viscosity of Vinyl Chloride Polymers,” 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.
(1) Solvent. N,N- Dimethylacetamide, technical grade.
(2) Solution. Powdered resin and solvent are heated at 120 °C until the resin is dissolved.
(3) Temperature. Flow times of the solvent and solution are determined at 110 °C.
(4) Viscometer. Cannon-Ubbelohde size 50 semimicro dilution viscometer (or equivalent).
(5) Calculation. The calculation method used is that described in appendix X 1.3 (ASTM method D1243-79, “Standard Test Method for Dilute Solution Viscosity of Vinyl Chloride Polymers,” which is incorporated by reference; see paragraph (b) of this section for availability of the incorporation by reference) with the reduced viscosity determined for three concentration levels not greater than 0.5 gram per deciliter and extrapolated to zero concentration for intrinsic viscosity. The following formula is used for determining reduced viscosity:
§ 175.300   Resinous and polymeric coatings.
Resinous and polymeric coatings may be safely used as the food-contact surface of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, in accordance with the following prescribed conditions:
(a) The coating is applied as a continuous film or enamel over a metal substrate, or the coating is intended for repeated food-contact use and is applied to any suitable substrate as a continuous film or enamel that serves as a functional barrier between the food and the substrate. The coating is characterized by one or more of the following descriptions:
(1) Coatings cured by oxidation.
(2) Coatings cured by polymerization, condensation, and/or cross-linking without oxidation.
(3) Coatings prepared from prepolymerized substances.
(b) The coatings are formulated from optional substances that may include:
(1) Substances generally recognized as safe in food.
(2) Substances the use of which is permitted by regulations in this part or which are permitted by prior sanction or approval and employed under the specific conditions, if any, of the prior sanction or approval.
(3) Any substance employed in the production of resinous and polymeric coatings that is the subject of a regulation in subchapter B of this chapter and conforms with any specification in such regulation. Substances named in this paragraph (b)(3) and further identified as required:
(i) Drying oils, including the triglycerides or fatty acids derived therefrom:
(ii) Reconstituted oils from triglycerides or fatty acids derived from the oils listed in paragraph (b)(3)(i) of this section to form esters with:
(iii) Synthetic drying oils, as the basic polymer:
(iv) Natural fossil resins, as the basic resin:
(v) Rosins and rosin derivatives, with or without modification by polymerization, isomerization, incidental decarboxylation, and/or hydrogenation, as follows:
( a ) Rosins, refined to color grade of K or paler:
( b ) Rosin esters formed by reacting rosin (paragraph (b)(3)(v)( a ) of this section) with:
( c ) Rosin esters (paragraph (b)(3)(v)( b ) of this section) modified by reaction with:
( d ) Rosin salts:
(vi) Phenolic resins as the basic polymer formed by reaction of phenols with formaldehyde:
( a ) Phenolic resins formed by reaction of formaldehyde with:
( b ) Adjunct for phenolic resins: Aluminum butylate.
(vii) Polyester resins (including alkyd-type), as the basic polymers, formed as esters of acids listed in paragraph (b)(3)(vii)( a ) and ( b ) of this section by reaction with alcohols in paragraph (b)(3)(vii)( c ) and ( d ) of this section.
( a ) Polybasic acids:
( b ) Monobasic acids:
( c ) Polyhydric alcohols:
( d ) Monohydric alcohols:
( e ) Catalysts:
(viii) Epoxy resins, catalysts, and adjuncts:
( a ) Epoxy resins, as the basic polymer:
( b ) Catalysts and cross-linking agents for epoxy resins:
( c ) Adjuncts for epoxy resins:
(ix) Coumarone-indene resin, as the basic polymer.
(x) Petroleum hydrocarbon resin (cyclopentadiene type), as the basic polymer.
(xi) Terpene resins, as the basic polymer, from one or more of the following:
(xii) Urea-formaldehyde, resins and their curing catalyst:
( a ) Urea-formaldehyde resins, as the basic polymer:
( b ) Curing (cross-linking) catalyst for urea-formaldehyde resins:
(xiii) Triazine-formaldehyde resins and their curing catalyst:
( a ) Triazine-formaldehyde resins, as the basic polymer:
( b ) Curing (cross-linking) catalyst for triazine-formaldehyde resins:
(xiv) Modifiers (for oils and alkyds, including polyesters), as the basic polymer:
(xv) Vinyl resinous substance, as the basic polymers:
(xvi) Cellulosics, as the basic polymer:
(xvii) Styrene polymers, as the basic polymer:
Acrylonitrile.
α-Methylstyrene.
(xviii) Polyethylene and its copolymers as the basic polymer:
(xix) Polypropylene as the basic polymer:
(xx) Acrylics and their copolymers, as the basic polymer:
(xxi) Elastomers, as the basic polymer:
(xxii) Driers made by reaction of a metal from paragraph (b)(3)(xxii)( a ) of this section with acid, to form the salt listed in paragraph (b)(3)(xxii)( b ) of this section:
( a ) Metals:
( b ) Salts:
(xxiii) Waxes:
(xxiv) Plasticizers:
(xxv) Release agents, as the basic polymer, when applicable:
(xxvi) Colorants used in accordance with § 178.3297 of this chapter.
(xxvii) Surface lubricants:
(xxviii) Silicones and their curing catalysts:
( a ) Silicones as the basic polymer:
( b ) Curing (cross-linking) catalysts for silicones (the maximum amount of tin catalyst used shall be that required to effect optimum cure but shall not exceed 1 part of tin per 100 parts of siloxane resins solids):
(xxix) Surface active agents:
(xxx) Antioxidants:
(xxxi) Can end cements (sealing compounds used for sealing can ends only): In addition to the substances listed in paragraph (b) of this section and those listed in § 177.1210(b)(5) of this chapter, the following may be used:
(xxxii) Side seam cements: In addition to the substances listed in paragraph (b)(3)(i) to (xxx), inclusive, of this section, the following may be used.
(xxxiii) Miscellaneous materials:
(xxxiv) Polyamide resins derived from dimerized vegetable oil acids (containing not more than 20 percent of monomer acids) and ethylenediamine, as the basic resin, for use only in coatings that contact food at temperatures not to exceed room temperature.
(xxxv) Polyamide resins having a maximum acid value of 5 and a maximum amine value of 8.5 derived from dimerized vegetable oil acids (containing not more than 10 percent of monomer acids), ethylenediamine, and 4,4-bis (4-hydroxyphenyl) pentanoic acid (in an amount not to exceed 10 percent by weight of said polyamide resins); as the basic resin, for use only in coatings that contact food at temperatures not to exceed room temperature provided that the concentration of the polyamide resins in the finished food-contact coating does not exceed 5 milligrams per square inch of food-contact surface.
(xxxvi) Methacrylonitrile grafted polybutadiene copolymers containing no more than 41 weight percent of total polymer units derived from methacrylonitrile; for use only in coatings that are intended for contact, under conditions of use D, E, F, or G described in table 2 of paragraph (d) of this section, with food containing no more than 8 percent of alcohol.
(xxxvii) Polymeric resin as a coating component prepared from terephthalic acid, isophthalic acid, succinic anhydride, ethylene glycol, diethylene glycol, and 2,2-dimethyl-1,3-propanediol for use in contact with aqueous foods and alcoholic foods containing not more than 20 percent (by volume) of alcohol under conditions of use D, E, F, and G described in table 2 of § 176.170 of this chapter. The resin shall contain no more than 30 weight percent of 2,2-dimethyl-1,3-propanediol.
(c) The coating in the finished form in which it is to contact food, when extracted with the solvent or solvents characterizing the type of food, and under conditions of time and temperature characterizing the conditions of its intended use as determined from tables 1 and 2 of paragraph (d) of this section, shall yield chloroform-soluble extractives, corrected for zinc extractives as zinc oleate, not to exceed the following:
(1) From a coating intended for or employed as a component of a container not to exceed 1 gallon and intended for one-time use, not to exceed 0.5 milligram per square inch nor to exceed that amount as milligrams per square inch that would equal 0.005 percent of the water capacity of the container, in milligrams, divided by the area of the food-contact surface of the container in square inches. From a fabricated container conforming with the description in this paragraph (c)(1), the extractives shall not exceed 0.5 milligram per square inch of food-contact surface nor exceed 50 parts per million of the water capacity of the container as determined by the methods provided in paragraph (e) of this section.
(2) From a coating intended for or employed as a component of a container having a capacity in excess of 1 gallon and intended for one-time use, not to exceed 1.8 milligrams per square inch nor to exceed that amount as milligrams per square inch that would equal 0.005 percent of the water capacity of the container in milligrams, divided by the area of the food-contact surface of the container in square inches.
(3) From a coating intended for or employed as a component of a container for repeated use, not to exceed 18 milligrams per square inch nor to exceed that amount as milligrams per square inch that would equal 0.005 percent of the water capacity of the container in milligrams, divided by the area of the food-contact surface of the container in square inches.
(4) From coating intended for repeated use, and employed other than as a component of a container, not to exceed 18 milligrams per square inch of coated surface.
(d) Tables:
Table 2—Test Procedures for Determining Amount of Extractives From Resinous or Polymeric Coatings, Using Solvents Simulating Types of Foods and Beverages
1 Heptane extractant not to be used on wax-lined containers.
2 Heptane extractivity results must be divided by a factor of five in arriving at the extractivity for a food product.
(e) Analytical methods —(1) Selection of extractability conditions. First ascertain the type of food product (table 1, paragraph (d) of this section) that is being packed commercially in the test container and the normal conditions of thermal treatment used in packaging the type of food involved. Using table 2 (paragraph (d) of this section), select the food-simulating solvent or solvents (demineralized distilled water, heptane, and/or 8 percent ethyl alcohol) and the time-temperature exaggerations of the container-use conditions. Aqueous products (Types I, II, IV-B, and VI-B) require only a water-extractability test at the temperature and time conditions shown for the most severe “conditions of use.” Aqueous products with free oil or fat, and water-oil emulsions (types III, IV-A, and VII) will require determinations of both water extractability and heptane extractability. Low-moisture fats and oils (type V with no free water) require only the heptane extractability. Alcoholic beverages (type VI-A) require only the 8 percent alcohol extractant. Having selected the appropriate extractant or extractants simulating various types of foods and beverages and the time-temperature exaggerations over normal use, follow the applicable extraction procedure. Adapt the procedure, when necessary, for containers having a capacity of over 1 gallon.
(2) Selection of coated-container samples. For consumer-sized containers up to 1 gallon, quadruplicate samples of representative containers (using for each replicate sample the number of containers nearest to an area of 180 square inches) should be selected from the lot to be examined.
(3) Cleaning procedure preliminary to determining the amount of extractables from coated containers. Quadruplicate samples of representative containers should be selected from the lot to be examined and must be carefully rinsed to remove extraneous material prior to the actual extraction procedure. Soda fountain pressure-type hot water rinsing equipment, consisting in its simplest form of a 1/8 -inch- 1/4 -inch internal diameter metal tube attached to a hot water line and bent so as to direct a stream of water upward, may be used. Be sure hot water has reached a temperature of 190 °F-200 °F before starting to rinse the container. Invert the container over the top of the fountain and direct a strong stream of hot water against the bottom and all sides for 1 minute, drain, and allow to dry.
(4) Exposure conditions —(i) Water ( 250 °F for 2 hours ), simulating high-temperature heat sterilization. Fill the container within 1/4 -inch of the top with a measured volume of demineralized distilled water. Cover the container with clean aluminum foil and place the container on a rack in a pressure cooker. Add a small amount of demineralized distilled water to the pressure cooker, but do not allow the water to touch the bottom of the container. Close the cooker securely and start to heat over a suitable burner. When a steady stream of steam emerges from the vent, close the vent and allow the pressure to rise to 15 pounds per square inch (250 °F) and continue to maintain this pressure for 2 hours. Slowly release the pressure, open the pressure cooker when the pressure reads zero, and composite the water of each replicate immediately in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(ii) Water ( 212 °F for 30 minutes ), simulating boiling water sterilization. Fill the container within 1/4 -inch of the top with a measured volume of boiling, demineralized distilled water. Cover the container with clean aluminum foil and place the container on a rack in a pressure cooker in which a small amount of demineralized distilled water is boiling. Do not close the pressure vent, but operate at atmospheric pressure so that there is a continuous escape of a small amount of steam. Continue to heat for 30 minutes, then remove the test container and composite the contents of each replicate immediately in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(iii) Water ( from boiling to 100 °F ), simulating hot fill or pasteurization above 150 °F. Fill the container within 1/4 -inch of the top with a measured volume of boiling, demineralized distilled water. Insert a thermometer in the water and allow the uncovered container to stand in a room at 70 °F-85 °F. When the temperature reads 100 °F, composite the water from each replicate immediately in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(iv) Water ( 150° for 2 hours ), simulating hot fill or pasteurization below 150 °F. Preheat demineralized distilled water to 150 °F in a clean Pyrex flask. Fill the container within 1/4 -inch of the top with a measured volume of the 150 °F water and cover with clean aluminum foil. Place the test container in an oven maintained at 150 °F. After 2 hours, remove the test container from the oven and immediately composite the water of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(v) Water ( 120 °F for 24 hours ), simulating room temperature filling and storage. Preheat demineralized distilled water to 120 °F in a clean Pyrex flask. Fill the container within 1/4 -inch of the top with a measured volume of the 120 °F water and cover with clean aluminum foil. Place the test container in an incubator or oven maintained at 120 °F. After 24 hours, remove the test container from the incubator and immediately composite the water of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(vi) Water ( 70 °F for 48 hours ), simulating refrigerated storage. Bring demineralized distilled water to 70 °F in a clean Pyrex flask. Fill the container within 1/4 -inch of the top with a measured volume of the 70 °F water, and cover with clean aluminum foil. Place the test container in a suitable room maintained at 70 °F. After 48 hours, immediately composite the water of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(vii) Water ( 70 °F for 24 hours ), simulating frozen storage. Bring demineralized distilled water to 70 °F in a clean Pyrex flask. Fill the container within 1/4 -inch of the top with a measured volume of the 70 °F water and cover with clean aluminum foil. Place the container in a suitable room maintained at 70 °F. After 24 hours, immediately composite the water of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(viii) Water ( 212 °F for 30 minutes ), simulating frozen foods reheated in the container. Fill the container to within 1/4 -inch of the top with a measured volume of boiling, demineralized distilled water. Cover the container with clean aluminum foil and place the container on a rack in a pressure cooker in which a small amount of demineralized distilled water is boiling. Do not close the pressure vent, but operate at atmospheric pressure so that there is a continuous escape of a small amount of steam. Continue to heat for 30 minutes, then remove the test container and composite the contents of each replicate immediately in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(ix) Heptane ( 150 °F for 2 hours ) simulating high-temperature heat sterilization for fatty foods only. Preheat redistilled reagent-grade heptane (boiling point 208 °F) carefully in a clean Pyrex flask on a water bath or nonsparking hot plate in a well-ventilated hood to 150 °F. At the same time preheat a pressure cooker or equivalent to 150 °F in an incubator. This pressure cooker is to serve only as a container for the heptane-containing test package inside the incubator in order to minimize the danger of explosion. Fill the test container within 1/4 -inch of the top with a measured volume of the 150 °F heptane and cover with clean aluminum foil. Place the test container in the preheated pressure cooker and then put the assembly into a 150 °F incubator. After 2 hours, remove the pressure cooker from the incubator, open the assembly, and immediately composite the heptane of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(x) Heptane ( 120 °F for 30 minutes ), simulating boiling water sterilization of fatty foods only. Preheat redistilled reagent-grade heptane (boiling point 208 °F) carefully in a clean Pyrex flask on a water bath or nonsparking hot plate in a well-ventilated hood to 120 °F. At the same time, preheat a pressure cooker or equivalent to 120 °F in an incubator. This pressure cooker is to serve only as a vented container for the heptane-containing test package inside the incubator in order to minimize the danger of explosion. Fill the test container within 1/4 -inch of the top with a measured volume of the 120 °F heptane and cover with clean aluminum foil. Place the test container in the preheated pressure cooker and then put the assembly into a 120 °F incubator. After 30 minutes, remove the pressure cooker from the incubator, open the assembly, and immediately composite the heptane of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xi) Heptane ( 120 °F for 15 minutes ), simulating hot fill or pasteurization above 150 °F for fatty foods only. Preheat redistilled reagent-grade heptane (boiling point 208 °F) carefully in a clean Pyrex flask on a water bath or nonsparking hot plate in a well-ventilated hood to 120 °F. At the same time, preheat a pressure cooker or equivalent to 120 °F in an incubator. This pressure cooker is to serve only as a container for the heptane-containing test package inside the incubator in order to minimize the danger of explosion. Fill the test container within 1/4 -inch of the top with a measured volume of the 120 °F heptane and cover with clean aluminum foil. Place the test container in the preheated pressure cooker and then put the assembly into a 120 °F incubator. After 15 minutes, remove the pressure cooker from the incubator, open the assembly, and immediately composite the heptane of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xii) Heptane ( 100 °F for 30 minutes ), simulating hot fill or pasteurization below 150 °F for fatty foods only. Preheat redistilled reagent-grade heptane (boiling point 208 °F) carefully in a clean Pyrex flask on a water bath or nonsparking hot plate in a well-ventilated hood to 100 °F. At the same time, preheat a pressure cooker or equivalent to 100 °F in an incubator. This pressure cooker is to serve only as a container for the heptane-containing test package inside the incubator in order to minimize the danger of explosion. Fill the test container within 1/4 -inch of the top with a measured volume of the 100 °F heptane and cover with clean aluminum foil. Place the test container in the preheated pressure cooker and then put the assembly into a 100 °F incubator. After 30 minutes, remove the pressure cooker from the incubator, open the assembly and immediately composite the heptane of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xiii) Heptane ( 70 °F for 30 minutes ), simulating room temperature filling and storage of fatty foods only. Fill the test container within 1/4 -inch of the top with a measured volume of the 70 °F heptane and cover with clean aluminum foil. Place the test container in a suitable room maintained at 70 °F. After 30 minutes, composite the heptane of each replicate in a clean Pyrex flask or beaker. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xiv) Heptane ( 120 °F for 30 minutes ), simulating frozen fatty foods reheated in the container. Preheat redistilled reagent-grade heptane (boiling point 208 °F) carefully in a clean Pyrex flask on a water bath or hot plate in a well-ventilated hood to 120 °F. At the same time, preheat a pressure cooker to 120 °F in an incubator. This pressure cooker is to serve only as a container for the heptane-containing test package inside the incubator in order to minimize the danger of explosion. Fill the test container within 1/4 -inch of the top with a measured volume of the 120 °F heptane and cover with clean aluminum foil. Place the test container in the preheated pressure cooker and then put the assembly into a 120 °F incubator. After 30 minutes, remove the pressure cooker from the incubator, open the assembly and immediately composite the heptane from each replicate into a clean Pyrex flask. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xv) Alcohol—8 percent ( 150 °F for 2 hours ), simulating alcoholic beverages hot filled or pasteurized below 150 °F. Preheat 8 percent (by volume) ethyl alcohol in demineralized distilled water to 150 °F in a clean Pyrex flask. Fill the test container with within 1/4 -inch of the top with a measured volume of the 8 percent alcohol. Cover the container with clean aluminum foil and place in an oven maintained at 150 °F. After 2 hours, remove the container from the oven and immediately composite the alcohol from each replicate in a clean Pyrex flask. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xvi) Alcohol—8 percent ( 120 °F for 24 hours ), simulating alcoholic beverages room-temperature filled and stored. Preheat 8 percent (by volume) ethyl alcohol in demineralized distilled water to 120 °F in a clean Pyrex flask. Fill the test container within 1/4 -inch of the top with a measured volume of the 8 percent alcohol, cover the container with clean aluminum foil and place in an oven or incubator maintained at 120 °F. After 24 hours, remove the container from the oven or incubator and immediately composite the alcohol from each replicate into a clean Pyrex flask. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
(xvii) Alcohol—8 percent ( 70 °F for 48 hours ), simulating alcoholic beverages in refrigerated storage. Bring 8 percent (by volume) ethyl alcohol in demineralized distilled water to 70 °F in a clean Pyrex flask. Fill the test container within 1/4 -inch of the top with a measured volume of the 8 percent alcohol. Cover the container with clean aluminum foil. Place the test container in a suitable room maintained at 70 °F. After 48 hours, immediately composite the alcohol from each replicate into a clean Pyrex flask. Proceed with the determination of the amount of extractives by the method described in paragraph (e)(5) of this section.
The tests specified in paragraph (e)(4)(i) through (xvii) of this section are applicable to flexible packages consisting of coated metal contacting food, in which case the closure end is double-folded and clamped with metal spring clips by which the package can be suspended.
(5) Determination of amount of extractives —(i) Total residues. Evaporate the food-simulating solvents from paragraph (e)(4)(i) to (xvii), inclusive, of this section to about 100 milliliters in the Pyrex flask and transfer to a clean, tared platinum dish, washing the flask three times with the solvent used in the extraction procedure, and evaporate to a few milliliters on a nonsparking low-temperature hotplate. The last few milliliters should be evaporated in an oven maintained at a temperature of 212 °F. Cool the platinum dish in a desiccator for 30 minutes and weigh the residue to the nearest 0.1 milligram ( e ). Calculate the extractives in milligrams per square inch and in parts per million for the particular size of container being tested and for the specific food-simulating solvent used.
( a ) Water and 8-percent alcohol.
( b ) Heptane.
(ii) Chloroform-soluble extractives residue. Add 50 milliliters of chloroform (freshly distilled reagent grade or a grade having an established consistently low blank) to the dried and weighed residue, ( e ), in the platinum dish, obtained in paragraph (e)(5)(i) of this section. Warm carefully, and filter through Whatman No. 41 filter paper in a Pyrex funnel, collecting the filtrate in a clean, tared platinum dish. Repeat the chloroform extraction, washing the filter paper with this second portion of chloroform. Add this filtrate to the original filtrate and evaporate the total down to a few milliliters on a low-temperature hotplate. The last few milliliters should be evaporated in an oven maintained at 212 °F. Cool the platinum dish in a desiccator for 30 minutes and weigh to the nearest 0.1 milligram to get the chloroform-soluble extractives residue ( e ′). This e ′ is substituted for e in the equations in paragraph (e)(5)(i)( a ) and ( b ) of this section. If the concentration of extractives ( Ex ) still exceeds 50 parts per million or the extractives in milligrams per square inch exceed the limitations prescribed in paragraph (c) of this section for the particular container size, proceed as follows to correct for zinc extractives (“C” enamels only): Ash the residue in the platinum dish by heating gently over a Meeker-type burner to destroy organic matter and hold at red heat for about 1 minute. Cool in the air for 3 minutes, and place the platinum dish in the desiccator for 30 minutes and weigh to the nearest 0.1 milligram. Analyze this ash for zinc by standard Association of Official Agricultural Chemists methods or equivalent. Calculate the zinc in the ash as zinc oleate, and subtract from the weight of chloroform-soluble extractives residue ( e ′) to obtain the zinc-corrected chloroform-soluble extractives residue ( ee ′). This ee ′ is substituted for e in the formulas in paragraph (e)(5)(i)( a ) and ( b ) of this section. To comply with the limitations in paragraph (c) of this section, the chloroform-soluble extractives residue (but after correction for the zinc extractives in case of “C” enamels) must not exceed 50 parts per million and must not exceed in milligrams per square inch the limitations for the particular article as prescribed in paragraph (c) of this section.
(f) Equipment and reagent requirements —(1) Equipment.
Rinsing equipment, soda fountain pressure-type hot water, consisting in simplest form of a 1/8 -inch- 1/4 -inch inside diameter metal tube attached to a hot water line delivering 190 °F-200 °F water and bent so as to direct a stream of water upward.
Pressure cooker, 21-quart capacity with pressure gage, safety release, and removable rack, 12.5 inches inside diameter × 11 inches inside height, 20 pounds per square inch safe operating pressure.
Oven, mechanical convection, range to include 120 °F-212 °F explosion-proof, inside dimensions (minimum), 19″ × 19″ × 19″, constant temperature to ±2 °F (water bath may be substituted).
Incubator, inside dimensions (minimum) 19″ × 19″ × 19″ for use at 100 °F±2 °F explosion proof (water bath may be substituted).
Constant-temperature room or chamber 70 °F±2 °F minimum inside dimensions 19″ × 19″ × 19″.
Hot plate, nonsparking (explosion proof), top 12″ × 20″, 2,500 watts, with temperature control.
Platinum dish, 100-milliliter capacity minimum.
All glass, Pyrex or equivalent.
(2) Reagents.
Water, all water used in extraction procedure should be freshly demineralized (deionized) distilled water.
Heptane, reagent grade, freshly redistilled before use, using only material boiling at 208 °F.
Alcohol, 8 percent (by volume), prepared from undenatured 95 percent ethyl alcohol diluted with demineralized or distilled water.
Chloroform, reagent grade, freshly redistilled before use, or a grade having an established, consistently low blank.
Filter paper, Whatman No. 41 or equivalent.
(g) In accordance with good manufacturing practice, finished coatings intended for repeated food-contact use shall be thoroughly cleansed prior to their first use in contact with food.
(h) Acrylonitrile copolymers identified in this section shall comply with the provisions of § 180.22 of this chapter.
(i) Epoxy resins derived by the reaction of 4,4′-isopropylidenediphenol and epichlorohydrin, as described in paragraph (b)(3)(viii)( a ) of this section, may be used in accordance with this section except as coatings in packaging for powdered and liquid infant formula.
§ 175.320   Resinous and polymeric coatings for polyolefin films.
Resinous and polymeric coatings may be safely used as the food-contact surface of articles intended for use in producing, manufacturing, packing, processing, preparing, treating, packaging, transporting, or holding food, in accordance with the following prescribed conditions:
(a) The coating is applied as a continuous film over one or both sides of a base film produced from one or more of the basic olefin polymers complying with § 177.1520 of this chapter. The base polyolefin film may contain optional adjuvant substances permitted for use in polyolefin film by applicable regulations in parts 170 through 189 of this chapter.
(b) The coatings are formulated from optional substances which are:
(1) Substances generally recognized as safe for use in or on food.
(2) Substances the use of which is permitted under applicable regulations in parts 170 through 189 of this chapter, by prior sanctions, or approvals.
(3) Substances identified in this paragraph (b)(3) and subject to such limitations as are provided:
(c) The coating in the finished form in which it is to contact food, when extracted with the solvent or solvents characterizing the type of food, and under 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, shall yield net chloroform-soluble extractives not to exceed 0.5 milligram per square inch of coated surface.
(d) Acrylonitrile copolymers identified in this section shall comply with the provisions of § 180.22 of this chapter.
§ 175.350   Vinyl acetate/crotonic acid copolymer.
A copolymer of vinyl acetate and crotonic acid may be safely used as a coating or as a component of a coating which is the food-contact surface of polyolefin films intended for packaging food, subject to the provisions of this section.
(a) The copolymer may contain added optional substances to impart desired properties.
(b) The quantity of any optional substance does not exceed the amount reasonably required to accomplish the intended physical or technical effect nor any limitations further provided.
(c) 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 specifications in such regulation.
(d) Optional substances as provided in paragraph (a) of this section include:
(1) Substances generally recognized as safe in food.
(2) Substances subject to prior sanction or approval for uses with a copolymer of vinyl acetate and crotonic acid and used in accordance with such sanction or approval.
(3) Substances identified in this subparagraph and subject to such limitations as are provided:
(e) Copolymer of vinyl acetate and crotonic acid used as a coating or as a component of a coating conforming with the specifications of paragraph (e)(1) of this section are used as provided in paragraph (e)(2) of this section.
(1) Specifications. (i) The chloroform-soluble portion of the water extractives of the coated film obtained with distilled water at 120 °F for 24 hours does not exceed 0.5 milligram per square inch of coated surface.
(ii) The chloroform-soluble portion of the n- heptane extractives of the coated film obtained with n- heptane at 70 °F for 30 minutes does not exceed 0.5 milligram per square inch of coated surface.
(2) Conditions of use. The copolymer of vinyl acetate and crotonic acid is used as a coating or as a component of a coating for polyolefin films for packaging bakery products and confectionery.
§ 175.360   Vinylidene chloride copolymer coatings for nylon film.
Vinylidene chloride copolymer coatings identified in this section and applied on nylon film may be safely used as food-contact surfaces, in accordance with the following prescribed conditions:
(a) The coating is applied as a continuous film over one or both sides of a base film produced from nylon resins complying with § 177.1500 of this chapter.
(b) The coatings are prepared from vinylidene chloride copolymers produced by copolymerizing vinylidene chloride with one or more of the monomers acrylic acid, acrylonitrile, ethyl acrylate, methacrylic acid, methyl acrylate, methyl methacrylate (CAS Reg. No. 80-62-6; maximum use level 6 weight percent) and 2-sulfoethyl methacrylate (CAS Reg. No. 10595-80-9; maximum use level 1 weight percent). The finished copolymers contain at least 50 weight percent of polymer units derived from vinylidene chloride. The finished coating produced from vinylidene chloride copolymers produced by copolymerizing vinylidene chloride with methyl methacrylate and/or 2-sulfoethyl methacrylate, or with methyl methacrylate and/or 2-sulfoethyl methacrylate together with one or more of the other monomers from this section, is restricted to use at or below room temperature.
(c) Optional adjuvant substances employed in the production of the coatings or added thereto to impart desired properties may include sodium dodecylbenzenesulfonate.
(d) The coating in the finished form in which it is to contact food, when extracted with the solvent or solvents characterizing the type of food, and under 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, shall yield net chloroform-soluble extractives not to exceed 0.5 milligram per square inch of coated surface when tested by the methods described in § 176.170(d) of this chapter.
(e) Acrylonitrile copolymers identified in this section shall comply with the provisions of § 180.22 of this chapter.
§ 175.365   Vinylidene chloride copolymer coatings for polycarbonate film.
Vinylidene chloride copolymer coatings identified in this section and applied on polycarbonate film may be safely used as food-contact surfaces, in accordance with the following prescribed conditions:
(a) The coating is applied as a continuous film over one or both sides of a base film produced from polycarbonate resins complying with § 177.1580 of this chapter.
(b) The coatings are prepared from vinylidene chloride copolymers produced by copolymerizing vinylidene chloride with acrylonitrile, methyl acrylate, and acrylic acid. The finished copolymers contain at least 50 weight-percent of polymer units derived from vinyldene chloride.
(c) Optional adjuvant substances employed in the production of the coatings or added thereto to impart desired properties may include sodium dodecylbenzenesulfonate in addition to substances described in § 174.5(d) of this chapter.
(d) The coating in the finished form in which it is to contact food, 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, shall yield net chloroform-soluble extractives in each extracting solvent not to exceed 0.5 milligram per square inch of coated surface as determined by the methods described in § 176.170(d) of this chapter. In testing the finished food-contact articles, a separate test sample is to be used for each required extracting solvent.
(e) Acrylonitrile copolymers identified in this section shall comply with the provisons of § 180.22 of this chapter.
§ 175.380   Xylene-formaldehyde resins condensed with 4,4′-isopropylidenediphenol-epichlorohydrin epoxy resins.
The resins identified in paragraph (a) of this section may be safely used as a food-contact coating for articles intended for use in contact with food, in accordance with the following prescribed conditions.
(a) The resins are produced by the condensation of xylene-formaldehyde resin and 4,4′-isopropylidenediphenol-epichlorohydrin epoxy resins, to which may have been added certain optional adjuvant substances required in the production of the resins or added to impart desired physical and technical properties. The optional adjuvant substances may include resins produced by the condensation of allyl ether of mono-, di-, or trimethylol phenol and capryl alcohol and also may include substances identified in § 175.300(b)(3), with the exception of paragraph (b)(3)(xxxi) and (xxxii) of that section.
(b) The resins identified in paragraph (a) of this section may be used as a food-contact coating for articles intended for contact at temperatures not to exceed 160 °F with food of Types I, II, VI-A and B, and VIII described in table 1 of § 176.170(c) of this chapter provided that the coating in the finished form in which it is to contact food meets the following extractives limitations when tested by the methods provided in § 175.300(e):
(1) The coating when extracted with distilled water at 180 °F for 24 hours yields total extractives not to exceed 0.05 milligram per square inch of food-contact surface.
(2) The coating when extracted with 8 percent (by volume) ethyl alcohol in distilled water at 160 °F for 4 hours yields total extractives not to exceed 0.05 milligram per square inch of food-contact surface.
(c) The resins identified in paragraph (a) of this section may be used as a food-contact coating for articles intended for contact at temperatures not to exceed room temperature with food of Type VI-C described in table 1 of § 176.170(c) of this chapter provided the coating in the finished form in which it is to contact food meets the following extractives limitations when tested by the methods provided in § 175.300(e):
(1) The coating when extracted with distilled water at 180 °F for 24 hours yields total extractives not to exceed 0.05 milligram per square inch of food-contact surface.
(2) The coating when extracted with 50 percent (by volume) ethyl alcohol in distilled water at 180 °F for 24 hours yields total extractives not to exceed 0.05 milligram per square inch.
§ 175.390   Zinc-silicon dioxide matrix coatings.
Zinc-silicon dioxide matrix coatings may be safely used as the food-contact surface 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 coating is applied to a metal surface, cured, and washed with water to remove soluble substances.
(b) The coatings are formulated from optional substances which include:
(1) Substances generally recognized as safe.
(2) Substances for which safe conditions of use have been prescribed in § 175.300.
(3) Substances identified in paragraph (c) of this section, subject to the limitations prescribed.
(c) The optional substances permitted are as follows:
(d) The coating in the finished form in which it is to contact food, when extracted with the solvent or solvents characterizing the type of food, and under the conditions of its intended use as shown in table 1 and 2 of § 175.300(d) (using 20 percent alcohol as the solvent when the type of food contains approximately 20 percent alcohol) shall yield total extractives not to exceed those prescribed in § 175.300(c)(3); lithium extractives not to exceed 0.025 milligram per square inch of surface; and chromium extractives not to exceed 0.05 microgram per square inch of surface.
(e) The coatings are used as food-contact surfaces for bulk reusable containers intended for storing, handling, and transporting food.