[Code of Federal Regulations]
[Title 21, Volume 3]
[Revised as of January 1, 2007]
From the U.S. Government Printing Office via GPO Access
[CITE: 21CFR178.3910]
[Page 445-450]
TITLE 21--FOOD AND DRUGS
CHAPTER I--FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN
SERVICES (CONTINUED)
PART 178 INDIRECT FOOD ADDITIVES: ADJUVANTS, PRODUCTION AIDS, AND
Subpart D Certain Adjuvants and Production Aids
Sec. 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.
------------------------------------------------------------------------
List of substances Limitations
------------------------------------------------------------------------
[alpha]-Butyl-[Omega]--hydroxypoly
(oxyethylene)-poly (oxypropylene) (CAS
Reg. No. 9038-95-3) produced by random
condensation of a 1:1 mixture by
weight of ethylene oxide and propylene
oxide with butanol and having a
minimum molecular weight of 1,000.
[alpha]-Butyl-[Omega]-hydroxypoly(oxypr
opylene) (CAS Reg. No. 9003.13-8)
having a minimum molecular weight of
1000.
[alpha]-Lauroyl-[Omega]-hydroxpoly(oxye
thylene) (CAS Reg. No. 9004-81-3)
having a minimum molecular weight of
200.
Acetate esters derived from synthetic
straight chain alcohols (complying
with Sec. 172.864 of this chapter)
that have even numbers of carbon atoms
in the range C8-C18.
alpha-Alkyl-omega-
hydroxypoly(oxyethylene) produced by
the condensation of 1 mole of C12-C15
straight chain primary alcohols with
an average of 3 moles of ethylene
oxide (CAS Reg. No. 68002-97.1).
Benzotriazole (CAS Reg. No. 95.14-7)...
Bis(hydrogenated tallow alkyl)amine Not to be used in combination
(CAS Reg. No. 61789-79-5). with sodium nitrite.
Bis(hydrogenated tallow
alkyl)aminoethanol (CAS Reg. No.
116438-56-3).
N,N-Bis(2-hydroxyethyl)butylamine (CAS
Reg. No. 102-79-4).
Tert-Butyl alcohol.....................
Di(2-ethylhexyl)phthalate..............
Diethyl phthalate......................
Diethylene glycol monobutylether (CAS
Reg. No. 112-34-5).
Dimers, trimers, and/or their partial For use only at a level not to
methyl esters; such dimers and trimers exceed 10 percent by weight of
are of unsaturated C18 fatty acids finished lubricant
derived from animal and vegetable fats formulation.
and oils and/or tall oil, and such
partial methyl esters meet the
following specifications:
Saponification value 180-200, acid
value 70.130, and maximum iodine value
120.
Di-n-octyl sebacate....................
Ethylenediaminetetraacetic acid, sodium
salts.
Isopropyl alcohol......................
Isopropyl laurate (CAS Reg. No. 10233- For use at a level not to
13-3). exceed 10 percent by weight of
the finished lubricant
formulation.
Isopropyl oleate.......................
Isotridecyl alcohol, ethoxylated (CAS
Reg. No. 9043-30-5).
Methyl esters of coconut oil fatty
acids.
Methyl esters of fatty acids (C16-C18)
derived from animal and vegetable fats
and oils.
Polybutene, hydrogenated: complying
with the identity prescribed under
Sec. 178.3740(b).
Polyethylene glycol (400) monostearate.
Polyisobutylene (minimum molecular
weight 300).
[[Page 446]]
Polyoxyethylated (5 moles) tallow amine
(CAS Reg. No. 61791-26-2).
Polyvinyl alcohol......................
Sodium nitrite......................... For use only as a rust
inhibitor in lubricant
formulations provided the
total residual sodium nitrite
on the metallic article in the
form in which it contacts food
does not exceed 0.007
milligram per square inch of
metallic food-contact surface.
Sodium petroleum sulfonate, MW 440-450
(CAS Reg. No. 68608-26-4) derived from
naphthenic oil having a Saybolt
viscosity range of 500-600 Saybolt
Universal Seconds (SUS at 37-8 [deg]C
(100 [deg]F) as determined by ASTM
method D88-81, ``Standard Test Method
for Saybolt Viscosity,'' which is
incorporated by reference. Copies are
available from the American Society
for Testing Materials, 1961 Race St.,
Philadelphia, PA 19103, 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..
Synthetic alcohol mixture of straight-
and branched-chain alcohols that have
even numbers of carbon atoms in the
range C4C18 and that are prepared from
ethylene, aluminum, and hydrogen such
that the finished synthetic alcohol
mixture contains not less than 75 pct
of straight-chain primary alcohols and
contains not less than 85 pct total
C10 and C12 alcohols.
Synthetic primary alcohol mixture of For use at a level not to
straight- and branched-chain alcohols exceed 8 pct by weight of the
that contain at least 99 pct primary finished lubricant
alcohols consisting of the following: formulation.
not less than 70 pct normal alcohols;
not less than 96.5 pct C12-C15
alcohols; and not more than 2.5 pct
alpha, omega C13-C16 diols. The
alcohols are prepared from linear
olefins from a purified kerosene
fraction, carbon monoxide and hydrogen
using a modified oxo process, such
that the finished primary alcohol
mixture meets the following
specifications: Molecular weight,
2074; hydroxyl number, 266-
276.
Synthetic primary alcohol mixture of For use only at a level not to
straight- and branched-chain alcohols exceed 8 pct by weight of the
that contain at least 99 pct primary finished lubricant
alcohols consisting of the following: formulation.
not less than 70 percent normal
alcohols; not less than 93 pct C12-C13
alcohols; not more than 5 pct C14-C15
alcohols; and not more than 2.5 pct
alpha, omega, C13-C16 diols. The
alcohols are prepared from linear
olefins from a purified kerosene
fraction, carbon monoxide and hydrogen
using a modified oxo process, such
that the finished primary alcohol
mixture meets the following
specifications:
Molecular weight 1945; hydroxyl number, 283-296.
Tallow, sulfonated.....................
Triethanolamine........................
------------------------------------------------------------------------
(3) Mineral oil conforming to the identity prescribed in Sec.
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 [deg]C minimum and final boiling
point is 288 [deg]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
[[Page 447]]
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 [deg]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 [deg]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 Sec.
178.3620(c) as determined by the analytical method described therein.
(ii) Ultraviolet absorbance limits on residual lubricants are as
follows:
------------------------------------------------------------------------
Maximum
absorbance
per 5
Wavelength (m[micro]) centimeters
optical
pathlength
------------------------------------------------------------------------
280-289.................................................... 0.7
290-299.................................................... .6
300-359.................................................... .4
360-400.................................................... .09
------------------------------------------------------------------------
(iii) The analytical method for determining ultraviolet absorbance
limits on residual lubricants is as follows:
general instructions
Because of the sensitivity of the test, the possibility of errors
arising from contamination is great. It is of the greatest importance
that all glassware be scrupulously cleaned to remove all organic matter
such as oil, grease, detergent, residues, etc. Examine all glassware
including stoppers and stopcocks, under ultraviolet light to detect any
residual fluorescent contamination. As a precautionary measure it is
recommended practice to rinse all glassware with purified isooctane
immediately before use. No grease is to be used on stopcocks or joints.
Great care to avoid contamination of oil samples in handling and to
assure absence of any extraneous material arising from inadequate
packaging is essential. Because some of the polynuclear hydrocarbons
sought in this test are very susceptible to photo-oxidation, the entire
procedure is to be carried out under subdued light.
apparatus
Separatory funnels. 250-milliliter, 500-milliliter, 1,000-
milliliter, and preferably 2,000-milliliter capacity, equipped with
tetrafluoroethylene polymer stopcocks.
Evaporation flask (optional). 250-milliliter or 500-milliliter
capacity all-glass flask equipped with standard-taper stopper having
inlet and outlet tubes to permit passage of nitrogen across the surface
of contained liquid to be evaporated.
Spectrophotometric cells. Fused quartz cells, optical path length in
the range of 5,000 centimeters 0.005 centimeter;
also for checking spectrophotometer performance only, optical path
length in the range 1.000 centimeter 0.005
centimeter. With distilled water in the cells, determine any absorbance
differences.
Spectrophotometer. Special range 250 millicrons-400 millimicrons
with spectral slit width of 2 millimicrons or less; under instrument
operating conditions for these absorbance measurements, the
spectrophotometer shall also meet the following performance
requirements:
Absorbance repeatability, 0.01 at 0.4
absorbance.
Absorbance accuracy, \1\ 0.05 at 0.4
absorbance.
---------------------------------------------------------------------------
\1\ As determined by procedure using potassium chromate for
reference standard and described in National Bureau of Standards
Circular 484, Spectrometry, U.S. Department of Commerce (1949), which is
incorporated by reference. Copies are available from the Center for Food
Safety and Applied Nutrition (HFS-200), Food and Drug Administration,
5100 Paint Branch Pkwy., 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.
[[Page 448]]
Soxhlet apparatus. 60-millimeter diameter body tubes fitted with
condenser and 500-milliliter round-bottom boiling flask. A supply of
paper thimbles to fit is required.
Nitrogen cylinder. Water-pumped or equivalent purity nitrogen in
cylinder equipped with regulator and valve to control flow at 5 p.s.i.g.
reagents and materials
Organic solvents. All solvents used throughout the procedure shall
meet the specifications and tests described in this specification. The
isooctane (2,2,4-trimethylpentane) shall pass the following test:
Place 180 milliliters of solvent in a 250-milliliter Erlenmeyer
flask, add 1 milliliter of purified n-hexadecane and evaporate on the
steam bath under a stream of nitrogen (a loose aluminum foil jacket
around the flask will speed evaporation). Discontinue evaporation when
not over 1 milliliter of residue remains.
Alternatively, the evaporation time can be reduced by using the
optional evaporation flask. In this case the solvent and n-hexadecane
are placed in the flask on the steam bath, the tube assembly is
inserted, and a stream of nitrogen is fed through the inlet tube while
the outlet tube is connected to a solvent trap and vacuum line in such a
way as to prevent any flow-back of condensate into the flask.
Dissolve the 1 milliliter of hexadecane residue in isooctane and
make to 25 milliliters volume. Determine the absorbance in the 5-
centimeter path length cells compared to isooctane as reference. The
absorbance of the solution of the solvent residue shall not exceed 0.01
per centimeter path length between 280 and 400 m[micro]. 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 m[micro]-400 m[micro]. 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).
------------------------------------------------------------------------
Absorbance
Wavelength (maximum)
------------------------------------------------------------------------
261.5....................................................... 1.00
270......................................................... .20
275......................................................... .09
280......................................................... .06
300......................................................... .015
------------------------------------------------------------------------
There shall be no irregularities in the absorbance curve within
these wavelengths.
Phosphoric acid. 85 percent A.C.S. reagent grade.
Sodium sulfate, anhydrous, A.C.S. reagent grade, preferably in
granular form. For each bottle of sodium sulfate reagent used, establish
as follows the necessary sodium sulfate prewash to provide such filters
required in the method: Place approximately 35 grams of anhydrous sodium
sulfate in a 30-milliliter coarse, fritted-glass funnel or in a 65-
milliliter filter funnel with glass wool plug; wash with successive 15-
milliliter portions of the indicated solvent until a 15-milliliter
portion of the wash shows 0.00 absorbance per centimeter path length
between 280 m[micro] and 400 m[micro] 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 m[micro] to 400
m[micro].
Place 300 milliliters of dimethyl sulfoxide in a 1-liter separatory
funnel and add 75 milliliters of phosphoric acid. Mix the contents of
the funnel and allow to stand for 10 minutes. (The reaction between the
sulfoxide and the acid is exothermic. Release pressure after mixing,
then keep funnel stoppered.) Add 150 milliliters of isooctane and shake
to pre-equilibrate the solvents. Draw off the individual layers and
store in glass-stoppered flasks.
procedure
Sample. Select metal foil or sheet stock for the test which has not
been previously contaminated by careless handling or exposure to
atmospheric dust and fumes. A commercial coil in the form supplied for
spindle mounting in a packaging line or wrapping machine is most
suitable. Strip off the outside turn of metal and discard. Carefully
avoid contamination or damage from handling the metal (wear gloves).
Remove a 16.18-foot length from the coil and place it on a flat surface
protected by a length of new kraft paper. Cut four 15-foot strips from
the sample, each 3 inches wide (avoid tearing the edges of the strips).
Using a piece of suitable glass rod, roll the strips of metal into loose
coils and insert each into a Soxhlet thimble. Each turn of coil should
be visibly separated from the adjacent turn.
[[Page 449]]
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 280m[micro]-400m[micro] (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.
------------------------------------------------------------------------
List of substances Limitations
------------------------------------------------------------------------
Acetyl tributyl citrate................
Acetyl triethyl citrate................
Butyl stearate.........................
Castor oil.............................
Dibutyl sebacate.......................
Di(2-ethylhexyl) azelate...............
Di(2-ethylhexyl) sebacate..............
Diisodecyl phthalate...................
Dimethylpolysiloxane................... Conforming to the identity
prescribed in Sec. 181.28 of
this chapter.
Dipropylene glycol.....................
Epoxidized soybean oil................. Conforming to the identity
prescribed in Sec. 181.27 of
this chapter.
[[Page 450]]
Fatty acids derived from animal and
vegetable fats and oils, and salts of
such acids, single or mixed, as
follows:
Aluminum
Magnesium
Potassium
Sodium
Zinc
Fatty alcohols, straight-chain with
even number carbon atoms (C10 or
greater).
Isobutyl stearate......................
Lanolin................................
Linoleic acid amide....................
Mineral oil............................ Conforming to the identity
prescribed in Sec. 178.3620
(a) or (b).
Mono-, di-, and tristearyl citrate.....
Oleic acid amide.......................
Palmitic acid amide....................
Petrolatum............................. Conforming to the identity
prescribed in Sec. 178.3700.
Phosphoric acid, mono- and dihexyl For use only at levels not to
esters, compounds with exceed 0.5 percent by weight
tetramethylnonylamines and C11 14- of the finished surface
alkylamines (CAS Reg. No. 80939-62-4). lubricant formulation.
Polyethylene glycol (molecular weight Mono- and diethylene glycol
300 or greater). content not to exceed a total
of 0.2 pct.
Stannous stearate......................
Stearic acid amide.....................
Stearyl stearate.......................
Tetrakis[methylene (3,5-di-tert-butyl-4- For use at a level not to
hydroxyhydrocinnamate)] methane (CAS exceed 0.5 percent by weight
Registry No. 6683.19-8). of the finished surface
lubricant formulation.
Triethylene glycol..................... Diethylene glycol content not
to exceed 0.1 pct.
Wax, petroleum......................... Complying with Sec. 178.3710.
------------------------------------------------------------------------
(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 Sec. 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 Sec. 179.45 of this
chapter shall comply with any applicable specifications prescribed by
such regulation.
[42 FR 14609, Mar. 15, 1977, as amended at 48 FR 238, Jan. 4, 1983; 49
FR 10113, Mar. 19, 1984; 49 FR 29579, July 23, 1984; 50 FR 36874, Sept.
10, 1985; 52 FR 10223, Mar. 31, 1987; 54 FR 6124, Feb. 8, 1989; 54 FR
24899, June 12, 1989; 56 FR 55456, Oct. 28, 1991; 57 FR 23953, June 5,
1992; 58 FR 17513, Apr. 5, 1993; 64 FR 47110, Aug. 30, 1999; 69 FR
24512, May 4, 2004]
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