Code of Federal Regulations: Containing a Codification of Documents of ...

812. Product development and pilot plant uses (own use only).

$21.79 Formula No. 44.

(a) Formula. To every 100 gallons of alcohol add:

Ten gallons of n-butyl alcohol

(b) Authorized uses. (1) As a solvent: 430. Sterilizing and preserving solutions. (2) Miscellaneous uses:

812. Product development and pilot plant uses (own use only).

$21.80 Formula No. 45.

(a) Formula. To every 100 gallons of alcohol add:

Three hundred pounds of refined white or orange shellac.

(b) Authorized uses. (1) As a solvent: 015. Candy glazes.

(2) Miscellaneous uses:

812 Product development and pilot plant uses (own use only).

$21.81 Formula No. 46.

(a) Formula. To every 100 gallons of alcohol add:

Twenty-five fluid ounces of phenol, U.S.P., and 4 fluid ounces of methyl salicylate, N.F. (b) Authorized uses. (1) As a solvent: 220. An antiseptic, sterilizing, and bathing solution having restricted use.

(2) Miscellaneous uses:

812. Product development and pilot plant uses (own use only).

(c) Conditions governing use. This formula may be used only by institutions and organizations which are of a semipublic character and engaged in charitable work.

Subpart E-Specifications for Denaturants

$21.91 General.

Denaturants prescribed in this part shall comply with the specifications set forth in this subpart. However, in order to meet requirements of national defense or for other valid reasons, the appropriate ATF officer may, pursuant to written application filed by the

denaturer, authorize variations from such specifications or authorize the use of substitute denaturants if such variation or substitution will not jeopardize the revenue. Each such application shall identify the applicant by name, address, and permit number; state the number of each formula of specially denatured alcohol involved; explain why the use of the substitute denaturant, or the variation from specifications, as the case may be, is necessary; and include, as applicable, either the identity of the approved denaturant for which substitution is desired and the identity of the substitute denaturant (including the name of the manufacturer) or the identity of the prescribed specifications and the proposed variation from those specifications. The application shall be accompanied by an 8-ounce sample of the proposed denaturing material for analysis.

[T.D. ATF-133, 48 FR 24673, June 2, 1983, as amended by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

$21.92 Denaturants listed as U.S.P. or N.F.

Denaturing materials and products listed in this part as "U.S.P." or "N.F." shall meet the specifications set forth in the current United States Pharmacopoeia or National Formulary, or the latest volume of these publications in which the denaturants appeared as official preparations.

$21.93 Acetaldehyde.

(a) Aldehyde content (as acetaldehyde). Not less than 95.0 percent by weight. (b) Color. Colorless. (c) Odor. fruity odor.

Characteristic pungent,

(d) Specific gravity at 15.56 °/15.56 °C. Not less than 0.7800.

$21.94 Acetaldol.

(a) Purity. Not less than 90 percent by weight acetaldol as determined by the following method:

Dissolve 15 grams of the acetaldol in distilled water and dilute to 1 liter in a volumetric flask. Transfer 5 ml of this solution to a 250 ml glass-stoppered flask containing 25 ml distilled water. Add 25 ml of a freshly prepared 1 percent sodium bisulfite solution. Prepare a blank omitting the acetaldol solution. Place the flasks in a dark place away

from excessive heat or cold and allow to stand six hours. Remove flasks and titrate free bisulfite with 0.1 N iodine solution using starch indicator.

Percent acetaldol by weight=(ml_blank-ml test)x200x0.44/weight of sample

Titrations in excess of 100 percent may be obtained if the sample contains appreciable amounts of acetaldehyde.

(b) Specific gravity at 20 °C. 1.098 to 1.105.

$21.95 Alpha terpineol.

(a) Boiling point at 752mm 218.8-219.4 °C.

(b) Density at 15° 0.9386.

$21.96 Ammonia, aqueous.

(a) Alkalinity. Strongly alkaline to litmus.

(b) Ammonia content. 27 to 30 percent by weight. Accurately weigh a glassstoppered flask containing 25 ml of water, add about 2 ml of the sample, stopper, and weigh again. Add methyl red indicator, and titrate with 1 N sulfuric acid. Each ml of 1 N sulfuric acid is equivalent to 17.03 mg of NH3

(d) Non-volatile residue. 2 mg maximum. Dilute a portion of the sample with 11⁄2 times its volume of distilled water. Evaporate 10 ml of this product to dryness in a tared platinum or porcelain dish. Dry residue at 105 °C. for 1 hour, cool and weigh.

(e) Odor. Characteristic (exceedingly pungent).

(f) Specific gravity at 20°/4 °C. 0.8920 to 0.9010.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF 442, 66 FR 12854, Mar. 1, 2001]

(d) Water solubility. When 10 ml of benzene are shaken with an equal volume of water in a glass-stoppered bottle, graduated to 0.1 ml, and allowed to stand 5 minutes to separate, the upper layer of liquid shall measure not less than 9.5 ml.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.98 Bone oil (Dipple's oil).

(a) Color. The color shall be a deep brown.

(b) Distillation range. When 100 ml are distilled in the manner described for pyridine bases, not more than 5.0 ml should distill below 90 °C.

(c) Pyrrol reaction. Prepare a 1.0 percent solution of bone oil in 95 percent alcohol. Prepare a second solution containing 0.025 percent bone oil by diluting 2.50 ml of the first solution to 100 ml with 95 percent alcohol. Dip a splinter of pine, previously moistened with concentrated hydrochloric acid, into 10 ml of the 0.025 percent bone oil solution. After a few minutes the splinter should show a distinct red coloration.

(d) Reaction with mercuric chloride. Add 5 ml of the 1.0 percent bone oil solution above to 5 ml of a 2 percent alcoholic solution of mercuric chloride. A turbidity is formed at once which separates into a flocculent precipitate on standing several minutes. Add 5.0 ml of the 0.025 percent bone oil solution to 5.0 ml of a 2.0 percent alcoholic solution of mercuric chloride. A faint turbidity appears after several minutes.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF 442, 66 FR 12854, Mar. 1, 2001]

$21.99 Brucine alkaloid.

(a) Identification test. Add a few drops of concentrated nitric acid to about 10 mg of brucine alkaloid. A vivid red color is produced. Dilute the red solution with a few drops of water and add a few drops of freshly made dilute stannous chloride solution. A reddish purple (violet) color is produced.

(b) Melting point. 178 °+1 °C. Dry the alkaloid in an oven for one hour at 100 °C., increase the temperature to 110°

and dry to a constant weight before taking melting point.

NOTE. Brucine alkaloid tetrahydrate melts at 105 °C. while the anhydrous form melts at 178 °C.

(c) Strychnine test. Brucine alkaloid shall be free of strychnine when tested by the method listed under Brucine Sulfate, N.F. IX.

NOTE. If the brucine contains as much as 0.05 percent strychnine, a clear distinctive violet color, characteristic of strychnine, will be obtained.

(d) Sulfate test. No white precipitate is formed that is not dissolved by hydrochloric acid when several drops of a 1 N barium chloride solution are added to 10 ml of a solution of the alkaloid.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.100 n-Butyl alcohol.

(a) Acidity (as acetic acid). 0.03 percent by weight maximum.

(b) Color. Colorless.

(d) Odor. Characteristic odor.

(e) Specific gravity at 20 °/20°C. 0.810 to 0.815.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF 442, 66 FR 12854, Mar. 1, 2001]

§ 21.101 tert-Butyl alcohol.

(a) Acidity (as acetic acid). 0.003 percent by weight maximum.

(b) Color. Colorless.

(c) Distillation range. When 100 ml of tertiary butyl alcohol are distilled, none should distill below 78 °C. and none above 85 °C. More than 95 percent should distill between 81 - 83 °C.

(d) Dryness at 20 °C. Miscible without turbidity with 19 volumes of 60° Bél. gasoline.

(e) Freezing point (first needle). Above 20 °C.

(f) Identification test. Place five drops of a solution containing approximately 0.1 percent tertiary butyl alcohol in ethyl alcohol in a test tube. Add 2 ml of Denige's reagent (dissolve 5 grams of red mercuric oxide in 20 ml of concentrated sulfuric acid; add this solution to 80 ml of distilled water, and filter when cool). Heat the mixture just

to the boiling point and remove from the flame. A yellow precipitate forms within a few seconds.

(g) Nonvolatile matter. Less than 0.005 percent by weight.

(h) Odor. Characteristic odor. (i) Residual odor after evaporation. None.

(j) Specific gravity at 25 °/25 °C. 0.780 to 0.786.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.102 Caustic soda, liquid.

(a) The liquid caustic soda may consist of either 50 percent or 73 percent by weight sodium hydroxide in aqueous solution. The amount of caustic soda used shall be such that each 100 gallons of alcohol will contain not less than 8.76 pounds of sodium hyroxide, anhydrous basis.

(b) Color. A 2 percent solution of the sodium hydroxide in water shall be water-white.

Accurately weigh 2 grams of liquid caustic soda into a 100 ml volumetric flask, dissolve, and dilute to the mark with distilled water at room temperature. Transfer a 25 ml aliquot of the solution to a titration flask, add 10 ml of 1 percent barium chloride solution, 0.2 ml of 1 percent phenolphthalein indicator, and 50 ml of distilled water. Titrate with 0.25 N hydrochloric acid to the disappearance of the pink color. Not less than 25 ml of the hydrochloric acid shall be required to neutralize the sample of diluted 50 percent caustic soda, and not less than 36.5 ml of the hydrochloric acid shall be required to neutralize the sample of diluted 73 percent caustic soda.

One ml of 0.25 N hydrochloric acid equals 0.01 gram of sodium hydroxide (anhydrous). [T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF 442, 66 FR 12854, Mar. 1, 2001]

§ 21.104 Cinchonidine.

(a) Melting point. 208° to 210 °C. (b) Color. White powder.

(d) Test. A solution of cinchonidine in dilute sulfuric acid shall not have more than a faint blue fluorescence (to distinguish from quinine and quinoidine). [T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF -442, 66 FR 12854, Mar. 1, 2001]

§ 21.105 Citronella oil, natural.

(a) Java type:

(1) Alcohol content (as Geraniol). Not less than 85 percent by weight.

(2) Aldehyde content (as Citronellal). Not less than 30 percent by weight.

(3) Refractive index at 20 °C. 1.4660 to 1.4745.

(4) Specific gravity at 25 °/25 °C. 0.875 to 0.893.

(5) Odor. Characteristic odor. (b) Ceylon type:

(1) Alcohol content (as Geraniol). Not less than 55 percent by weight.

(2) Aldehyde content (as Citronellal). Not less than 7 percent by weight.

(3) Refractive index at 20 °C. 1.4790 to 1.4850.

(4) Specific gravity at 25 °/25 °C. 0.891 to 0.904.

(5) Odor. Characteristic odor.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF 442, 66 FR 12854, Mar. 1, 2001]

$21.106 Diethyl phthalate.

(a) Refractive index at 25 °C. 1.497 to 1.502.

(b) Color. Colorless.

(d) Solubility. Soluble in 20 parts of 60 percent alcohol.

(e) Specific gravity at 25 °/25 °C. 1.115 to 1.118.

(f) Ester content (as diethyl phthalate). Not less than 99 percent by weight.

NOTE. The sample taken for ester determination should be approximately 0.8 gram. The number of ml of 0.5 N potassium hydroxide used in saponification multiplied by 0.05555 indicates the number of grams of ester in the sample taken for assay.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF 442, 66 FR 12854, Mar. 1, 2001]

$21.107 Ethyl acetate.

(a) 85 percent ester:

(1) Acidity (as acetic acid). Not more than 0.015 percent by weight.

(2) Color. Colorless.

(3) Odor. Characteristic odor.

(4) Ester content. Not less than 85 percent by weight.

(5) Specific gravity at 20°/20°C. Not less than 0.882.

(6) Distillation range. (For applicable ASTM method, see 1980 Annual Book of ASTM Standards, Part 29, page 70, Standard No. D 302-58 (1975); for incorporation by reference, see §21.6(b).) When 100 ml of ethyl acetate are distilled by this method, none shall distill below 70 °C., not more than 10 ml shall distill below 72 °C., and none above 80 °C.

(b) 100 percent ester:

(1) Acidity (as acetic acid). Not more than 0.010 percent by weight.

(2) Color. Colorless.

(3) Odor. Characteristic odor.

(4) Ester content. Not less than 99 percent by weight.

(5) Specific gravity at 20°/20 °C. Not less than 0.899.

(6) Distillation range. (For applicable ASTM method, see 1980 Annual Book of ASTM Standards, Part 29, page 433, Standard No. D 3127-77; for incorporation by reference, see §21.6(b).) When 100 ml of ethyl acetate are distilled by this method, not more than 2 ml shall distill below 75 °C., and none above 80 °C. (760 mm).

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

(b) Odor. Characteristic odor.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.110 Gasoline, unleaded.

Conforms to specifications as established by the American Society for Testing and Materials (ASTM) in the 1980 Annual Book of ASTM Standards, Part 23, page 229, Standard No. D 43979. Any of the "seasonal and geographical" volatility classes for unleaded gasoline are considered suitable as a denaturant. (For incorporation by reference, see § 21.6(b).)

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

821.111 Gentian violet.

(a) Gentian violet (methyl violet, methylrosaniline chloride) occurs as a dark green powder or crystals having metallic luster.

(b) Arsenic content. Not more than 15 ppm. (as As2 O3) as determined by the applicable U.S.P. method.

(c) Identification test. Sprinkle about 1 mg of sample on 1 ml of sulfuric acid; it dissolves in the acid with an orange or brown-red color. When this solution is diluted cautiously with water, the color changes to brown, then to green, and finally to blue.

(d) Insoluble matter. Not to exceed 0.25 percent when tested by the following method:

Transfer 1.0 gram of sample to a 150 ml beaker containing 50 ml of alcohol. Stir to complete solution and filter through a weighed Whatman No. 4 filter paper. Wash residue with small amounts of alcohol totaling about 50 ml. Dry paper in oven for 30 minutes at 80 °C. and weigh. Calculate insoluble material.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.112 Heptane.

(a) Distillation range. No distillate should come over below 200 °F. and none above 211 °F.

(b) Odor. Characteristic odor.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.113 Isopropyl alcohol.

Specific gravity at 15.56 °/15.56 °C. 0.810 maximum.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.114 Kerosene.

(a) Distillation range. (For applicable ASTM method, see 1980 Annual Book of ASTM Standards, Part 25, page 395, Standard No. D 3699-78 for burner fuel; see Part 23, page 849, Standard Nos. D 1655-80a for aviation turbine fuels and D 86-78 for distillation of petroleum products; for incorporation by reference, see §21.6(b).) No distillate should come over below 340 °F. and none above 570 °F.

(b) Flash point. 115 °F. minimum. (c) Odor. Characteristic odor.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.115 Kerosene (deodorized).

(a) Distillation range. No distillate should come over below 340 °F. and none above 570 °F.

(b) Flash point. 155 °F. minimum.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

$21.116 Methyl alcohol.

Specific gravity at 15.56 °/15.56 °C. 0.810 maximum.

[T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]

§ 21.117 Methyl isobutyl ketone.

(a) Acidity (as acetic acid). 0.02 percent by weight, maximum.

(b) Color. Colorless.

(c) Distillation range. (For applicable ASTM method, see 1980 Annual Book of ASTM Standards, Part 29, page 147, Standard No. D 1153-77; for incorporation by reference, see §21.6(b).) No distillate should come over below 111 °C. and none above 117 °C.

(d) Odor. Characteristic odor.

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