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

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).

(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.

§ 21.105 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.

§ 21.106 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.

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.

§ 21.98 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.

§ 21.99 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.

§ 21.100 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° Bé. 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.

§ 21.101 Caustic soda, liquid.

(a) The liquid caustic soda may consist of either 50 percent or 73 percent by weight sodium hydroxide in aque ous 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.

One ml of 0.25 N hydrochloric acid equals 0.01 gram of sodium hydroxide (anhydrous).

(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.

(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.

§ 21.106 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.

(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).

§ 21.107 Ethyl ether.

(a) Odor. Characteristic odor.

(b) Specific gravity at 15.56°/15.56° C. Not more than 0.728.

§ 21.110 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 As2O,) 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.

§ 21.111 Heptane.

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

(b) Odor. Characteristic odor.

§ 21.112 Isopropyl alcohol.

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

(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.

§ 21.114 Kerosene (deodorized).

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

(b) Flash point. 155° F. minimum.

§ 21.115 Methyl alcohol.

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

§ 21.116 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.

(e) Specific gravity at 20°/20° C. 0.799 to 0.804.

§ 21.117 Methyl n-butyl ketone.

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

(d) Refractive index at 20° C. 1.396 to 1.404.

(e) Specific gravity at 20°/20° C. 0.800 to 0.835.

(f) Distillation range. No distillate should come over below 123° C. and none above 129° C.

§ 21.118 Nicotine solution.

(a) Composition. Five gallons of an aqueous solution containing 40 percent nicotine; 3.6 avoirdupois ounces

of methylene blue, U.S.P.; water sufficient to make 100 gallons.

(b) Color. One ml of the nicotine solution (previously agitated in the presence of air) is measured into 100 ml of water and thoroughly mixed. Fifty ml of this colored solution is compared, using Nessler tubes, with 50 ml of a standard color solution containing 5 grams of CuSO,.5H2O, C.P. in 100 ml of water. The color intensity of the solution tested should be equal to or greater than that of the standard solution.

(c) Nicotine content. The above solution must contain not less than 1.88 percent of nicotine determined by the following process: 20 ml of the solution are measured into a 500 ml Kjeldahl flask provided with a suitable bulb tube, 50 ml of 0.1 N NaOH added and the mixture distilled in a current of steam until the distillate is no longer alkaline (about 500 ml). The distillate is then titrated with 0.1 N H,SO, using rosolic acid or methyl red as indicator. Not less than 23.2 ml should be required for neutralization.

§ 21.119 Nitropropane, mixed isomers of. (a) Nitropropane content. A minimum of 94 percent by weight. (b) Total nitroparaffin content. A minimum of 99 percent by weight.

§ 21.120 Phenyl mercuric benzoate.

(a) Assay (as phenyl mercuric benzoate). Not less than 99.0 percent by weight.

(b) Melting point. Not less than 94° C.

§ 21.121 Pyridine bases.

(a) Alkalinity. One ml of pyridine bases dissolved in 10 ml of water is titrated with 1 N H2SO, until a drop of the mixture placed upon Congo paper shows a distinct blue border, which soon disappears. A minimum of 9.5 ml of the acid must be required for the end point. (Congo paper: filter paper treated with 0.1 percent aqueous solution of Congo red and dried.)

(b) Distillation range. One hundred ml of the denaturant are distilled in the following manner: The sample is

placed in a short-necked glass flask of about 200 ml capacity which is rested on an asbestos plate having a circular opening of 30 mm in diameter. The neck of this flask is fitted with a fractionating tube 12 mm in diameter and 170 mm long and having a bulb just 1 cm below the side tube which is connected with a Liebig condenser having a water jacket not less than 400 mm in length. A standardized thermometer is placed in the fractionating tube so that the mercury bulb is suspended in the center of the fractionating bulb. Heat is applied slowly and in such manner that 5 ml of distillate is collected per minute in a graduated cylinder. At least 50 ml must distill at or below 140° C. and at least 90 ml below 160° C.

(1) Ten ml of this solution are treated with 5 ml of 5 percent aqueous solution of anhydrous fused CaCl, and the mixture vigorously shaken. An abundant crystalline separation should occur within 10 minutes.

(2) Ten ml of the pyridine solution mixed with 50 ml of Nessler's reagent must give a white precipitate.

(d) Water content. Twenty ml of pyridine bases are shaken with 20 ml of a caustic soda solution having a specific gravity of 1.40 (15.56°/15.56° C.) and the mixture allowed to stand until completely separated into two layers. The amount of pyridine base layer should be 18.5 ml, minimum.

§ 21.122 Pyronate.

Pyronate is a product of the destructive distillation of hardwood meeting the following requirements:

(a) Acidity (as acetic acid). Not more than 0.1 percent by weight, determined as follows:

Add 5.0 ml sample to 100 ml distilled water in an Erlenmeyer flask and titrate with 0.1 N NaOH to a bromthymol blue endpoint.

(b) Color. The color shall be no darker than the color produced by 2.0 grams of potassium dichromate in 1 liter of water. The comparision shall be made in 4-ounce oil sample bottles viewed crosswise.

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