: between 1.5440 and 1.5465 at 20

Hydrocyanic acid— Shake 0.5 mL with 5 mL of water, add 0.5 mL of sodium hydroxide TS and 0.1 mL of ferrous sulfate TS, and warm the mixture gently. Add a slight excess of hydrochloric acid: no greenish-blue color or blue precipitate is observed within 15 minutes.

Benzalkonium Chloride —Use Benzalkonium Chloride (NF monograph).

Benzamidine Hydrochloride Hydrate (Benzenecarboximidamide Monohydrochloride, Hydrate),

C7H8N2·HCl·xH2O—156.6

[206752-36-5]—White to off-white powder. Use a suitable grade.

[Note—A suitable grade is available from Sigma-Aldrich, www.sigma-aldrich.com. ]

Benzanilide,

C13H11NO—197.23

[93-98-1]—Off-white, light gray to grayish-green powder. Insoluble in water; sparingly soluble in alcohol; slightly soluble in ether.

: between 162

and 165

Solubility in acetone— A 1.0-g portion dissolves completely in 50 mL of acetone to yield a clear solution.

Benzene,

C6H6—78.11

[71-43-2]—Use ACS reagent grade.

Benzenesulfonamide,

C6H5SO2NH2—157.19

[98-10-2]—White to pale beige crystals.

: between 150

and 153

Benzenesulfonyl Chloride,

C6H5SO2Cl—176.62

[98-09-9]—Colorless, oily liquid. Insoluble in cold water; soluble in alcohol and in ether. Solidifies at 0

: between 14

and 17

Boiling range (Reagent test): between 251

and 252

Benzhydrol (

-Phenylbenzenemethanol),

C13H12O—184.23

[91-01-0]—White to pale yellow crystals. Very slightly soluble in water; soluble in alcohol, in ether, and in chloroform.

: between 65

and 67

, but the range between beginning and end of melting does not exceed 2

Benzoic Acid,

C6H5COOH—122.12

[65-85-0]—Use ACS reagent grade.

[Note—Benzoic Acid of a quality suitable as a primary standard is available from the National Institute of Standards and Technology, Office of Standard Reference Materials, www.nist.gov, as standard sample No. 350. ]

Benzophenone,

(C6H5)2CO—182.22

[119-61-9]—White, crystalline powder.

: between 47

and 49

p-Benzoquinone (Quinone),

C6H4O2—108.09

[106-51-4]—Dark yellow powder having a green cast. Slightly soluble in water; soluble in alcohol, in ether, and in fixed alkali solutions. May darken on standing. Darkened material may be purified by sublimation in vacuum.

: between 113

and 115

Benzoyl Chloride,

C6H5COCl—140.57

[98-88-4]—Use ACS reagent grade.

N-Benzoyl-l-arginine Ethyl Ester Hydrochloride,

C15H22N4O3·HCl—342.82—Determine suitability for use as a substrate as directed under Crystallized Trypsin (USP monograph).

3-Benzoylbenzoic Acid,

C14H10O3—226.23

[579-18-0]—White to off-white powder.

Assay— Prepare a mixture of 1% trifluoroacetic acid in water and 1% trifluoroacetic acid in acetonitrile (55:45) for the mobile phase. Inject about 20 µL into a suitable liquid chromatograph (see Chromatography

) equipped with a 230-nm detector and a 4.6-mm × 15-cm column that contains packing L1. The flow rate is about 1.5 mL per minute. The area of the C14H10O3 peak is not less than 98.5% of the total peak area.

Benzoylformic Acid (Phenylglyoxylic Acid),

C6H5COCO2H—150.14

[611-73-4]—Powder. Soluble in methanol.

: between 62

and 67

Benzphetamine Hydrochloride,

C17H21N·HCl—275.82

[5411-22-3]—White to off-white, crystalline powder. Freely soluble in water, in alcohol, and in chloroform; slightly soluble in ether.

Assay— Dissolve about 500 mg, accurately weighed, in a mixture of 50 mL of glacial acetic acid and 10 mL of mercuric acetate TS, add 1 drop of crystal violet TS, and titrate with 0.1 N perchloric acid VS to a blue-green endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 27.58 mg of C17H21N·HCl. Between 98.0% and 101.0%, calculated on the dried basis, is found.

: between 152

and 158

Specific rotation

781

: between +22

and +26

, determined in a solution containing 200 mg in 10 mL, the specimen having been previously dried in vacuum at 60

for 3 hours.

Loss on drying

731

— Dry it in vacuum at 60

for 3 hours: it loses not more than 1% of its weight.

Residue on ignition

281

: not more than 0.2%.

2-Benzylaminopyridine,

C12H12N2—184.24

[6935-27-9]—Use a suitable grade.

1-Benzylimidazole,

C10H10N2—158.20

[4238-71-5]—White crystals.

Assay— Transfer about 40 mg, accurately weighed, to a 100-mL beaker. Dissolve in 50 mL of glacial acetic acid. Titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically using a combination calomel-platinum electrode. Perform a blank determination and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 15.82 mg of C10H10N2. Not less than 99% is found.

Benzyltrimethylammonium Chloride,

C6H5CH2N(CH3)3Cl—185.69

[56-93-9]—Available as a 60% aqueous solution. Is clear and is colorless or not more than slightly yellow.

Assay— Pipet 2 mL into a 50-mL volumetric flask, and add water to volume. Pipet 20 mL of the solution into a 125-mL conical flask, add about 30 mL of water, then add 0.25 mL of dichlorofluorescein TS, and titrate with 0.1 N silver nitrate VS. Each mL of 0.1 N silver nitrate is equivalent to 18.57 mg of C6H5CH2N(CH3)3Cl. Between 59.5% and 60.5% is found.

Beta-lactamase —Beta-lactamase is an enzyme produced by a variety of bacteria, but is usually obtained from culture filtrates of a strain of Bacillus cereus. It has the specific property of inactivating penicillins and cephalosporins by splitting the bond linking the nitrogen of the thiazolidine to the adjacent carbonyl carbon.

It occurs in the form of small, brown, easily pulverizable pieces or granules. Freely soluble in water, forming a slightly opalescent solution that is practically neutral to litmus paper. Is precipitated from its water solutions by acetone, by alcohol, and by dioxane, and is inactivated by contact with these solvents. Is rapidly inactivated by ethyl acetate and is irreversibly destroyed at a temperature of about 80

Beta-lactamase is assayed by a procedure depending upon a determination of the amount of penicillin G potassium or penicillin G sodium destroyed at a pH of 7.0 in a solution of such concentration that the inactivation proceeds as a zero-order reaction.

Betanaphthol —See 2-Naphthol.

Bibenzyl (Dibenzyl),

C14H14—182.26

[103-29-7]—Colorless crystals. Freely soluble in chloroform and in ether; sparingly soluble in alcohol; practically insoluble in water.

: between 53

and 55

Bile Salts —A concentrate of beef bile, the principal constituent of which is sodium desoxycholate, determined as cholic acid. Soluble in water and in alcohol; the solutions foam strongly when shaken.

Insoluble substances— Dissolve 5 g in 100 mL of dilute alcohol (84 in 100), warming if necessary to aid solution. Filter within 15 minutes through a tared filter, and wash with small portions of the dilute alcohol until the last washing is colorless or practically so, then dry the residue at 105

for 1 hour, and weigh: the weight of the residue does not exceed 0.1%.

Assay—

Standard Cholic Acid Solution— Dissolve 50.0 mg of cholic acid, accurately weighed, in dilute acetic acid (6 in 10) to make 100 mL, and mix. Store in a refrigerator.

Procedure— Dissolve 1.0 g, accurately weighed, in 50 mL of dilute acetic acid (6 in 10). Filter the solution, if necessary, into a 100-mL volumetric flask, wash the original container and the filter with small portions of dilute acetic acid (6 in 10), add the same acetic acid to volume, and mix. Dilute 10 mL of this solution, accurately measured, with dilute acetic acid (6 in 10) to make 100 mL, and mix.

Pipet 1 mL each of the Standard Cholic Acid Solution and the solution of the Bile Salts into two matched test tubes. To each tube add 1 mL, accurately measured, of freshly prepared furfural solution (1 in 100), immediately place the tubes in an ice-bath for 5 minutes, then add to each tube 13 mL, accurately measured, of dilute sulfuric acid, made by cautiously mixing 50 mL of sulfuric acid with 65 mL of water. Mix the contents of the tubes, and place them in a water bath maintained at a temperature of 70

for 10 minutes. Immediately transfer the tubes to an ice-bath for 2 minutes, then determine the absorbance of each solution at the wavelength of maximum absorbance at about 670 nm, with a suitable spectrophotometer. Calculate the quantity, in mg, of cholic acid (C24H40O5) in the weight of the Bile Salts taken by the formula:

500(AU/AS)

in which AU and AS are the absorbances of the solutions from the Bile Salts and the Standard Cholic Acid Solution, respectively. Not less than 45% of cholic acid is found.

Biphenyl,

C12H10—154.21

[92-52-4]—Colorless to white crystals or crystalline powder. Insoluble in water; soluble in alcohol and in ether. Boils at about 254

: between 68

and 72

2,2¢-Bipyridine (

¢-Dipyridyl),

C10H8N2—156.18

[366-18-7]—White or pink, crystalline powder. Soluble in water and in alcohol. Melts at about 69

, and boils at about 272

Sensitiveness— Prepare the following solutions: (A)—Dissolve 350 mg of ferrous ammonium sulfate in 50 mL of water containing 1 mL of sulfuric acid, and add 500 mg of hydrazine sulfate, then add water to make 500 mL. For use, dilute this solution with water in the ratio of 1 in 100 mL. (B)—Dissolve 8.3 g of sodium acetate and 12 mL of glacial acetic acid in water to make 100 mL. Add 1 mL of a solution of the specimen (1 in 1000) to a mixture of 10 mL of water and 1 mL of each of solutions A and B: a pink color results immediately.

Solubility— A 100-mg portion dissolves completely in 10 mL of water.

Residue on ignition (Reagent test): not more than 0.2%.

4,4¢-Bis(4-amino-1-naphthylazo)-2,2¢-stilbenedisulfonic Acid,

C34H26N6O6S2—678.74

[5463-64-9]—Use a suitable grade.

[Note—A suitable grade is available from TCI America, www.tciamerica.com. ]

Bis(2-ethylhexyl) Maleate,

C20H36O4—340.50

[142-16-5]—Colorless to pale yellow, clear liquid. Miscible with acetone and with alcohol. Specific gravity about 0.945.

Assay— Place about 2.5 g, accurately weighed, in a 250-mL flask, add 50.0 mL of 0.5 N alcoholic potassium hydroxide VS, and reflux for 45 minutes. Cool, add 0.5 mL of phenolphthalein TS, and titrate the excess alkali with 0.5 N hydrochloric acid VS. Perform a blank determination at the same time, using the same amount of 0.5 N alcoholic potassium hydroxide (see Residual Titrations under Titrimetry

541

). The difference, in mL, between the volumes of 0.5 N hydrochloric acid consumed in the test titration and blank titration, multiplied by 85.1, represents the quantity, in mg, of bis(2-ethylhexyl) maleate in the portion taken. Not less than 97% is found.

Bis(2-ethylhexyl) Phthalate,

C6H4-1,2-[COOCH2(C2H5)CH(CH2)3CH3]2—390.56

[117-81-7]—Colorless to light yellow liquid.

: between 1.4855 and 1.4875, at 20

Bis(2-ethylhexyl) Sebacate (Dioctyl Sebacate),

C8H17OOC(CH2)8COOC8H17—426.67

[122-62-3]—Pale straw-colored liquid. Insoluble in water. Refractive index about 1.448. Suitable for use in gas chromatography.

Specific gravity, 20

/20

841

: between 0.913 and 0.917.

Boiling range: between 243

and 248

at 5 mm of mercury.

[Note—A suitable grade is “Dioctyl Sebacate,” available from Sigma-Aldrich, www.sigma-aldrich.com. ]

Bis(2-ethylhexyl)phosphoric Acid [Bis(2-ethylhexyl) Phosphate],

[CH3(CH2)3CH(C2H5)CH2]2HPO4—322.42

[298-07-7]—Light yellow, viscous liquid. Insoluble in water; freely soluble in chloroform and in ethyl acetate. Refractive index: about 1.443. Specific gravity: about 0.997.

Assay— Dissolve about 250 mg, accurately weighed, in 50 mL of dimethylformamide, add 3 drops of a 1 in 100 solution of thymol blue TS in dimethylformamide, and titrate with 0.1 N sodium methoxide VS to a blue endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N sodium methoxide is equivalent to 32.24 mg of (C8H17)2HPO4. Between 95% and 105% is found.

Solubility— One volume dissolves in 9 volumes of chloroform to yield a clear solution, and 1 volume dissolves in 9 volumes of ethyl acetate to yield a clear solution.

Color— A 1 in 100 solution in chloroform exhibits an absorptivity of not more than 0.03 at 420 nm.

Bis(4-sulfobutyl) Ether Disodium,

Na2C8H16O7S2—334.32—Use a suitable grade with a content of NLT 95%.

[Note—A suitable grade is available as catalog number RM-969-C50 from www.cydexpharma.com. ]

Add the following:

Bismuth,

Bi—208.98

[

7440-69-9]— Use a suitable grade with a content of NLT 99.999%.

1S (USP38)

Bismuth Nitrate Pentahydrate,

Bi(NO3)3·5H2O—485.07

[10035-06-0]—Use ACS reagent grade.

Bismuth Subnitrate (Bismuth(III) Nitrate Basic),

Bi5O (OH)9(NO3)4—1461.99

[1304-85-4]—Use Bismuth Subnitrate (USP monograph).

Bismuth Sulfite Agar —Use a suitable grade.

Bis(trimethylsilyl)acetamide (N,O-Bis(trimethylsilyl)acetamide; BSA),

CH3CON[Si(CH3)3]2—203.43

[10416-59-8]—Clear, colorless liquid. Readily hydrolyzes when exposed to moist air. Handle under nitrogen, and store in a cool place.

Assay— Not less than 90% of CH3CON[Si(CH3)3]2, a suitable gas chromatograph equipped with a thermal conductivity detector being used. The following conditions are suitable and provide a retention time of approximately 15 minutes.

Column: 3-mm × 1.83-m stainless steel containing 5% phase G1 on support S1A.

Injection Temperature: 160

Column Temperature: 90

, programmed to rise 4

per minute to 160

Carrier Gas: Helium.

: between 1.4150 and 1.4170 at 20

Bis(trimethylsilyl)trifluoroacetamide (N,O-Bis(trimethylsilyl)trifluoroacetamide; BSTFA),

CF3CON[Si(CH3)3]2—257.40

[25561-30-2]—Clear, colorless liquid. Readily hydrolyzes when exposed to moist air. Store in a cool place.

Assay— Not less than 98% of CF3CON[Si(CH3)3]2, a suitable gas chromatograph equipped with a thermal conductivity detector being used. The following conditions are suitable and provide a retention time of approximately 15 minutes.

Column: 3-mm × 1.83-m stainless steel containing 5% phase G1 on support S1A.

Injection Temperature: 170

Column Temperature: 70

, programmed to rise 4

per minute to 140

Carrier Gas: Helium.

: between 1.3820 and 1.3860 at 20

Bis(trimethylsilyl)trifluoroacetamide with Trimethylchlorosilane

[25561-30-2]—Use a suitable grade.

[Note—A suitable grade is available from Sigma-Aldrich, www.sigma-aldrich.com. ]

Blood (for carbon monoxide test in gases)—Use oxalated or defibrinated blood of dogs, sheep, cattle, or human beings within 24 hours after bleeding. Prepare oxalated blood by adding 10 mg of sodium oxalate to each mL of the freshly drawn blood.

Blood Group A1 Red Blood Cells and Blood Group B Red Blood Cells— These cells must be obtained from manufacturers or suppliers licensed by the Center for Biologics Evaluation and Research/Food and Drug Administration. The use of reagents from an unlicensed manufacturer or supplier may invalidate the results. Generally, they are available as part of a kit for ABO Blood Group testing. The cells licensed for use in test tubes can also be used in the microtiter plate method described in the monographs of Red Blood Cells and Whole Blood.

[Note—There are many manufacturers and suppliers of these reagents that are licensed by the Center for Biologics Evaluation and Research Food and Drug Administration. Some examples of licensed manufacturers or suppliers are the following: Gamma Biologics, Houston, TX; and Ortho Diagnostics, Raritan, NJ. ]

Anti-A Blood Grouping Reagent, Anti-B Blood Grouping Reagent, and Anti-AB Blood Grouping Reagent— The reagents can be monoclonal or polyclonal and must be obtained from manufacturers or suppliers licensed by the Center for Biologics Evaluation and Research, Food and Drug Administration for use in microplate tests. The use of reagents from an unlicensed manufacturer or supplier may invalidate the results. Generally, all three reagents are available as part of a kit.

[Note—There are many manufacturers and suppliers of these reagents that are licensed by the Center for Biologics Evaluation and Research, Food and Drug Administration. Some examples of licensed manufacturers or suppliers are the following: Gamma Biologics, Houston, TX; and Ortho Diagnostics, Raritan, NJ. ]

Blue Tetrazolium (3,3¢-(3,3¢-Dimethoxy[1,1¢-biphenyl]-4,4¢-diyl)bis[2,5-diphenyl-2H-tetrazolium]dichloride),

C40H32Cl2N8O2—727.64

[1871-22-3]—Lemon-yellow crystals. Slightly soluble in water; freely soluble in chloroform and in methanol; insoluble in acetone and in ether.

Solubility in methanol— Dissolve 1 g in 100 mL of methanol: complete solution results, and the solution is clear.

Color— Transfer a portion of the methanol solution obtained in the preceding test to a 1-cm cell, and determine its absorbance at 525 nm, against water as the blank: the absorbance does not exceed 0.20.

Molar absorptivity

851

— Its molar absorptivity in methanol, at 252 nm, is not less than 50,000.

Suitability test—

Standard Preparation— Dissolve in alcohol a suitable quantity of USP Hydrocortisone RS, previously dried at 105

for 3 hours and accurately weighed, and prepare by stepwise dilution a solution containing about 10 µg per mL.

Procedure— Pipet 10-, 15-, and 20-mL portions of Standard Preparation into separate, glass-stoppered, 50-mL conical flasks. Add 10 mL and 5 mL, respectively, of alcohol to the flasks containing the 10- and 15-mL portions of Standard Preparation, and swirl to mix. To each of the flasks, and to a fourth flask containing 20 mL of alcohol, add 2.0 mL of a solution prepared by dissolving 50 mg of blue tetrazolium in 10 mL of alcohol, mix, and then add 2.0 mL of a solution prepared by diluting 1 mL of tetramethylammonium hydroxide TS with alcohol to 10 mL. Mix, allow the flasks to stand in the dark for 90 minutes, and determine the absorbances of the three solutions of the steroid standard at 525 nm, with a suitable spectrophotometer, using the solution in the fourth flask as the blank. Plot the absorbances on the abscissa and the amount of hydrocortisone on the ordinate scale of arithmetic coordinate paper, and draw the curve of best fit: the absorbance of each solution is proportional to the concentration, and the absorbance of the solution containing 200 µg of hydrocortisone is not less than 0.50.

Boldine (2,9-Dihydroxy-1,10-dimethoxyaporphine),

C19H21NO4—327.37

[476-70-0]—Use a suitable grade.

Boric Acid,

H3BO3—61.83

[10043-35-3]—Use ACS reagent grade.

(–)-Bornyl Acetate (1,7,7-Trimethylbicyclo[2,2,1]-heptan-2-ol acetate),

C12H20O2—196.29

[5655-61-8]—Use a suitable grade.

Boron Trifluoride,

BF3—67.81

[7637-07-2]—Use a suitable grade.

14% Boron Trifluoride–Methanol

[373-57-9]—Use a suitable grade.

Bovine Collagen— Use a suitable grade that contains less than 1 µg glycosaminoglycan per mg.

[Note—A suitable grade is available from Sigma-Aldrich, www.sigma-aldrich.com. ]

7 Percent Bovine Serum Albumin Certified Standard —Available from the National Institute of Standards and Technology, www.nist.gov, as SRM 927.

Branched Polymeric Sucrose—about 400 kDa

[26873-85-8]—White to off-white powder. Synthetic polymer made by the copolymerization of sucrose and epicholrohydrin. Use a suitable grade.

[Note—A suitable grade is available commercially as “Ficoll” from Pharmacia Fine Chemicals, Inc., 800 Centennial Ave., Piscataway, NJ 08854. ]

Brilliant Green (Malachite Green G),

C27H34N2O4S—482.64

[3051-11-4]—Glistening, golden-yellow crystals. Soluble in water and in alcohol. Absorption maximum: 623 nm.

Bromelain— A proteolytic enzyme isolated from pineapple. Use a suitable grade.

Bromine,

Br—At. Wt. 79.904

[7726-95-6]—Use ACS reagent grade.

-Bromo-2¢-acetonaphthone (Bromomethyl 2-naphthyl ketone),

C12H9BrO—249.10—Tannish–pink crystals.

between 81

and 83

p-Bromoaniline,

C6H6BrN—172.02

[106-40-1]—White to off-white crystals. Insoluble in water; soluble in alcohol and in ether.

Assay— Transfer about 650 mg, accurately weighed, to a suitable container, and dissolve in 50 mL of glacial acetic acid TS. Add crystal violet TS, and titrate with 0.1 N perchloric acid VS. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 17.20 mg of C6H6BrN. Not less than 98% is found.

: between 60

and 65

, within a 2

range.

Bromofluoromethane— Use a suitable grade.

N-Bromosuccinimide,

C4H4BrNO2—177.98

[128-08-5]—White to off-white crystals or powder. Freely soluble in water, in acetone, and in glacial acetic acid. [Caution—Highly irritating to eyes, skin, and mucous membranes. ]

Assay— Transfer 200 mg, accurately weighed, to a conical flask, add 25 mL of 0.5 N alcoholic potassium hydroxide, cover with a watch glass, heat to boiling, and boil for 5 minutes. Cool, transfer the solution to a beaker, rinsing the flask with water until the total volume of solution plus rinsings is about 100 mL, and add 10 mL of glacial acetic acid. Insert suitable electrodes, and titrate with 0.1 N silver nitrate VS, determining the endpoint potentiometrically. Each mL of 0.1 N silver nitrate is equivalent to 17.80 mg of C4H4BrNO2. Not less than 98% is found.

Change to read:

Brucine Sulfate,

(C23H26N2O4)2·H2SO4·7H2O—1013.11

[60583-39-3]

USP38

—Use ACS reagent grade.

Buffers —See Buffer Solutions under Solutions.

Butane-1,2-diol (1,2-Butanediol),

C4H10O2—90.12

[584-03-2]—Use a suitable grade with a content of NLT 97%.

Butane-1,4-diol (1,4-Butanediol, 1,4-Butylene Glycol),

C4H10O2—90.12

[110-63-4]—Use a suitable grade with a content of NLT 98%.

Butane-2,3-diol (2,3-Butanediol, 2,3-Butylene Glycol),

C4H10O2—90.12

[513-85-9]—Use a suitable grade with a content of NLT 97%.

1,3-Butanediol (1,3-Butylene Glycol),

C4H10O2—90.12

[107-88-0]—Viscous, colorless liquid. Very hygroscopic. Soluble in water, in alcohol, in acetone, and in methyl ethyl ketone; practically insoluble in aliphatic hydrocarbons, in benzene, and in toluene.

Assay— Inject an appropriate specimen into a suitable gas chromatograph (see Chromatography

) equipped with a flame-ionization detector, helium being used as the carrier gas. The following conditions have been found suitable: a 3-mm × 1.8-m stainless steel column containing 20% phase G16 on support S1A; the injection port temperature is maintained at 265

; the column temperature is maintained at 150

and programmed to rise 8

per minute to 210

. The area of the butanediol peak is not less than 98% of the total peak area.

: between 1.4390 and 1.4410 at 20

2,3-Butanedione (Diacetyl),

CH3COCOCH3—86.09

[431-03-8]—Bright yellow to yellowish-green liquid. Soluble in water. Miscible with alcohol and with ether. Boils at about 88

Assay—

hydroxylamine hydrochloride solution— Dissolve 20 g of hydroxylamine hydrochloride in 40 mL of water, and dilute with alcohol to 400 mL. Add, with stirring, 300 mL of 0.5 N alcoholic potassium hydroxide VS, and filter. Discard after 2 days.

procedure— Transfer about 1 g, accurately weighed, to a glass-stoppered, 250-mL flask, add 75.0 mL of Hydroxylamine hydrochloride solution, and insert the stopper in the flask. Reflux the mixture for 1 hour, then cool to room temperature. Add bromophenol blue TS, and titrate with 0.5 N hydrochloric acid VS to a greenish-yellow endpoint. [Note—Alternatively, the solution may be titrated potentiometrically to a pH of 3.4. ] Perform a blank test with the same quantities of reagent used for the test specimen, and make any necessary correction. Each mL of 0.5 N hydrochloric acid is equivalent to 43.05 mg of CH3COCOCH3. Not less than 97% of CH3COCOCH3 is found.

Congealing temperature

651

: between

2.0

and

5.5

: between 1.3935 and 1.3965, at 20

Specific gravity

841

: about 0.98.

1-Butanesulfonic Acid Sodium Salt (Sodium 1-butanesulfonate),

C4H9NaO3S—160.16

[2386-54-1]—Use a suitable grade with a content of not less than 99.0%.

1,4-Butane Sultone (4-Hydroxybutane-1-sulfonic Acid delta-sultone),

C4H8O3S—136.17

[1633-83-6]—Use a suitable grade with a content of NLT 99%.

Butanol —See Butyl Alcohol.

Butyl Acetate, Normal,

CH3COO(CH2)3CH3—116.16

[123-86-4]—Use ACS reagent grade.

Butyl Alcohol (1-Butanol; Normal Butyl Alcohol),

CH3(CH2)2CH2OH—74.12

[71-36-3]—Use ACS reagent grade.

Butyl Alcohol, Normal —See Butyl Alcohol.

Butyl Alcohol, Secondary (2-Butanol),

CH3CH2CH(OH)CH3—74.12

[78-92-2]—Use a suitable grade with a content of NLT 99%.

Butyl Alcohol, Tertiary,

(CH3)3COH—74.12

[75-65-0]—Use ACS reagent grade tert-Butyl Alcohol.

Butyl Benzoate,

C11H14O2—178.23

[136-60-7]—Thick, oily, colorless to pale yellow liquid. Practically insoluble in water; soluble in alcohol and in ether.

Assay— When examined by gas-liquid chromatography, it shows a purity of not less than 98%. The following conditions have been found suitable for assaying it: use a 3-mm × 1.8-m stainless steel column packed with liquid phase G4 on support S1A. Helium is the carrier gas, the injection port temperature is maintained at 180

, the column temperature is maintained at 190

, and the flame-ionization detector is maintained at 280

. The retention time is about 15 minutes.

: between 1.4980 and 1.5000, at 20

n-Butyl Chloride (1-Chlorobutane),

C4H9Cl—92.57

[109-69-3]—Clear, colorless, volatile liquid. [Caution——Highly flammable. ] Practically insoluble in water. Miscible with alcohol and with ether. Use HPLC grade.

Butyl Ether (n-Dibutyl Ether),

C8H18O—130.23

[142-96-1]—Use a suitable grade.

Butyl Methacrylate,

C8H14O2—142.20

[97-88-1]—Use a suitable grade.

tert-Butyl Methyl Ether,

C5H12O—88.15

[1634-04-4]—Colorless liquid.

Assay— Inject an appropriate specimen into a gas chromatograph (see Chromatography

) equipped with a flame-ionization detector, helium being used as the carrier gas. The following conditions have been found suitable: a 0.25-mm × 30-m capillary column coated with a 1-µm layer of phase G2; the injection port temperature is maintained at 100

; the detector temperature is maintained at 300

; and the column temperature is maintained at ambient temperature and programmed to rise 10

per minute to 150

. The area of the C5H12O peak is not less than 99.8% of the total peak area.

: between 1.367 and 1.371 at 20

n-Butylamine,

CH3CH2CH2CH2NH2—73.14

[109-73-9]—Colorless to pale yellow, flammable liquid. Miscible with water, with alcohol, and with ether. Store it in tight containers. Specific gravity: about 0.740.

Distilling range, Method I

721

— Not less than 95% distills between 76

and 78

Water, Method I

921

: not more than 1.0%, determined by the Titrimetric Method.

Chloride (Reagent test)— One g (1.5 mL) shows not more than 0.01 mg of Cl (0.001%).

Acidic impurities— To 50 mL add 5 drops of a saturated solution of azo violet in benzene, and titrate quickly with 0.1 N sodium methoxide VS to a deep blue endpoint, observing precautions to prevent absorption of atmospheric carbon dioxide as by use of an atmosphere of nitrogen: not more than 1.0 mL of 0.1 N sodium methoxide is required for neutralization.

tert-Butylamine,

C3H9CNH2—73.14

[75-64-9]—Liquid.

Assay— Inject an appropriate volume into a gas chromatograph (see Chromatography

; the detector temperature is maintained at 300

; the column temperature is maintained at 130

and programmed to rise 10

per minute to 280

. The area of the C3H9CNH2 peak is not less than 99.5% of the total peak area.

: between 1.3770 and 1.3790 at 20

4-(Butylamino)benzoic Acid,

C11H5NO2—193.25

[4740-24-3]—Use a suitable grade.

[Note—A suitable grade is available from Sigma-Aldrich, Inc., P.O. Box 2060, Milwaukee, WI 53201; www.sigma- aldrich.com. ]

n-Butylboronic Acid (1-Butaneboronic Acid),

C4H9B(OH)2—101.94

[4426-47-5]—Use a suitable grade.

[Note—This reagent is usually shipped and stored under water. Before use, remove any excess water by light vacuum filtration. A suitable grade is available from Sigma-Aldrich, www.sigma-aldrich.com. ]

tert-Butyldimethylchlorosilane in N-Methyl-N-tert-butyldimethylsilyltrifluoroacetamide, (1 in 100) —Use a suitable grade.

[Note—A suitable grade is available as 99% MTBSTFA, 1% TBDMCS from Regis Chemical Company, 8210 Austin Ave., P.O. Box 519, Morton Grove, IL 60053. ]

4-tert-Butylphenol,

C10H14O—150.22

[98-54-4]—White, crystalline flakes or needles. Practically insoluble in water; soluble in alcohol and in ether.

: between 98

and 101

t-Butylthiol (tert-Butylthiol; tert-Butyl Mercaptan; 2-Methyl-2-propanethiol; TBM),

(CH3)3CSH—90.19

[75-66-1]—Use a suitable grade with a content of NLT 98.0%.

[Note—A suitable grade is available as catalog number 20230 at www.sigma-aldrich.com. ]

Butyraldehyde (Butanal),

C4H8O—72.11

[123-72-8]—Use a suitable grade, purified by redistillation, with a content of not less than 99.5%.

Butyric Acid,

C4H8O2—88.11

[107-92-6]—Clear, colorless to faint yellow liquid. Miscible with water and with methanol.

Assay— Weigh accurately about 500 mg, transfer to a suitable container, add 30 mL of water, and mix. Add 40 mL of water, and mix. Add phenolphthalein TS, and titrate with 0.1 N sodium hydroxide VS. Each mL of 0.1 N sodium hydroxide is equivalent to 8.81 mg of C4H8O2: not less than 99.0% of C4H8O2 is found.