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USP 40 Solutions / Test Solutions 2411

Citrate Buffer
0.1 M
Citric
Acid,
mL 82.0 77.5 73.0 68.5 63.5 59.0 54.0 49.5 44.5 40.0 35.0 30.5 25.5 21.0 16.0 11.5 8.0
0.1 M
Sodium
Citrate,
mL 18.0 22.5 27.0 31.5 36.5 41.0 46.0 50.5 55.5 60.0 65.0 69.5 74.5 79.0 84.0 88.5 92.0

COLORIMETRIC SOLUTIONS (CS) Ferric Chloride CS—Dissolve about 55 g of ferric chloride

(FeCl3 · 6H2O) in enough of a mixture of 25 mL of hydro-
chloric acid and 975 mL of water to make 1000 mL. Pipet
10 mL of this solution into a 250-mL iodine flask, add 15 mL
1. DEFINITION of water, 3 g of potassium iodide, and 5 mL of hydrochloric
acid, and allow the mixture to stand for 15 minutes. Dilute
Colorimetric solutions are used in the preparation of the with 100 mL of water, and titrate the liberated iodine with
colorimetric standards for certain drugs and for the 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as
carbonization tests with sulfuric acid that are specified in the indicator. Perform a blank determination with the same
some monographs. quantities of the same reagents, and make any necessary
For the preparation of matching fluids, see Color and correction. Each mL of 0.1 N sodium thiosulfate is equiva-
Achromicity 〈631〉. lent to 27.03 mg of FeCl3 · 6H2O. Adjust the final volume of
the solution by the addition of enough of the mixture of
2. STORAGE hydrochloric acid and water so that each mL contains
45.0 mg of FeCl3 · 6H2O.
Store colorimetric solutions in suitably resistant, tight
containers. INDICATORS SOLUTIONS
3. COMPARISON OF COLORS See TEST SOLUTIONS.

Comparison of colors as directed in the Pharmacopeial TEST SOLUTIONS (TS)

tests preferably is made in matched color-comparison tubes
or in a suitable colorimeter under conditions that ensure
that the colorimetric reference solution and that of the spec-
imen under test are treated alike in all respects. The com- 1. USE AS INDICATORS
parison of colors is best made in layers of equal depth, and
viewed transversely against a white background (see also Certain test solutions are intended for use as acid-base
Nephelometry, Turbidimetry, and Visual Comparison 〈855〉). indicators in volumetric analyses. Such solutions should be
It is particularly important that the solutions be compared so adjusted that when 0.15 mL of the indicator solution is

Reagents
at the same temperature, preferably 25°. added to 25 mL of carbon dioxide-free water, 0.25 mL of
0.02 N acid or alkali will produce the characteristic color
Cobaltous Chloride CS—Dissolve about 65 g of cobaltous change. Similar solutions are intended for use in pH meas-
chloride (CoCl2 · 6H2O) in enough of a mixture of 25 mL of urement. Where no special directions for their preparation
hydrochloric acid and 975 mL of water to make 1000 mL. are given, the same solution is suitable for both purposes.
Pipet 5 mL of this solution into a 250-mL iodine flask, add
5 mL of hydrogen peroxide TS and 15 mL of sodium hy- 2. VOLUMETRIC SOLUTIONS USED AS TEST
droxide solution (1 in 5), boil for 10 minutes, cool, and add
2 g of potassium iodide and 20 mL of dilute sulfuric acid (1 SOLUTIONS
in 4). When the precipitate has dissolved, titrate the liber-
ated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL Where it is directed that a volumetric solution be used as
of starch TS as the indicator. Perform a blank determination the test solution in a qualitative procedure, standardization
with the same quantities of the same reagents, and make of the solution used as the test solution is not required.
any necessary correction. Each mL of 0.1 N sodium thiosul-
fate is equivalent to 23.79 mg of CoCl2 · 6H2O. Adjust the 3. SOLUTIONS PREPARED FRESH
final volume of the solution by the addition of enough of
the mixture of hydrochloric acid and water so that each mL In general, the directive to prepare a solution “fresh” indi-
contains 59.5 mg of CoCl2 · 6H2O. cates that the solution is of limited stability and must be
prepared on the day of use.
Cupric Sulfate CS—Dissolve about 65 g of cupric sulfate
(CuSO4 · 5H2O) in enough of a mixture of 25 mL of hydro- Acetaldehyde TS—Mix 4 mL of acetaldehyde, 3 mL of alco-
chloric acid and 975 mL of water to make 1000 mL. Pipet hol, and 1 mL of water. Prepare this solution fresh.
10 mL of this solution into a 250-mL iodine flask, add 40 mL
of water, 4 mL of acetic acid, 3 g of potassium iodide, and Acetate Buffer TS—Dissolve 320 g of ammonium acetate in
5 mL of hydrochloric acid, and titrate the liberated iodine 500 mL of water, add 5 mL of glacial acetic acid, dilute with
with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS water to 1000.0 mL, and mix. This solution has a pH be-
as the indicator. Perform a blank determination with the tween 5.9 and 6.0.
same quantities of the same reagents, and make any neces-
sary correction. Each mL of 0.1 N sodium thiosulfate is
equivalent to 24.97 mg of CuSO4 · 5H2O. Adjust the final
volume of the solution by the addition of enough of the Add the following:
mixture of hydrochloric acid and water so that each mL
contains 62.4 mg of CuSO4 · 5H2O. ▲1 M Acetic Acid TS—Transfer 57.4 mL of glacial acetic acid
to a 1000-mL volumetric flask. Dilute with water to volume.
▲USP40

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2412 Test Solutions / Solutions USP 40

Add the following: Alkaline Cupric Iodide TS—See Cupric Iodide TS, Alkaline.

▲2 M Acetic Acid TS—Transfer 114.8 mL of glacial acetic Alkaline Cupric Tartrate TS (Fehling’s Solution)—see Cupric
acid to a 1000-mL volumetric flask. Dilute with water to Tartrate TS, Alkaline.
volume.▲USP40
Alkaline Mercuric–Potassium Iodide TS—See
Acetic Acid, Glacial, TS—Determine the water content of a Mercuric–Potassium Iodide TS, Alkaline.
specimen of glacial acetic acid by the Titrimetric Method (see
Water Determination 〈921〉). If the acid contains more than Alkaline Picrate TS—See Picrate TS, Alkaline.
0.4% of water, add a few mL of acetic anhydride, mix, al-
low to stand overnight, and again determine the water con- Alkaline Sodium Hydrosulfite TS—See Sodium Hydrosulfite
tent. If the acid contains less than 0.02% of water, add TS, Alkaline.
sufficient water to make the final concentration between
0.02% and 0.4%, mix, allow to stand overnight, and again Amaranth TS—Dissolve 20 mg of amaranth in 10 mL of
determine the water content. Repeat the adjustment with water.
acetic anhydride or water, as necessary, until the resulting
solution shows a water content of not more than 0.4%. Aminonaphtholsulfonic Acid TS—Accurately weigh 5 g of
sodium sulfite, 94.3 g of sodium bisulfite, and 700 mg of
Acetic Acid, Strong, TS—Add 300.0 mL of glacial acetic 1,2,4-aminonaphtholsulfonic acid, and mix. Prepare amino-
acid, and dilute with water to 1000 mL. This solution con- naphtholsulfonic acid TS fresh on the day of use by dissolv-
tains about 30% (v/v) of CH3COOH and has a concentration ing 1.5 g of the dry mixture in 10 mL of water.
of about 5 N.
Ammonia TS—It contains between 9.5% and 10.5% of
Acetic Acid–Ammonium Acetate Buffer TS—Dissolve NH3. Prepare by diluting 350 mL of Ammonia Water,
77.1 g of ammonium acetate in water, add 57 mL of glacial Stronger (see in the section, Reagents) with water to make
acetic acid, and dilute with water to 1000 mL. 1000 mL.

Acetone, Buffered, TS—Dissolve 8.15 g of sodium acetate Ammonia TS 2—Prepare by diluting 13.5 mL of Ammonia
and 42 g of sodium chloride in about 100 mL of water, and Water, Stronger (see Reagent Specifications in the section Re-
add 68 mL of 0.1 N hydrochloric acid and 150 mL of ace- agents) with water to make 100 mL.
tone. Mix, and dilute with water to 500 mL.
Ammonia TS, Alcoholic—A solution of ammonia gas in al-
Acid Ferric Chloride TS—Mix 60 mL of glacial acetic acid cohol. Clear, colorless liquid having a strong odor of ammo-
with 5 mL of sulfuric acid, add 1 mL of ferric chloride TS, nia. Specific gravity: about 0.80. It contains between 9%
mix, and cool. and 11% of NH3. Store it in alkali-resistant containers, in a
cold place.
Acid Ferrous Sulfate TS—See Ferrous Sulfate, Acid, TS.
Ammonia TS, Stronger—Use Ammonia Water, Stronger (see
Acid Stannous Chloride TS—See Stannous Chloride, Acid, in the section Reagents).
TS.
Reagents

Ammonia–Ammonium Chloride Buffer TS—Dissolve

Acid Stannous Chloride TS, Stronger—See Stannous Chlo- 67.5 g of ammonium chloride in water, add 570 mL of am-
ride, Acid, Stronger, TS. monium hydroxide, and dilute with water to 1000 mL.

Albumen TS—Carefully separate the white from the yolk of Ammonia–Cyanide TS—Dissolve 2 g of potassium cyanide
a strictly fresh hen’s egg. Shake the white with 100 mL of in 15 mL of ammonium hydroxide, and dilute with water to
water until mixed and all but the chalaza has undergone 100 mL.
solution; then filter. Prepare the solution fresh.
Ammoniacal Potassium Ferricyanide TS—Dissolve 2 g of
Alcohol–Phenol TS—Dissolve 780 mg of phenol in alcohol potassium ferricyanide in 75 mL of water, add 25 mL of am-
to make 100 mL. monium hydroxide, and mix.

Alcoholic TS—It contains 95 parts of specially denaturated Ammoniated Cupric Oxide TS—See Cupric Oxide, Ammoni-
alcohol 3A with 5 parts of isopropyl alcohol. The final con- ated, TS.
centrations are approximately 90% alcohol, 5% methanol,
and 5% isopropanol. Ammonium Acetate TS—Dissolve 10 g of ammonium ace-
[NOTE—A suitable grade is available as Reagent alcohol, tate in water to make 100 mL.
catalog number R8382, available at [Link]-aldrich.
com.] Ammonium Carbonate TS—Dissolve 20 g of ammonium
carbonate and 20 mL of ammonia TS in water to make
Alcoholic Ammonia TS—See Ammonia TS, Alcoholic. 100 mL.

Alcoholic Mercuric Bromide TS—See Mercuric Bromide TS, Ammonium Carbonate TS 2—Prepare a 158-mg/mL solu-
Alcoholic. tion of ammonium carbonate in water.

Alcoholic Potassium Hydroxide TS—See Potassium Hydrox- Ammonium Chloride TS—Dissolve 10.5 g of ammonium
ide TS, Alcoholic. chloride in water to make 100 mL.

Alkaline Cupric Citrate TS—See Cupric Citrate TS, Alkaline. Ammonium Chloride–Ammonium Hydroxide TS—Mix
equal volumes of water and ammonium hydroxide, and sat-
Alkaline Cupric Citrate TS 2—See Cupric Citrate TS 2, Alka- urate with ammonium chloride.
line.

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USP 40 Solutions / Test Solutions 2413

Add the following: Barium Hydroxide TS—A saturated solution of barium hy-
droxide in recently boiled water. Prepare the solution fresh.
▲1 M Ammonium Hydroxide TS—Transfer 67.6 mL of am-
monium hydroxide to a 1000-mL volumetric flask. Dilute Barium Nitrate TS—Dissolve 6.5 g of barium nitrate in
with water to volume.▲USP40 water to make 100 mL.
Betanaphthol TS—See 2-Naphthol TS.
Add the following: Biuret Reagent TS—Dissolve 1.5 g of cupric sulfate and
6.0 g of potassium sodium tartrate in 500 mL of water in a
▲2 M Ammonium Hydroxide TS—Transfer 135 mL of am- 1000-mL volumetric flask. Add 300 mL of carbonate-free so-
monium hydroxide to a 1000-mL volumetric flask. Dilute dium hydroxide solution (1 in 10), dilute with carbonate-
with water to volume.▲USP40 free sodium hydroxide solution (1 in 10) to 1000 mL, and
mix.
Ammonium Molybdate TS—Dissolve 6.5 g of finely pow-
dered molybdic acid in a mixture of 14 mL of water and Blue Tetrazolium TS—Dissolve 500 mg of blue tet-
14.5 mL of ammonium hydroxide. Cool the solution, and razolium in alcohol to make 100 mL.
add it slowly, with stirring, to a well-cooled mixture of
32 mL of nitric acid and 40 mL of water. Allow to stand for Brilliant Blue G TS—Transfer 25 mg of brilliant blue G to a
48 hours, and filter through a fine-porosity, sintered-glass 100-mL volumetric flask, add 12.5 mL of alcohol and 25 mL
crucible. This solution deteriorates upon standing and is un- of phosphoric acid, dilute with water to volume, and mix.
suitable for use if, upon the addition of 2 mL of dibasic so-
dium phosphate TS to 5 mL of the solution, an abundant Bromine TS (Bromine Water)—A saturated solution of bro-
yellow precipitate does not form at once or after slight mine, prepared by agitating 2 to 3 mL of bromine with
warming. Store it in the dark. If a precipitate forms during 100 mL of cold water in a glass-stoppered bottle, the stop-
storage, use only the clear supernatant. per of which should be lubricated with petrolatum. Store it
in a cold place, protected from light.
Ammonium Oxalate TS—Dissolve 3.5 g of ammonium oxa-
late in water to make 100 mL. Bromine–Sodium Acetate TS—Dissolve 100 g of sodium
acetate in 1000 mL of glacial acetic acid, add 50 mL of bro-
Ammonium Phosphate, Dibasic, TS (Ammonium Phosphate mine, and mix.
TS)—Dissolve 13 g of dibasic ammonium phosphate in
water to make 100 mL. p-Bromoaniline TS—Add 8 g of p-bromoaniline to a mix-
ture of 380 mL of thiourea-saturated glacial acetic acid,
Ammonium Polysulfide TS—Yellow liquid, made by saturat- 10 mL of sodium chloride solution (1 in 5), 5 mL of oxalic
ing ammonium sulfide TS with sulfur. acid solution (1 in 20), and 5 mL of dibasic sodium phos-
phate solution (1 in 10) in a low-actinic glass bottle. Mix,
Ammonium Pyrrolidinedithiocarbamate, Saturated, TS— and allow to stand overnight before using. Protect from
Add about 10 g of ammonium pyrrolidinedithiocarbamate light, and use within 7 days.
to a 1000-mL volumetric flask, and dilute with water to vol-

Reagents
ume. Bromocresol Blue TS—Use Bromocresol Green TS.
Ammonium Reineckate TS—Shake about 500 mg of am- Bromocresol Green TS—Dissolve 50 mg of bromocresol
monium reineckate with 20 mL of water frequently during green in 100 mL of alcohol, and filter if necessary.
1 hour, and filter. Use within 2 days.
Bromocresol Green–Methyl Red TS—Dissolve 0.15 g of
Ammonium Sulfide TS—Use ACS reagent-grade Ammo- bromocresol green and 0.1 g of methyl red in 180 mL of
nium Sulfide Solution. alcohol, and dilute with water to 200 mL.
Ammonium Thiocyanate TS—Dissolve 8 g of ammonium Bromocresol Purple TS—Dissolve 250 mg of bromocresol
thiocyanate in water to make 100 mL. purple in 20 mL of 0.05 N sodium hydroxide, and dilute
with water to 250 mL.
Ammonium Vanadate TS—Dissolve 2.5 g of ammonium
vanadate in 500 mL of boiling water, cool, and add 20 mL Bromophenol Blue TS—Dissolve 100 mg of bromophenol
of nitric acid. Mix, cool, and add water to make 1 L. Store blue in 100 mL of diluted alcohol, and filter if necessary.
in polyethylene containers.
Bromothymol Blue TS—Dissolve 100 mg of bromothymol
Anthrone TS—Within 12 hours of use, rapidly dissolve blue in 100 mL of diluted alcohol, and filter if necessary.
35 mg of anthrone in a hot mixture of 35 mL of water and
65 mL of sulfuric acid. Immediately cool in an ice bath to Buffered Acetone TS—See Acetone, Buffered, TS.
room temperature, and filter through glass wool. Allow the
solution to stand at room temperature for 30 minutes before Calcium Chloride TS—Dissolve 7.5 g of calcium chloride in
use. water to make 100 mL.
Antimony Trichloride TS—Dissolve 20 g of antimony Calcium Hydroxide TS—Use Calcium Hydroxide Topical Solu-
trichloride in chloroform to make 100 mL. Filter if necessary. tion (USP monograph).
10% Ascorbic Acid TS—Transfer 10 g of ascorbic acid to a Calcium Sulfate TS—A saturated solution of calcium sulfate
100-mL volumetric flask. Dissolve in and dilute with water in water.
to volume.
Ceric Ammonium Nitrate TS—Dissolve 6.25 g of ceric am-
Barium Chloride TS—Dissolve 12 g of barium chloride in monium nitrate in 10 mL of 0.25 N nitric acid. Use within 3
water to make 100 mL. days.

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2414 Test Solutions / Solutions USP 40

Chloral Hydrate TS—Dissolve 50 g of chloral hydrate in a and filter. In a second flask, dissolve about 27.06 g of cupric
mixture of 15 mL of water and 10 mL of glycerin. sulfate (CuSO4 · 5H2O) in about 100 mL of water. Slowly
combine the two solutions while stirring, and dilute with
Chlorine TS (Chlorine Water)—A saturated solution of chlo- water to 1000 mL.
rine in water. Place the solution in small, completely filled,
light-resistant containers. Chlorine TS, even when kept from Cupric Iodide TS, Alkaline—Dissolve 7.5 g of cupric sulfate
light and air, is apt to deteriorate. Store it in a cold, dark (CuSO4 · 5H2O) in about 100 mL of water. In a separate
place. For full strength, prepare this solution fresh. container dissolve 25 g of anhydrous sodium carbonate,
20 g of sodium bicarbonate, and 25 g of potassium sodium
Chromotropic Acid TS—Dissolve 50 mg of chromotropic tartrate in about 600 mL of water. With constant stirring,
acid or its disodium salt in 100 mL of 75% sulfuric acid, add the cupric sulfate solution to the bottom of the alkaline
which may be made by cautiously adding 75 mL of sulfuric tartrate solution by means of a funnel that touches the bot-
acid to 33.3 mL of water. tom of the container. Add 1.5 g of potassium iodide, 200 g
of anhydrous sodium sulfate, 50 to 150 mL of 0.02 M po-
Cobalt–Uranyl Acetate TS—Dissolve, with warming, 40 g tassium iodate, and sufficient water to make 1000 mL.
of uranyl acetate in a mixture of 30 g of glacial acetic acid
and sufficient water to make 500 mL. Similarly, prepare a Cupric Oxide, Ammoniated, TS (Schweitzer’s Reagent)—
solution containing 200 g of cobaltous acetate in a mixture Dissolve 10 g of cupric sulfate in 100 mL of water, add suffi-
of 30 g of glacial acetic acid and sufficient water to make cient sodium hydroxide solution (1 in 5) to precipitate the
500 mL. Mix the two solutions while still warm, and cool to copper hydroxide, collect the latter on a filter, and wash
20°. Maintain the temperature at 20° for about 2 hours to free from sulfate with cold water. Dissolve the precipitate,
separate the excess salts from solution, and then pass which must be kept wet during the entire process, in the
through a dry filter. minimum quantity of ammonia TS necessary for complete
solution.
Cobaltous Chloride TS—Dissolve 2 g of cobaltous chloride
in 1 mL of hydrochloric acid and sufficient water to make Cupric Sulfate TS—Dissolve 12.5 g of cupric sulfate in
100 mL. water to make 100 mL.
Congo Red TS—Dissolve 500 mg of congo red in a mixture Cupric Tartrate TS, Alkaline (Fehling’s Solution)
of 10 mL of alcohol and 90 mL of water. THE COPPER SOLUTION (A): Dissolve 34.66 g of carefully se-
lected, small crystals of cupric sulfate, showing no trace of
m-Cresol Purple TS—Dissolve 0.10 g of metacresol purple efflorescence of adhering moisture, in water to make
in 13 mL of 0.01 N sodium hydroxide, dilute with water to 500 mL. Store this solution in small, tight containers.
100 mL, and mix. THE ALKALINE TARTRATE SOLUTION (B): Dissolve 173 g of
crystallized potassium sodium tartrate and 50 g of sodium
Cresol Red TS—Triturate 100 mg of cresol red in a mortar hydroxide in water to make 500 mL. Store this solution in
with 26.2 mL of 0.01 N sodium hydroxide until solution is small, alkali-resistant containers.
complete, then dilute the solution with water to 250 mL. For use, mix exactly equal volumes of Solutions A and B
at the time required.
Cresol Red–Thymol Blue TS—Add 15 mL of thymol blue TS
Reagents

to 5 mL of cresol red TS, and mix. Delafield’s Hematoxylin TS—Prepare 400 mL of a saturated
solution of ammonium alum (Solution A). Dissolve 4 g of
Crystal Violet TS—Dissolve 100 mg of crystal violet in hematoxylin in 25 mL of alcohol, mix it with Solution A, and
10 mL of glacial acetic acid. allow it to stand for 4 days in a flask closed with a pledget
of purified cotton and exposed to light and air (Solution B).
Cupric Acetate TS—Dissolve 100 mg of cupric acetate in Then filter Solution B, and add to it a Solution C consisting of
about 5 mL of water to which a few drops of acetic acid a mixture of 100 mL of glycerin and 100 mL of methanol.
have been added. Dilute to 100 mL, and filter, if necessary. Mix, and allow the mixture to stand in a warm place, ex-
posed to light, for 6 weeks until it becomes dark-colored.
Cupric Acetate TS, Stronger (Barfoed’s Reagent)—Dissolve Store in tightly stoppered bottles.
13.3 g of cupric acetate in a mixture of 195 mL of water For use in staining endocrine tissue, dilute this test solu-
and 5 mL of acetic acid. tion with an equal volume of water.
Cupric-Ammonium Sulfate TS—To cupric sulfate TS add Denaturated Alcoholic TS—A specially denaturated alcohol
ammonia TS, dropwise, until the precipitate initially formed containing either rubber hydrocarbon solvent of heptane or
is nearly but not completely dissolved. Allow to settle, and toluene. [NOTE—A suitable grade is available from [Link]-
decant the clear solution. Prepare this solution fresh. [Link] or from [Link], as Ethanol SDA 2B HEP
200, or Ethanol SDA 2B TOL 200, or Ethanol SDA 2B TOL
Cupric Citrate TS—Dissolve 25 g of cupric sulfate, 50 g of 190, or Alcohol SDA 2B-2.]
citric acid, and 144 g of anhydrous sodium carbonate in
water, and dilute with water to 1000 mL. Denigès’ Reagent—See Mercuric Sulfate TS.
Cupric Citrate TS, Alkaline—With the aid of heat, dissolve Diazobenzenesulfonic Acid TS—Place in a beaker 1.57 g of
173 g of dihydrated sodium citrate and 117 g of monohy- sulfanilic acid, previously dried at 105° for 3 hours, add
drated sodium carbonate in about 700 mL of water, and 80 mL of water and 10 mL of diluted hydrochloric acid, and
filter through paper, if necessary, to obtain a clear solution. warm on a steam bath until dissolved. Cool to 15° (some of
In a separate container dissolve 17.3 g of cupric sulfate in the sulfanilic acid may separate but will dissolve later), and
about 100 mL of water, and slowly add this solution, with add slowly, with constant stirring, 6.5 mL of sodium nitrite
constant stirring, to the first solution. Cool the mixture, add solution (1 in 10). Then dilute with water to 100 mL.
water to make 1000 mL, and mix.
Dichlorofluorescein TS—Dissolve 100 mg of dichlorofluo-
Cupric Citrate TS 2, Alkaline—With the aid of heat, dis- rescein in 60 mL of alcohol, add 2.5 mL of 0.1 N sodium
solve about 173 g of sodium citrate dihydrate and 117 g of hydroxide, mix, and dilute with water to 100 mL.
sodium carbonate monohydrate in about 700 mL of water,

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USP 40 Solutions / Test Solutions 2415

2,7-Dihydroxynaphthalene TS—Dissolve 100 mg of 2,7- Ferroin TS—Dissolve 0.7 g of ferrous sulfate and 1.76 g of
dihydroxynaphthalene in 1000 mL of sulfuric acid, and allow o-phenanthroline monohydrochloride monohydrate in
the solution to stand until the yellow color disappears. If the water, and dilute with water to 100 mL.
solution is very dark, discard it and prepare a new solution
from a different supply of sulfuric acid. This solution is stable Ferrous Sulfate TS—Dissolve 8 g of clear crystals of ferrous
for approximately 1 month if stored in a dark bottle. sulfate in about 100 mL of recently boiled and thoroughly
cooled water. Prepare this solution fresh.
Diiodofluorescein TS—Dissolve 500 mg of diiodofluorescein
in a mixture of 75 mL of alcohol and 30 mL of water. Ferrous Sulfate, Acid, TS—Dissolve 7 g of ferrous sulfate
crystals in 90 mL of recently boiled and thoroughly cooled
Diluted Lead Subacetate TS—See Lead Subacetate TS, Di- water, and add sulfuric acid to make 100 mL. Prepare this
luted. solution immediately prior to use.
p-Dimethylaminobenzaldehyde TS—Dissolve 125 mg of p- Folin-Ciocalteu Phenol TS—Into a 1500-mL flask introduce
dimethylaminobenzaldehyde in a cooled mixture of 65 mL 100 g of sodium tungstate, 25 g of sodium molybdate,
of sulfuric acid and 35 mL of water, and add 0.05 mL of 700 mL of water, 50 mL of phosphoric acid, and 100 mL of
ferric chloride TS. Use within 7 days. hydrochloric acid. Gently reflux the mixture for about
10 hours, and add 150 g of lithium sulfate, 50 mL of water,
Dinitrophenylhydrazine TS—Carefully mix 10 mL of water and a few drops of bromine. Boil the mixture, without the
and 10 mL of sulfuric acid, and cool. To the mixture, con- condenser, for about 15 minutes, or until the excess bro-
tained in a glass-stoppered flask, add 2 g of 2,4-dinitrophen- mine is expelled. Cool, dilute with water to 1 L, and filter:
ylhydrazine, and shake until dissolved. To the solution add the filtrate has no greenish tint. Before use, dilute 1 part of
35 mL of water, mix, cool, and filter. the filtrate with 1 part of water. When used for protein de-
termination (i.e., Lowry assay), this reagent must be further
Diphenylamine TS—Dissolve 1.0 g of diphenylamine in diluted (1:5) with water. See Method 2 in Total Protein Assay
100 mL of sulfuric acid. The solution should be colorless. under Biotechnology-Derived Articles—Total Protein Assay
〈1057〉.
Diphenylcarbazone TS—Dissolve 1 g of crystalline
diphenylcarbazone in 75 mL of alcohol, then add alcohol to Formaldehyde TS—Use Formaldehyde Solution (see in the
make 100 mL. Store in a brown bottle. section Reagents).
Dithizone TS—Dissolve 25.6 mg of dithizone in 100 mL of Fuchsin–Pyrogallol TS—Dissolve 100 mg of basic fuchsin in
alcohol. Store in a cold place, and use within 2 months. 50 mL of water that previously has been boiled for 15 min-
utes and allowed to cool slightly. Cool, add 2 mL of a satu-
Dragendorff’s TS—Mix 850 mg of bismuth subnitrate with rated solution of sodium bisulfite, mix, and allow to stand
40 mL of water and 10 mL of glacial acetic acid (Solution A). for not less than 3 hours. Add 0.9 mL of hydrochloric acid,
Dissolve 8 g of potassium iodide in 20 mL of water (Solution mix, and allow to stand overnight. Add 100 mg of pyrogal-
B). Mix equal portions of Solution A and Solution B to obtain lol, shake until solution is effected, and dilute with water to
a stock solution, which can be stored for several months in 100 mL. Store in an amber-colored glass bottle in a refriger-
a dark bottle. Mix 10 mL of the stock solution with 20 mL of ator.

Reagents
glacial acetic acid, and dilute with water to make 100 mL.
Fuchsin–Sulfurous Acid TS—Dissolve 200 mg of basic fuch-
Edetate Disodium TS—Dissolve 1 g of edetate disodium in sin in 120 mL of hot water, and allow the solution to cool.
950 mL of water, add 50 mL of alcohol, and mix. Add a solution of 2 g of anhydrous sodium sulfite in 20 mL
of water, then add 2 mL of hydrochloric acid. Dilute the
solution with water to 200 mL, and allow to stand for at
least 1 hour. Prepare this solution fresh.
Add the following:
Gastric Fluid, Simulated, TS—Dissolve 2.0 g of sodium
▲0.01 M Edetate Disodium TS—Transfer 100 mL of 0.1 M chloride and 3.2 g of purified pepsin, that is derived from
edetate disodium VS to a 1000-mL volumetric flask. Dilute porcine stomach mucosa, with an activity of 800 to 2500
with water to volume.▲USP40 units per mg of protein, in 7.0 mL of hydrochloric acid and
sufficient water to make 1000 mL. [NOTE—Pepsin activity is
Eosin Y TS (adsorption indicator)—Dissolve 50 mg of eosin described in the Food Chemicals Codex specifications under
Y in 10 mL of water. General Tests and Assays.] This test solution has a pH of
about 1.2.
Eriochrome Black TS—Dissolve 200 mg of eriochrome black
T and 2 g of hydroxylamine hydrochloride in methanol to Gelatin TS (for the assay of Corticotropin Injection)—Dissolve
make 50 mL. 340 g of acid-treated precursor gelatin (Type A) in water to
make 1000 mL. Heat the solution in an autoclave at 115°
Eriochrome Cyanine TS—Dissolve 750 mg of eriochrome for 30 minutes after the exhaust line temperature has
cyanine R in 200 mL of water, add 25 g of sodium chloride, reached 115°. Cool the solution, and add 10 g of phenol
25 g of ammonium nitrate, and 2 mL of nitric acid, and di- and 1000 mL of water. Store in tight containers in a refrig-
lute with water to 1000 mL. erator.
Fehling’s Solution—See Cupric Tartrate TS, Alkaline. Glacial Acetic Acid TS—See Acetic Acid, Glacial, TS.
Ferric Ammonium Sulfate TS—Dissolve 8 g of ferric ammo- Glucose Oxidase–Chromogen TS—A solution containing,
nium sulfate in water to make 100 mL. in each mL, 0.5 µmol of 4-aminoantipyrine, 22.0 µmol of
sodium p-hydroxybenzoate, not less than 7.0 units of glu-
Ferric Chloride TS—Dissolve 9 g of ferric chloride in water cose oxidase, and not less than 0.5 units of peroxidase, and
to make 100 mL. buffered to a pH of 7.0 ± 0.1.
SUITABILITY: When used for determining glucose in Inulin,
ascertain that no significant color results by reaction with

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2416 Test Solutions / Solutions USP 40

fructose, and that a suitable absorbance-versus-concentra- greenish tint develops in the solution. Then add 60% alco-
tion slope is obtained with glucose. hol to make 100 mL.
[NOTE—Glucose oxidase can be from Aspergillus niger.]
8-Hydroxyquinoline TS—Dissolve 5 g of 8-hydroxy-
Glycerin Base TS—To 200 g of glycerin add water to bring quinoline in alcohol to make 100 mL.
the total weight to 235 g. Add 140 mL of 1 N sodium hy-
droxide and 50 mL of water. Indigo Carmine TS (Sodium Indigotindisulfonate TS)—Dis-
solve a quantity of sodium indigotindisulfonate, equivalent
Gold Chloride TS—Dissolve 1 g of gold chloride in 35 mL to 180 mg of C16H8N2O2(SO3Na)2, in water to make 100 mL.
of water. Use within 60 days.
0.001 N Hydrochloric Acid TS—Transfer 1.0 mL of 1 N hy- Indophenol–Acetate TS (for the assay of Corticotropin Injec-
drochloric acid VS to a 1000-mL volumetric flask and dilute tion)—To 60 mL of standard dichlorophenol-indophenol so-
with water to volume. lution (see in the section Volumetric Solutions) add water to
make 250 mL. Add to the resulting solution an equal vol-
ume of sodium acetate solution freshly prepared by dissolv-
ing 13.66 g of anhydrous sodium acetate in water to make
Add the following: 500 mL and adjusting with 0.5 N acetic acid to a pH of 7.
Store in a refrigerator, and use within 2 weeks.
▲0.01 N Hydrochloric Acid TS—Transfer 100 mL of 0.1 N
hydrochloric acid VS to a 1000-mL volumetric flask. Dilute Intestinal Fluid, Simulated, TS—Dissolve 6.8 g of monoba-
with water to volume.▲USP40 sic potassium phosphate in 250 mL of water, mix, and add
77 mL of 0.2 N sodium hydroxide and 500 mL of water.
Add 10.0 g of pancreatin, mix, and adjust the resulting solu-
Add the following: tion with either 0.2 N sodium hydroxide or 0.2 N hydro-
chloric acid to a pH of 6.8 ± 0.1. Dilute with water to
▲0.025 N Hydrochloric Acid TS—Transfer 25 mL of 1 N hy- 1000 mL.
drochloric acid VS to a 1000-mL volumetric flask. Dilute
with water to volume.▲USP40 Iodine TS—Use 0.1 N Iodine (see in the section Volumetric
Solutions).
Iodine, Diluted TS: Transfer 10.0 mL of 0.1 N iodine VS to
Add the following: a 100-mL volumetric flask, dilute with water to volume, and
mix.
▲0.05 N Hydrochloric Acid TS—Transfer 4.1 mL of hydro-
chloric acid to a 1000-mL volumetric flask containing about Iodine Monochloride TS—Dissolve 10 g of potassium io-
500 mL of water. Cool and dilute with water to volume. dide and 6.44 g of potassium iodate in 75 mL of water in a
▲USP40 glass-stoppered container. Add 75 mL of hydrochloric acid
and 5 mL of chloroform, and adjust to a faint iodine color
0.06 N Hydrochloric Acid TS—Transfer 20.0 mL of 3 N hy- (in the chloroform) by adding dilute potassium iodide or
Reagents

drochloric acid TS to a 1000-mL volumetric flask. Dilute potassium iodate solution. If much iodine is liberated, use a
with water to volume. stronger solution of potassium iodate than 0.01 M at first,
making the final adjustment with the 0.01 M potassium io-
0.36 N Hydrochloric Acid TS—Transfer 120 mL of 3 N hy- date. Store in a dark place, and readjust to a faint iodine
drochloric acid TS to a 1000-mL volumetric flask. Dilute color as necessary.
with water to volume.
Iodine and Potassium Iodide TS 1—Dissolve 500 mg of io-
2 N Hydrochloric Acid TS—Transfer 17.0 mL of hydrochlo- dine and 1.5 g of potassium iodide in 25 mL of water.
ric acid to a 100-mL volumetric flask containing about
50 mL of water. Cool and dilute with water to volume. Iodine and Potassium Iodide TS 2—Dissolve 12.7 g of io-
dine and 20 g of potassium iodide in water, and dilute with
3 N Hydrochloric Acid TS—Transfer 246 mL of hydrochloric water to 1000.0 mL. To 10.0 mL of this solution, add 0.6 g
acid to a 1000-mL volumetric flask containing about 500 mL of potassium iodide, and dilute with water to 100.0 mL. Pre-
of water. Cool and dilute with water to volume. pare immediately before use.
6 N Hydrochloric Acid TS—Slowly transfer 49.8 mL of hy- Iodine and Potassium Iodide TS 3—Dissolve 0.127 g of io-
drochloric acid to a 100-mL volumetric flask containing dine and 0.20 g of potassium iodide in water, and dilute
about 45 mL of water. Cool and dilute with water to vol- with water to 10.0 mL.
ume.
Iodobromide TS—Dissolve 20 g of iodine monobromide in
Hydrogen Peroxide TS—Use Hydrogen Peroxide Topical Solu- glacial acetic acid to make 1000 mL. Store in glass contain-
tion (USP monograph). ers, protected from light.
Hydrogen Sulfide TS—A saturated solution of hydrogen Iodochloride TS—Dissolve 16.5 g of iodine monochloride in
sulfide, made by passing H2S into cold water. Store it in 1000 mL of glacial acetic acid.
small, dark amber-colored bottles, filled nearly to the top. It
is unsuitable unless it possesses a strong odor of H2S, and Iodoplatinate TS—Dissolve 300 mg of platinic chloride in
unless it produces at once a copious precipitate of sulfur 97 mL of water. Immediately prior to use, add 3.5 mL of
when added to an equal volume of ferric chloride TS. Store potassium iodide TS, and mix.
in a cold, dark place.
Iron–Phenol TS (Iron-Kober Reagent)—Dissolve 1.054 g of
Hydroxylamine Hydrochloride TS—Dissolve 3.5 g of hy- ferrous ammonium sulfate in 20 mL of water, and add 1 mL
droxylamine hydrochloride in 95 mL of 60% alcohol, and of sulfuric acid and 1 mL of 30 percent hydrogen peroxide.
add 0.5 mL of bromophenol blue solution (1 in 1000 of Mix, heat until effervescence ceases, and dilute with water
alcohol) and 0.5 N alcoholic potassium hydroxide until a to 50 mL. To 3 volumes of this solution contained in a volu-

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USP 40 Solutions / Test Solutions 2417

metric flask add sulfuric acid, with cooling, to make 100 Sodium Chloride 9.0 g
volumes. Purify phenol by distillation, discarding the first Potassium Chloride 0.42 g
10% and the last 5%, collecting the distillate, with exclusion Calcium Chloride 0.24 g
of moisture, in a dry, tared glass-stoppered flask of about
Magnesium Chloride 0.2 g
twice the volume of the phenol. Solidify the phenol in an
ice bath, breaking the top crust with a glass rod to ensure Sodium Bicarbonate 0.5 g
complete crystallization. Weigh the flask and its contents, Dextrose 0.5 g
add to the phenol 1.13 times its weight of the iron–sulfuric Water, recently distilled from a hard-glass
acid solution prepared as directed, insert the stopper in the flask, a sufficient quantity to make 1000 mL
flask, and allow to stand, without cooling but with occa-
sional mixing, until the phenol is liquefied. Shake the mix- Prepare fresh each day. The constituents (except the dex-
ture vigorously until mixed, allow to stand in the dark for trose and the sodium bicarbonate) may be made up in
16 to 24 hours, and again weigh the flask and its contents. stock solutions and diluted as needed.
To the mixture add 23.5% of its weight of a solution of 100
volumes of sulfuric acid in 110 volumes of water, mix, trans- Magnesia Mixture TS—Dissolve 5.5 g of magnesium chlo-
fer to dry glass-stoppered bottles, and store in the dark, ride and 7 g of ammonium chloride in 65 mL of water, add
protected from atmospheric moisture. Use within 6 months. 35 mL of ammonia TS, set the mixture aside for a few days
Dispense the reagent from a small-bore buret, arranged to in a well-stoppered bottle, and filter. If the solution is not
exclude moisture, capable of delivering 1 mL in 30 seconds perfectly clear, filter it before using.
or less, and having no lubricant, other than reagent, on its
stopcock. Wipe the buret tip with tissue before each addi- Magnesium Sulfate TS—Dissolve 12 g of crystals of magne-
tion. sium sulfate, selected for freedom from efflorescence, in
water to make 100 mL.
Iron Salicylate TS—Dissolve 500 mg of ferric ammonium
sulfate in 250 mL of water containing 10 mL of diluted sul- Malachite Green TS—Dissolve 1 g of malachite green oxa-
furic acid, and add water to make 500 mL. To 100 mL of late in 100 mL of glacial acetic acid.
the resulting solution add 50 mL of a 1.15% solution of so-
dium salicylate, 20 mL of diluted acetic acid, and 80 mL of a Mallory’s Stain—Dissolve 500 mg of water-soluble aniline
13.6% solution of sodium acetate, then add water to make blue, 2 g of orange G, and 2 g of oxalic acid in 100 mL of
500 mL. Store in a well-closed container. Protect from light. water.
Use within 2 weeks.
Mayer’s Reagent—See Mercuric–Potassium Iodide TS.
Lanthanum Nitrate TS—Dissolve 5.0 g of lanthanum nitrate
hexahydrate in 100 mL of water. Mercuric Acetate TS—Dissolve 6.0 g of mercuric acetate in
glacial acetic acid to make 100 mL. Store in tight containers,
Lead Acetate TS—Dissolve 9.5 g of clear, transparent crys- protected from direct sunlight.
tals of lead acetate in recently boiled water to make
100 mL. Store in well-stoppered bottles. Mercuric–Ammonium Thiocyanate TS—Dissolve 30 g of
ammonium thiocyanate and 27 g of mercuric chloride in
Lead Acetate TS, Alcoholic—Dissolve 2 g of clear, transpar- water to make 1000 mL.

Reagents
ent crystals of lead acetate in alcohol to make 100 mL. Store
in tight containers. Mercuric Bromide TS, Alcoholic—Dissolve 5 g of mercuric
bromide in 100 mL of alcohol, employing gentle heat to
Lead Nitrate Stock Solution TS—Dissolve 159.8 mg of lead facilitate solution. Store in glass containers, protected from
nitrate in 100 mL of water to which 1 mL of nitric acid has light.
been added, then dilute with water to 1000 mL. Prepare
and store this solution in glass containers free from soluble Mercuric Chloride TS—Dissolve 6.5 g of mercuric chloride
lead salts. in water to make 100 mL.

Lead Subacetate TS—Dissolve 40.0 g of lead acetate in Mercuric Iodide TS (Valser’s Reagent)—Slowly add potas-
90 mL of carbon dioxide-free water. Adjust with 10 M so- sium iodide solution (1 in 10) to red mercuric iodide until
dium hydroxide to a pH of 7.5, centrifuge, and use the clear almost all of the latter is dissolved, and filter off the excess.
supernatant. It contains NLT 16.7% (w/w) and NMT 17.4% A solution containing 10 g of potassium iodide in 100 mL
(w/w) of Pb in a form corresponding to the formula dissolves approximately 14 g of HgI2 at 20°.
C8H14O10Pb3. The solution remains clear when stored in a
well-closed container. Mercuric Nitrate TS—Dissolve 40 g of mercuric oxide (red
or yellow) in a mixture of 32 mL of nitric acid and 15 mL of
Lead Subacetate TS, Diluted—Dilute 3.25 mL of lead water. Store in glass containers, protected from light.
subacetate TS with water, recently boiled and cooled, to
make 100 mL. Store in small, well-filled, tight containers. Mercuric–Potassium Iodide TS (Mayer’s Reagent)—Dissolve
1.358 g of mercuric chloride in 60 mL of water. Dissolve 5 g
Litmus TS—Digest 25 g of powdered litmus with three suc- of potassium iodide in 10 mL of water. Mix the two solu-
cessive 100-mL portions of boiling alcohol, continuing each tions, and dilute with water to 100 mL.
extraction for about 1 hour. Filter, wash with alcohol, and
discard the alcohol filtrate. Macerate the residue with about Mercuric–Potassium Iodide TS, Alkaline (Nessler’s Rea-
25 mL of cold water for 4 hours, filter, and discard the fil- gent)—Dissolve 143 g of sodium hydroxide in 700 mL of
trate. Finally digest the residue with 125 mL of boiling water water. Dissolve 50 g of red mercuric iodide and 40 g of po-
for 1 hour, cool, and filter. tassium iodide in 200 mL of water. Pour the iodide solution
into the hydroxide solution, and dilute with water to
Locke-Ringer’s Solution—See Locke-Ringer’s TS. 1000 mL. Allow to settle, and use the clear supernatant.

Locke-Ringer’s TS (Locke-Ringer’s Solution) Mercuric Sulfate TS (Denigès’ Reagent)—Mix 5 g of yellow

mercuric oxide with 40 mL of water, and while stirring
slowly add 20 mL of sulfuric acid, then add another 40 mL
of water, and stir until completely dissolved.

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2418 Test Solutions / Solutions USP 40

Mercurous Nitrate TS—Dissolve 15 g of mercurous nitrate Add 5 mL more of the dilute nitric acid, and mix. Prepare
in a mixture of 90 mL of water and 10 mL of diluted nitric this solution fresh.
acid. Store in dark, amber-colored bottles in which a small
globule of mercury has been placed. Molybdo-phosphotungstate TS (Folin-Denis Reagent)—To
about 350 mL of water contained in a round-bottom flask
Metaphenylenediamine Hydrochloride TS—Dissolve 1 g of add 50 g of sodium tungstate, 12 g of phosphomolybdic
metaphenylenediamine hydrochloride in 200 mL of water. acid, and 25 mL of phosphoric acid. Boil the mixture under
The solution must be colorless when used. If necessary, de- a reflux condenser for 2 hours, then cool, dilute with water
colorize by heating with activated charcoal. to 500 mL, and mix. Store in tight containers, protected
from light, and in a cold place.
Metaphosphoric–Acetic Acids TS—Dissolve 15 g of meta-
phosphoric acid in 40 mL of glacial acetic acid and sufficient 1-Naphthol Reagent—Dissolve 1 g of 1-naphthol in 25 mL
water to make 500 mL. Store in a cold place, and use within of methanol. Prepare this solution fresh.
2 days.
1-Naphthol TS—Use 1-Naphthol Reagent.
Methoxyphenylacetic TS—Dissolve 2.7 g of methoxyphen-
ylacetic acid in 6 mL of Tetramethylammonium Hydroxide TS, 2-Naphthol TS (Betanaphthol TS)—Dissolve 1 g of 2-naph-
and add 20 mL of dehydrated alcohol. Store in a polyethyl- thol in 100 mL of sodium hydroxide solution (1 in 100).
ene container.
p-Naphtholbenzein TS—Dissolve 250 mg of p-naphthol-
Methyl Orange TS—Dissolve 100 mg of methyl orange in benzein in 100 mL of glacial acetic acid.
100 mL of water, and filter if necessary.
N-(1-Naphthyl)ethylenediamine Dihydrochloride TS—Dis-
Methyl Purple TS—Use Methyl Red–Methylene Blue TS. solve 100 mg of N-(1-naphthyl)ethylenediamine dihydro-
chloride in 100 mL of a mixture of 7 parts of acetone and
Methyl Red TS—Dissolve 100 mg of methyl red in 100 mL 3 parts of water.
of alcohol, and filter if necessary.
Nessler’s Reagent—See Mercuric–Potassium Iodide TS, Alka-
Methyl Red TS 2—To 1.86 mL of 0.1 M sodium hydroxide line.
and 50 mL of alcohol, add 50 mg of methyl red, and dilute
with water to 100 mL. Neutral Red TS—Dissolve 100 mg of neutral red in 100 mL
of 50% alcohol.
Methyl Red TS, Methanolic—Dissolve 1 g of methyl red in
100 mL of methanol, and filter, if necessary. Store protected Nickel Standard Solution TS—Dissolve 4.78 g of nickel (II)
from light, and use within 21 days. sulfate heptahydrate in water, and dilute with water to
1000 mL. Immediately prior to use, dilute 10.0 mL of the
Methyl Red–Methylene Blue TS—Add 10 mL of methyl red solution so obtained with water to 1000 mL. Suitable nickel
TS to 10 mL of methylene blue TS, and mix. standard solutions are also available commercially.
Methyl Violet TS—Use Crystal Violet TS. Ninhydrin TS—Use Triketohydrindene Hydrate TS.
Reagents

Methyl Yellow TS: Prepare a solution containing 0.10 mg 0.01 N Nitric Acid TS—Transfer 10.0 mL of 1 N nitric acid
per mL in alcohol. TS to a 1000-mL volumetric flask. Dilute with water to vol-
ume.
Methyl Yellow–Methylene Blue TS—Dissolve 1 g of methyl
yellow and 100 mg of methylene blue in 125 mL of metha- 0.2 N Nitric Acid TS—Slowly transfer 12.7 mL of nitric acid
nol. to a 1000-mL volumetric flask containing about 250 mL of
water. Cool and dilute with water to volume.
3-Methyl-2-benzothiazolinone Hydrazone Hydrochloride
TS—Dissolve 0.1 g of 3-methyl-2-benzothiazolinone 1 N Nitric Acid TS—Transfer 63.7 mL of nitric acid to a
hydrazone hydrochloride monohydrate in 10 mL of water, 1000-mL volumetric flask containing about 250 mL of water.
dilute the resulting solution with methanol to 100 mL, and Cool and dilute with water to volume.
mix.
2 N Nitric Acid TS—Transfer 12.74 mL of nitric acid slowly
Methylene Blue TS—Dissolve 125 mg of methylene blue in to a 100-mL volumetric flask containing about 40 mL of
100 mL of alcohol, and dilute with alcohol to 250 mL. water. Cool and dilute with water to volume.
Methylthionine Perchlorate TS—To 500 mL of potassium p-Nitroaniline TS—To 350 mg of p-nitroaniline add 1.5 mL
perchlorate solution (1 in 1000) add dropwise, with con- of hydrochloric acid, and mix. Dilute with water to 50 mL,
stant shaking, methylene blue solution (1 in 100) until a mix, and allow to settle. Place 5 mL of the clear supernatant
slight, permanent turbidity results. Allow the precipitate to in a 100-mL volumetric flask, and immerse it in an ice bath.
settle, decant the supernatant through paper, and use only While it is in the ice bath, add 1 mL of hydrochloric acid,
the clear solution. then add, in small portions, 2 mL of sodium nitrite solution
(1 in 100), dilute with water to volume, and mix.
Millon’s Reagent—To 2 mL of mercury in a conical flask
add 20 mL of nitric acid. Shake the flask under a hood to Nitrophenanthroline TS—Dissolve 150 mg of 5-nitro-1,10-
break up the mercury into small globules. After about phenanthroline in 15 mL of freshly prepared ferrous sulfate
10 minutes, add 35 mL of water, and, if a precipitate or solution (1 in 140).
crystals appear, add sufficient dilute nitric acid (1 in 5, pre-
pared from nitric acid from which the oxides have been Oracet Blue B TS—A 1 in 200 solution of oracet blue B in
removed by blowing air through it until it is colorless) to glacial acetic acid.
dissolve the separated solid. Add sodium hydroxide solution
(1 in 10) dropwise, with thorough mixing, until the curdy Orthophenanthroline TS—Dissolve 150 mg of
precipitate that forms after the addition of each drop no orthophenanthroline in 10 mL of a solution of ferrous sul-
longer redissolves but is dispersed to form a suspension. fate, prepared by dissolving 700 mg of ferrous sulfate in

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USP 40 Solutions / Test Solutions 2419

100 mL of water. The ferrous sulfate solution must be pre- Add the following:
pared immediately before dissolving the orthophenan-
throline. Store in well-closed containers. ▲0.06 M Phosphoric Acid TS—Transfer 4.2 mL of phos-
phoric acid to a volumetric flask containing about 500 mL of
Oxalic Acid TS—Dissolve 6.3 g of oxalic acid in water to water. Cool and dilute with water to volume.▲USP40
make 100 mL.
Palladium Chloride TS, Buffered—Weigh 500 mg of palla-
dium chloride into a 250-mL beaker, add 5 mL of concen- Add the following:
trated hydrochloric acid, and warm the mixture on a steam
bath. Add 200 mL of hot water in small increments with ▲1 N Phosphoric Acid TS—To a 1000-mL volumetric flask
continued heating until solution is complete. Transfer the containing about 800 mL of water, slowly add 22.8 mL of
solution to a 250-mL volumetric flask, and dilute with water phosphoric acid. Cool and dilute with water to volume.▲USP40
to volume. Transfer 50 mL to a 100-mL volumetric flask.
Add 10 mL of 1 M sodium acetate and 9.6 mL of 1 N hy- 10% Phosphoric Acid TS—Transfer 7 mL of phosphoric acid
drochloric acid. Dilute with water to volume. to a 100-mL volumetric flask containing about 50 mL of
water. Cool and dilute with water to volume.
Perchloric Acid TS—Dilute 8.5 mL of perchloric acid with
water to 100 mL.
Phenol TS—Dissolve 1.2 g of phenol in alcohol to make Add the following:
10 mL. Prepare weekly. ▲20% Phosphoric Acid TS—Transfer 14 mL of phosphoric
Phenol Red TS (Phenolsulfonphthalein TS)—Dissolve 100 mg acid to a 100-mL volumetric flask containing about 50 mL
of phenolsulfonphthalein in 100 mL of alcohol, and filter if of water. Cool and dilute with water to volume.▲USP40
necessary.
Phosphotungstic Acid TS—Dissolve 1 g of phosphotungstic
pH 4.7 Phenol Red TS—Dissolve 33 mg of phenolsulfon- acid in water to make 100 mL.
phthalein in 1.5 mL of 2 N sodium hydroxide solution, di-
lute with water to 100 mL, and mix (Solution A). Dissolve Picrate TS, Alkaline—Mix 20 mL of trinitrophenol solution
25 mg of ammonium sulfate in 235 mL of water, add (1 in 100) with 10 mL of sodium hydroxide solution (1 in
105 mL of 2 N sodium hydroxide solution and 135 mL of 20), dilute with water to 100 mL, and mix. Use within 2
2 N acetic acid, and mix (Solution B). Add 25 mL of Solution days.
A to Solution B, and mix. If necessary, adjust the pH of this
solution to 4.7. Picric Acid TS—See Trinitrophenol TS.

Phenoldisulfonic Acid TS—Dissolve 2.5 g of phenol in Platinic Chloride TS—Dissolve 2.6 g of platinic chloride in
15 mL of sulfuric acid in a flask of suitable capacity. Add water to make 20 mL.
7.5 mL of fuming sulfuric acid, stir well, and heat at 100°
for 2 hours. Transfer the product, while still fluid, to a glass- Platinum–Cobalt TS—Dissolve 1.246 g of potassium

Reagents
stoppered bottle, and, when desired for use, warm in a chloroplatinate (K2PtCl6) and 1.000 g of cobalt chloride
water bath until liquefied. (CoCl2 · 6H2O) in water, add 100 mL of hydrochloric acid,
and dilute with water to 1 L.
Phenolphthalein TS—Dissolve 1 g of phenolphthalein in
100 mL of alcohol. Potassium Acetate TS—Dissolve 10 g of potassium acetate
in water to make 100 mL.
Phenylhydrazine Acetate TS—Dissolve 10 mL of phenylhy-
drazine and 5 mL of glacial acetic acid in water to make Potassium–Bismuth Iodide TS—Dissolve 12.5 g of tartaric
100 mL. acid in 25 mL of water, then dissolve 1.06 g of bismuth sub-
nitrate in this mixture (Solution A). Dissolve 20 g of potas-
Phenylhydrazine–Sulfuric Acid TS—Dissolve 65 mg of phe- sium iodide in 25 mL of water (Solution B). Dissolve 100 g of
nylhydrazine hydrochloride in 100 mL of a cooled mixture tartaric acid in 450 mL of water (Solution C). Add Solutions A
of equal volumes of sulfuric acid and water. and B to Solution C, and mix.

Phloroglucinol TS—Dissolve 500 mg of phloroglucinol in Potassium Carbonate TS—Dissolve 7 g of anhydrous potas-

25 mL of alcohol. Store in tight containers, protected from sium carbonate in water to make 100 mL.
light.
Potassium Chromate TS—Dissolve 10 g of potassium chro-
Phosphatic Enzyme TS—Dissolve 5 g of phosphatic enzyme mate in water to make 100 mL.
in water to make 50 mL. Prepare this solution fresh.
Potassium Dichromate TS—Dissolve 7.5 g of potassium
Phosphomolybdic Acid TS—Dissolve 20 g of phosphomo- dichromate in water to make 100 mL.
lybdic acid in alcohol to make 100 mL. Filter the solution,
and use only the clear filtrate. Potassium Ferricyanide TS—Dissolve 1 g of potassium ferri-
cyanide in 10 mL of water. Prepare this solution fresh.
Potassium Ferrocyanide TS—Dissolve 1 g of potassium fer-
Add the following: rocyanide in 10 mL of water. Prepare this solution fresh.
▲0.05 M Phosphoric Acid TS—Transfer 3.4 mL of phos- Potassium Hydroxide TS—Dissolve 6.5 g of potassium hy-
phoric acid to a 1000-mL volumetric flask containing about droxide in water to make 100 mL.
500 mL of water. Cool and dilute with water to volume.
▲USP40

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2420 Test Solutions / Solutions USP 40

Add the following: Potassium Thiocyanate TS: Dissolve 9.7 g of potassium

thiocyanate in water to make 100 mL.
▲ 1.8 N Potassium Hydroxide TS—Dissolve 101 g of potas-
sium hydroxide in about 800 mL of water. Cool and dilute Pyridine–Pyrazolone TS—To 100 mL of a saturated solution
with water to 1000 mL.▲USP40 of 1-phenyl-3-methyl-2-pyrazoline-5-one add 20 mL of a 1
in 1000 solution of 3,3′-dimethyl-1,1′-diphenyl-[4,4′-bi-
2 N Potassium Hydroxide TS—Dissolve 112.2 g of potas- 2-pyrazoline]-5,5′-dione in pyridine. Store in a dark bottle,
sium hydroxide in about 800 mL of water. Cool and dilute and use within 3 days.
with water to 1000 mL.
Pyrogallol TS, Alkaline—Dissolve 500 mg of pyrogallol in
2 mL of water. Dissolve 12 g of potassium hydroxide in
8 mL of water. The solutions should be freshly prepared and
Add the following: mixed immediately before use.
▲ 45% Potassium Hydroxide TS—Transfer 53 g of potassium Quinaldine Red TS—Dissolve 100 mg of quinaldine red in
hydroxide to a 100-mL volumetric flask. Dissolve in and di- 100 mL of alcohol.
lute with water to volume.▲USP40
Quinone TS—Dissolve 500 mg of p-benzoquinone in 2.5 mL
Potassium Hydroxide TS, Alcoholic—Use 0.5 N Potassium of glacial acetic acid, and dilute with alcohol to 50 mL. Pre-
Hydroxide, Alcoholic (see in the section Volumetric Solutions). pare this solution fresh daily.
Potassium Hydroxide TS 2, Alcoholic—Dissolve 130 g of Resorcinol TS—Dissolve 1 g of resorcinol in hydrochloric
potassium hydroxide, with cooling, in 200 mL of water. Add acid to make 100 mL.
alcohol to 1000 mL. Store in a well-stoppered dark glass
bottle. Ruthenium Red TS—Dissolve 10 g of lead acetate in water,
dilute with water to 100 mL, and add 80 mg of ruthenium
Potassium Iodide TS—Dissolve 16.5 g of potassium iodide red. The solution is wine-red in color. [NOTE—If necessary,
in water to make 100 mL. Store in light-resistant containers. add additional ruthenium red to obtain a wine-red color.]
20% Potassium Iodide TS—Transfer 20 g of potassium io- Saline TS—Dissolve 9.0 g of sodium chloride in water to
dide to a 100-mL volumetric flask. Dissolve in and dilute make 1000 mL.
with water to volume. [NOTE—Where pyrogen-free saline TS is specified in this
Pharmacopeia, saline TS that has met the requirements of
Potassium Iodide and Starch TS: Dissolve 0.75 g of po- the Pyrogen Test 〈151〉 is to be used.]
tassium iodide in 100 mL of water. Heat to boiling, and
add, with stirring, a solution of 0.5 g of soluble starch in Saline TS, Pyrogen-Free—See Saline TS.
35 mL of water. Boil for 2 minutes, and allow to cool.
SENSITIVITY: Mix 15 mL in 0.05 mL of glacial acetic acid Schweitzer’s Reagent—See Cupric Oxide, Ammoniated, TS.
and 0.3 mL of diluted iodine TS: a blue color is produced.
Silver–Ammonia–Nitrate TS—Dissolve 1 g of silver nitrate
Reagents

Potassium Iodoplatinate TS—Dissolve 200 mg of platinic in 20 mL of water. Add ammonia TS, dropwise, with con-
chloride in 2 mL of water, mix with 25 mL of potassium stant stirring, until the precipitate is almost but not entirely
iodide solution (1 in 25), and add water to make 50 mL. dissolved. Filter, and store in tight, light-resistant containers.

Potassium Permanganate TS—Use 0.1 N Potassium Per- Silver–Ammonium Nitrate TS—See Silver–Ammonia–Nitrate
manganate (see in the section Volumetric Solutions). TS.
Silver Diethyldithiocarbamate TS—Dissolve 1 g of silver
diethyldithiocarbamate in 200 mL of pyridine from a freshly
Add the following: opened bottle or that which has been recently distilled.
Store in light-resistant containers, and use within 30 days.
▲0.02 M Monobasic Potassium Phosphate TS—Transfer
2.72 g of monobasic potassium phosphate to a 1000-mL Silver Nitrate TS—Use 0.1 N Silver Nitrate (see in the sec-
volumetric flask. Dissolve in and dilute with water to vol- tion Volumetric Solutions).
ume.▲USP40
Simulated Gastric Fluid TS—See Gastric Fluid, Simulated, TS.

Add the following: Simulated Intestinal Fluid TS—See Intestinal Fluid, Simu-
lated, TS.
▲ 0.2 M Dibasic Potassium Phosphate TS—Transfer 34.83 g
of dibasic potassium phosphate to a 1000-mL volumetric Sodium Acetate TS—Dissolve 13.6 g of sodium acetate in
flask. Dissolve in and dilute with water to volume.▲USP40 water to make 100 mL.

Potassium Pyroantimonate TS—Dissolve 2 g of potassium Sodium Alizarinsulfonate TS—Dissolve 100 mg of sodium

pyroantimonate in 85 mL of hot water. Cool quickly, and alizarinsulfonate in 100 mL of water, and filter.
add 50 mL of a solution containing 50 mg/mL of potassium
hydroxide in water and 1 mL of sodium hydroxide solution Sodium Aminoacetate TS (Sodium Glycinate TS)—Dissolve
(8.5 in 100). Allow to stand for 24 h, filter, and dilute with 3.75 g of aminoacetic acid in about 500 mL of water, add
water to 150 mL. 2.1 g of sodium hydroxide, and dilute with water to
1000 mL. Mix 9 mL of the resulting solution with 1 mL of
Potassium Sulfate TS—Dissolve 1 g of potassium sulfate in dilute glacial acetic acid (1 in 300). This test solution has a
water to make 100 mL. pH between 10.4 and 10.5.
Sodium Bisulfite TS—Dissolve 10 g of sodium bisulfite in
water to make 30 mL. Prepare this solution fresh.

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USP 40 Solutions / Test Solutions 2421

Sodium Bitartrate TS—Dissolve 1 g of sodium bitartrate in Add the following:

water to make 10 mL. Prepare this solution fresh.
▲10 N Sodium Hydroxide TS—Transfer 400 g of sodium hy-
Sodium Carbonate TS—Dissolve 10.6 g of anhydrous so- droxide to a 1000-mL volumetric flask, and dissolve in about
dium carbonate in water to make 100 mL. 800 mL of water. Cool and dilute with water to volume.
▲USP40
Sodium Chloride TS, Alkaline—Dissolve 2 g of sodium hy-
droxide in 100 mL of water, saturate the solution with so- Sodium Hydroxide TS 2—Transfer 8.5 g of sodium hydrox-
dium chloride, and filter. ide to a 100-mL volumetric flask, and dissolve in and dilute
with water to volume.
Sodium Citrate TS—Dissolve 73.5 g of sodium citrate dihy-
drate in water to make 250 mL. Sodium Hydroxide TS 3—Prepare a 420-mg/mL solution of
sodium hydroxide in water.
Sodium Citrate TS, Alkaline—Dissolve 50 g of sodium cit-
rate dihydrate and 2.5 g of sodium hydroxide in water to Sodium Hypobromite TS—To a solution of 20 g of sodium
make 250 mL. hydroxide in 75 mL of water add 5 mL of bromine. After
solution has taken place, dilute with water to 100 mL. Pre-
Sodium Cobaltinitrite TS—Dissolve 10 g of sodium cobal- pare this solution fresh.
tinitrite in water to make 50 mL, and filter if necessary.
Sodium Hypochlorite TS—Use Sodium Hypochlorite Solution
Sodium Fluoride TS—Dry about 500 mg of sodium fluoride (see in the section Reagent Specifications).
at 200° for 4 hours. Accurately weigh 222 mg of the dried
material, and dissolve in water to make 100.0 mL. Pipet Sodium Iodohydroxyquinolinesulfonate TS—Dissolve 8.8 g
10 mL of this solution into a 1-L volumetric flask, and dilute of iodohydroxyquinoline sulfonic acid in 200 mL of water,
with water to volume. Each mL of this solution corresponds and add 6.5 mL of 4 N sodium hydroxide. Dilute with water
to 0.01 mg of fluorine (F). to 250 mL, mix, and filter.
Sodium Hydrosulfite TS, Alkaline—Dissolve 25 g of potas- Sodium Nitroferricyanide TS—Dissolve 1 g of sodium ni-
sium hydroxide in 35 mL of water, and 50 g of sodium hy- troferricyanide in water to make 20 mL. Prepare this solution
drosulfite in 250 mL of water. When the test solution is re- fresh.
quired, mix 40 mL of the hydroxide solution with the
250 mL of the hydrosulfite solution. Prepare this solution Dibasic Sodium Phosphate TS—Dissolve 12 g of dibasic so-
fresh. dium phosphate in water to make 100 mL.
Sodium Hydroxide TS—Dissolve 4.0 g of sodium hydroxide Sodium Phosphotungstate TS—To a solution of 20 g of so-
in water to make 100 mL. dium tungstate in 100 mL of water add sufficient phos-
phoric acid to impart a strongly acid reaction to litmus, and
filter. When required for use, decant the clear solution from
Add the following: any sediment that may be present. Store in tight, light-resis-
tant containers.

Reagents
▲ 0.0025 N Sodium Hydroxide TS—Transfer 12.5 mL of 0.2
N sodium hydroxide TS to a 1000-mL volumetric flask. Di- Sodium Sulfide TS—Dissolve 1 g of sodium sulfide in water
lute with water to volume.▲USP40 to make 10 mL. Prepare this solution fresh.
Sodium Tartrate TS—Dissolve 11.5 g of sodium tartrate in
water to make 100 mL.
Add the following:
Sodium Tetraphenylboron TS—Dissolve 1.2 g of sodium
▲0.02 N Sodium Hydroxide TS—Transfer 10 mL of 2 N so- tetraphenylboron in water to make 200 mL. If necessary, stir
dium hydroxide TS to a 1000-mL volumetric flask. Dilute for 5 minutes with 1 g of aluminum oxide, and filter to clar-
with water to volume.▲USP40 ify.
0.2 N Sodium Hydroxide TS—Transfer 10.0 mL of 2 N so- Sodium Thioglycolate TS—Dissolve 1.5 g of sodium thiog-
dium hydroxide TS to a 100-mL volumetric flask and dilute lycolate in 450 mL of water, and add 50 mL of alcohol. Use
with water to volume. within 3 days.
Sodium Thiosulfate TS—Use 0.1 N Sodium Thiosulfate (see
in the section Volumetric Solutions).
Add the following:
Standard Lead Solution TS: On the day of use, dilute
▲2 N Sodium Hydroxide TS—Dissolve 80 g of sodium hy- 10.0 mL of lead nitrate stock solution TS with water to
droxide in about 800 mL of water. Cool and dilute with 100.0 mL. Each mL of standard lead solution TS contains
water to 1000 mL.▲USP40 the equivalent to 10 µg of lead.
Stannous Chloride, Acid, TS—Dissolve 8 g of stannous
Add the following: chloride in 500 mL of hydrochloric acid. Store in glass con-
tainers, and use within 3 months.
▲2.5 N Sodium Hydroxide TS—Dissolve 100 g of sodium
hydroxide in about 800 mL of water. Cool and dilute with Stannous Chloride, Acid, Stronger, TS—Dissolve 40 g of
water to 1000 mL.▲USP40 stannous chloride in 100 mL of hydrochloric acid. Store in
glass containers, and use within 3 months.
5 N Sodium Hydroxide TS—Transfer 20 g of sodium hy-
droxide to a 100-mL volumetric flask. Dissolve in about Starch TS—Mix 1 g of soluble starch with 10 mg of red
80 mL of water. Cool and dilute with water to volume. mercuric iodide and sufficient cold water to make a thin

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2422 Test Solutions / Solutions USP 40

paste. Add 200 mL of boiling water, and boil for 1 minute be checked frequently and solutions assaying more than
with continuous stirring. Cool, and use only the clear solu- 95.5% or less than 94.5% discarded.]
tion. [NOTE—Commercially available, stabilized starch indi-
cator solutions may be used, including mercury-free solu-
tions preserved with other compounds such as salicylic
acid.] Add the following:

Starch, Iodide-Free, TS—Mix 1 g of soluble starch with suf-

▲1 M Sulfuric Acid TS—Transfer 56.1 mL of sulfuric acid to
ficient cold water to make a thin paste. While stirring, add a 1000-mL volumetric flask containing about 500 mL of
100 mL of boiling water, and allow to cool. Prepare this water. Cool and dilute with water to volume.▲USP40
solution immediately before use. Iodide-free starch TS shows
a blue color when 20 mL of potassium iodide solution (1 in 0.02 N Sulfuric Acid TS—Transfer 2.9 mL of 7 N sulfuric
400) and 0.05 mL of an iodine–potassium iodide solution acid TS to a 1000-mL volumetric flask and dilute with water
(prepared by dissolving 127 mg of iodine and 800 mg of to volume.
potassium iodide in water and diluting with water to
100 mL) are added to 1 mL of the iodide-free starch TS.
Add the following:
Starch Iodide Paste TS—Heat 100 mL of water in a 250-mL
beaker to boiling, add a solution of 0.75 g of potassium ▲0.2 N Sulfuric Acid TS—Transfer 5.6 mL of sulfuric acid to
iodide in 5 mL of water, then add 2 g of zinc chloride dis- a 1000-mL volumetric flask containing about 500 mL of
solved in 10 mL of water, and, while the solution is boiling, water. Cool and dilute with water to volume.▲USP40
add, with stirring, a smooth suspension of 5 g of soluble
starch in 30 mL of cold water. Continue to boil for 2 min-
utes, then cool. Store in well-closed containers in a cold
place. Add the following:
Starch iodide paste TS must show a definite blue streak
when a glass rod, dipped in a mixture of 1 mL of 0.1 M ▲0.5 N Sulfuric Acid TS—Transfer 14 mL of sulfuric acid to
sodium nitrite, 500 mL of water, and 10 mL of hydrochloric a 1000-mL volumetric flask containing about 500 mL of
acid, is streaked on a smear of the paste. water. Cool and dilute with water to volume.▲USP40
Starch–Potassium Iodide TS—Dissolve 500 mg of potas-
sium iodide in 100 mL of freshly prepared starch TS. Prepare
this solution fresh. Add the following:

Stronger Cupric Acetate TS—See Cupric Acetate TS,

▲2 N Sulfuric Acid TS—Transfer 56.2 mL of sulfuric acid to a
Stronger. 1000-mL volumetric flask containing about 500 mL of water.
Cool and dilute with water to volume.▲USP40
Sudan III TS—Dissolve 0.05 g of Sudan III in 25 mL of alco-
hol, with warming if necessary. Cool, add 25 mL of glycerin, 6 N Sulfuric Acid TS—Slowly transfer 168.5 mL of sulfuric
and mix. Filter if undissolved material persists. acid to a 1000-mL volumetric flask containing about 500 mL
Reagents

of water. Cool and dilute with water to volume.

Sudan IV TS—Dissolve 0.5 g of Sudan IV in chloroform to
make 100 mL. 7 N Sulfuric Acid TS—Slowly transfer 196.5 mL of sulfuric
acid to a 1000-mL volumetric flask containing about 500 mL
Sulfanilic Acid TS—Dissolve 800 mg of sulfanilic acid in of water. Cool and dilute with water to volume.
100 mL of acetic acid. Store in tight containers.
Sulfuric Acid–Formaldehyde TS—Add 1 drop of formalde-
Diazotized Sulfanilic Acid TS—Dissolve 0.9 g of sulfanilic hyde TS to each mL of sulfuric acid, and mix. Prepare this
acid in 9 mL of hydrochloric acid with warming, and dilute solution fresh.
with water to 100 mL. Cool 10 mL of this solution in iced
water, and add 10 mL of a sodium nitrite solution (4.5 in Tannic Acid TS—Dissolve 1 g of tannic acid in 1 mL of alco-
100) previously cooled in iced water. Allow to stand at 0° hol, and dilute with water to 10 mL. Prepare this solution
for at least 15 minutes (the solution may be kept for 3 days fresh.
at this temperature). Immediately before use, add 20 mL of
sodium carbonate solution (1 in 10). Tartaric Acid TS—Dissolve 3 g of tartaric acid in water to
make 10 mL. Prepare this solution fresh.
Sulfanilic-1-Naphthylamine TS—Dissolve 500 mg of sulfan-
ilic acid in 150 mL of acetic acid. Dissolve 100 mg of Tetrabromophenolphthalein Ethyl Ester TS—Dissolve
1-naphthylamine hydrochloride in 150 mL of acetic acid, 100 mg of tetrabromophenolphthalein ethyl ester in 90 mL
and mix the two solutions. The pink color that may develop of glacial acetic acid, and dilute with glacial acetic acid to
on standing can be removed by treatment with zinc. 100 mL. Prepare this solution fresh.

Sulfanilic-α-Naphthylamine TS—See Sulfanilic-1-Naphthyl-

amine TS. Add the following:
Sulfomolybdic Acid TS—Dissolve, with the aid of heat, ▲0.02 M Tetrabutylammonium Hydrogen Sulfate TS—
2.5 g of ammonium molybdate in 20 mL of water, add Transfer 6.79 g of tetrabutylammonium hydrogen sulfate to
50 mL of 12 N sulfuric acid, and dilute with water to a 1000-mL volumetric flask. Dissolve in and dilute with
100 mL. Store this solution in a polyethylene container. water to volume.▲USP40
Sulfuric Acid TS—Add a quantity of sulfuric acid of known Tetramethylammonium Hydroxide TS—Use an aqueous
concentration to sufficient water to adjust the final concen- solution containing, in each 100 mL, the equivalent of 10 g
tration to between 94.5% and 95.5% (w/w) of H2SO4. of anhydrous tetramethylammonium hydroxide.
[NOTE—Since the acid concentration may change upon
standing or upon intermittent use, the concentration should

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USP 40 Solutions / Volumetric Solutions 2423

Thioacetamide TS—Dissolve 4 g of thioacetamide in 0.02 N = fiftieth normal

100 mL of water. 0.01 N = hundredth-normal
0.001 N = thousandth-normal
Thioacetamide–Glycerin Base TS—Mix 0.2 mL of thioacet- 1.2 Molar solutions: Molar solutions are solutions that
amide TS and 1 mL of glycerin base TS, and heat in a boil- contain 1 gram-molecule of the compound in 1 L of
ing water bath for 20 seconds. Use the mixture immediately. solution.
Thorium Nitrate TS—Dissolve 1 g of thorium nitrate in M = mol/L
water to make 100 mL. Filter, if necessary.
Thymol Blue TS—Dissolve 100 mg of thymol blue in M = weight (g)/mol weight × L
100 mL of alcohol, and filter if necessary.
Solutions containing one-tenth of a gram-molecule of the
Thymolphthalein TS—Dissolve 100 mg of thymolphthalein compound in 1 L are designated tenth-molar, 0.1 M; and
in 100 mL of alcohol, and filter if necessary. other molarities are similarly indicated.
1.3 Correction factor: It is frequently difficult to prepare
Titanium Trichloride TS—Dissolve 15 g of titanium trichlo- standard solutions of a desired theoretical normality or mo-
ride in 100 mL of 10% hydrochloric acid solution. larity, and this is not essential. A solution of approximately
the desired normality or molarity is prepared and standard-
Titanium Trichloride–Sulfuric Acid TS—Mix carefully 20 mL ized by titration against a standard. The correction factor so
of titanium trichloride TS in 13 mL of sulfuric acid. Add suffi- obtained is used in all calculations where such solutions are
cient 30% hydrogen peroxide to produce a yellow color. used. If necessary, the concentration of the solution may be
Heat until white fumes are evolved, allow to cool, and dilute adjusted to a given normality or molarity, by dilution or by
with water. Repeat the evaporation and addition of water addition of the appropriate reagent.
until a colorless solution is obtained. Dilute with water to The concentration of the volumetric solution does not dif-
100 mL. fer from the prescribed one by more than 10%. The correc-
tion factor is determined by an appropriate number of repli-
p-Toluenesulfonic Acid TS—Dissolve 2 g of p- cates. The repeatability does not exceed 0.2% (relative
toluenesulfonic acid in 10 mL of a mixture of 7 parts of ace- standard deviation). The correction factor should be redeter-
tone and 3 parts of water. mined frequently.
1.4 Blank determinations: Where it is directed that “any
Triketohydrindene Hydrate TS (Ninhydrin TS)—Dissolve necessary correction” be made by a blank determination,
200 mg of triketohydrindene hydrate in water to make the determination is to be conducted with the use of the
10 mL. Prepare this solution fresh. same quantities of the same reagents treated in the same
manner as the solution or mixture containing the portion of
Trinitrophenol TS (Picric Acid TS)—Dissolve the equivalent the substance under assay or test, but with the substance
of 1 g of anhydrous trinitrophenol in 100 mL of hot water. itself omitted.
Cool the solution, and filter if necessary.
Triphenyltetrazolium Chloride TS—Dissolve 500 mg of 2. PREPARATION AND STANDARDIZATION

Reagents
triphenyltetrazolium chloride in dehydrated alcohol to make
100 mL. 2.1 Scope
When solutions of a reagent are used in different concen-
Xylenol Orange TS—Dissolve 100 mg of xylenol orange in trations, the details of the preparation and standardization
100 mL of alcohol. are usually given for the concentration most frequently re-
quired. Stronger or weaker solutions are prepared and stan-
Zinc Uranyl Acetate TS—Dissolve 50 g of uranyl acetate in dardized in the same general manner as described, using
a mixture of 15 mL of glacial acetic acid and water to make proportionate amounts of the reagent.
500 mL. Then dissolve 150 g of zinc acetate in a mixture of 2.2 Preparation by dilution
15 mL of glacial acetic acid and water to make 500 mL. Mix It is possible in many instances to prepare lower concen-
the two solutions, allow to stand overnight, and pass trations accurately by making an exact dilution of a stronger
through a dry filter, if necessary. solution.
Volumetric solutions prepared by dilution should be
restandardized as directed for the stronger solution, using
VOLUMETRIC SOLUTIONS proportionate amounts of reagents.
Dilute solutions that are not stable, as, for instance, potas-
sium permanganate 0.01 N, are preferably prepared by ex-
1. DEFINITIONS actly diluting the higher normality with thoroughly boiled
and cooled water on the same day they are required for
1.1 Normal solutions: Normal solutions are solutions that use.
contain 1 gram equivalent weight of the compound in 1 L 2.3 Standardization
of solution. The following directions give only one method for stan-
dardization, but other methods of standardization, capable
N = equivalent/L of yielding at least the same degree of accuracy, may be
used.
The values obtained in the standardization of volumetric
N = weight (g)/equivalent weight (g) × L solutions are valid for all Pharmacopeial uses of these solu-
tions, regardless of the instrumental or chemical indicators
Normal solutions and solutions bearing a specific relation- used in the individual monographs.
ship to normal solutions, and used in volumetric determina- Where the apparent normality or molarity of a titrant de-
tions, are designated as follows: pends upon the special conditions of its use, the individual
1 N = normal monograph sets forth the directions for standardizing the
2 N = double normal reagent in the specified context.
0.5 N = half-normal For those salts that usually are available as certified pri-
0.1 N = tenth-normal mary standards or that are available as highly purified salts

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