美国药典USP32测试溶液配制.doc

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1、wordTEST SOLUTIONS (TS) Certain of the following test solutions are intended for use as acid-base indicators in volumetric analyses. Such solutions should be so adjusted that when 0.15 mL of the indicator solution is added to 25 mL of carbon dioxide-free water, 0.25 mL of 0.02 N acid or alkali, resp

2、ectively, will produce the characteristic color change. Similar solutions are intended for use in pH measurement. Where no special directions for their preparation are given, the same solution is suitable for both purposes.Where it is directed that a volumetric solution be used as the test solution,

3、 standardization of the solution used as TS is not required.In general, the directive to prepare a solution “fresh” indicates that the solution is of limited stability and must be prepared on the day of use.For the preparation of Test Solutions, use reagents of the quality described under Reagents.

4、Acetaldehyde TS Mix 4 mL of acetaldehyde, 3 mL of alcohol, and 1 mL of water. Prepare this solution fresh. Acetate Buffer TS Dissolve 320 g of ammonium acetate in 500 mL of water, add 5 mL of glacial acetic acid, dilute with water to 1000.0 mL, and mix. This solution has a pH between 5.9 and 6.0. Ac

5、etic Acid, Glacial, TS Determine the water content of a specimen of glacial acetic acid by the Titrimetric Method (see Water Determination 921). If the acid contains more than 0.05% of water, add a few mL of acetic anhydride, mix, allow to stand overnight, and again determine the water content. If t

6、he acid contains less than 0.02% of water, add sufficient water to make the final concentration between 0.02% and 0.05%, mix, allow to stand overnight, and again determine the water content. Repeat the adjustment with acetic anhydride or water, as necessary, until the resulting solution shows a wate

7、r content between 0.02% and 0.05%. Acetic Acid, Strong, TS Add 300.0 mL of glacial acetic acid, and dilute with water to 1000 mL. This solution contains about 30% (v/v) of CH3COOH and has a concentration of about 5 N. Acetic AcidAmmonium Acetate Buffer TS Dissolve 77.1 g of ammonium acetate in water

8、, add 57 mL of glacial acetic acid, and dilute with water to 1000 mL. Acetone, Buffered, TS Dissolve 8.15 g of sodium acetate and 42 g of sodium chloride in about 100 mL of water, and add 68 mL of 0.1 N hydrochloric acid and 150 mL of acetone. Mix, and dilute with water to 500 mL. Acid Ferric Chlori

9、de TS Mix 60 mL of glacial acetic acid with 5 mL of sulfuric acid, add 1 mL of ferric chloride TS, mix, and cool. Acid Ferrous Sulfate TS See Ferrous Sulfate, Acid, TS.Acid Stannous Chloride TS See Stannous Chloride, Acid, TS.Acid Stannous Chloride TS, Stronger See Stannous Chloride, Acid, TS.Albume

10、n TS Carefully separate the white from the yolk of a strictly fresh hens egg. Shake the white with 100 mL of water until mixed and all but the chalaza has undergone solution; then filter. Prepare the solution fresh. AlcoholPhenol TS Dissolve 780 mg of phenol in alcohol to make 100 mL. Alcoholic Ammo

11、nia TS See Ammonia TS, Alcoholic. Alcoholic Mercuric Bromide TS See Mercuric Bromide TS, Alcoholic. Alcoholic Potassium Hydroxide TS See Potassium Hydroxide TS, Alcoholic. Alkaline Cupric Citrate TS See Cupric Citrate TS, Alkaline. Alkaline Cupric Citrate TS 2 See Cupric Citrate TS 2, Alkaline. Alka

12、line Cupric Iodide TS See Cupric Iodide TS, Alkaline. Alkaline Cupric Tartrate TS (Fehlings Solution)See Cupric Tartrate TS, Alkaline. Alkaline MercuricPotassium Iodide TS See MercuricPotassium Iodide TS, Alkaline. Alkaline Picrate TS See Picrate TS, Alkaline. Alkaline Sodium Hydrosulfite TS See Sod

13、ium Hydrosulfite TS, Alkaline. Amaranth TS Dissolve 20 mg of amaranth in 10 mL of water. Aminonaphtholsulfonic Acid TS Accurately weigh 5 g of sodium sulfite, 94.3 g of sodium bisulfite, and 700 mg of 1,2,4-aminonaphtholsulfonic acid, and mix. Prepare aminonaphtholsulfonic acid TS fresh on the day o

14、f use by dissolving 1.5 g of the dry mixture in 10 mL of water. AmmoniaAmmonium Chloride Buffer TS Dissolve 67.5 g of ammonium chloride in water, add 570 mL of ammonium hydroxide, and dilute with water to 1000 mL. AmmoniaCyanide TS Dissolve 2 g of potassium cyanide in 15 mL of ammonium hydroxide, an

15、d dilute with water to 100 mL. Ammonia TS It contains between 9.5% and 10.5% of NH3. Prepare by diluting 350 mL of Ammonia Water, Stronger (see in the section, Reagents) with water to make 1000 mL. Ammonia TS, Alcoholic A solution of ammonia gas in alcohol. Clear, colorless liquid having a strong od

16、or of ammonia. Specific gravity: about 0.80. It contains between 9% and 11% of NH3. Store it in alkali-resistant containers, in a cold place. Ammonia TS, Stronger Use Ammonia Water, Stronger (see in the section Reagents). Ammoniacal Potassium Ferricyanide TS Dissolve 2 g of potassium ferricyanide in

17、 75 mL of water, add 25 mL of ammonium hydroxide, and mix. Ammoniated Cupric Oxide TS See Cupric Oxide, Ammoniated, TS. Ammonium Acetate TS Dissolve 10 g of ammonium acetate in water to make 100 mL. Ammonium Carbonate TS Dissolve 20 g of ammonium carbonate and 20 mL of ammonia TS in water to make 10

18、0 mL. Ammonium Chloride TS Dissolve 10.5 g of ammonium chloride in water to make 100 mL. Ammonium ChlorideAmmonium Hydroxide TS Mix equal volumes of water and ammonium hydroxide, and saturate with ammonium chloride. Ammonium Molybdate TS Dissolve 6.5 g of finely powdered molybdic acid in a mixture o

19、f 14 mL of water and 14.5 mL of ammonium hydroxide. Cool the solution, and 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 48 hours, and filter through a fine-porosity, sintered-glass crucible. This solution deteriorates upon stan

20、ding and is unsuitable for use if, upon the addition of 2 mL of dibasic sodium phosphate TS to 5 mL of the solution, an abundant yellow precipitate does not form at once or after slight warming. Store it in the dark. If a precipitate forms during storage, use only the clear supernatant. Ammonium Oxa

21、late TS Dissolve 3.5 g of ammonium oxalate in water to make 100 mL. Ammonium Phosphate, Dibasic, TS (Ammonium Phosphate TS) Dissolve 13 g of dibasic ammonium phosphate in water to make 100 mL. Ammonium Polysulfide TS Yellow liquid, made by saturating ammonium sulfide TS with sulfur. Ammonium Pyrroli

22、dinedithiocarbamate, Saturated, TS Add about 10 g of ammonium pyrrolidinedithiocarbamate to a 1000-mL volumetric flask, and dilute with water to volume. Ammonium Reineckate TS Shake about 500 mg of ammonium reineckate with 20 mL of water frequently during 1 hour, and filter. Use within 2 days. Ammon

23、ium Sulfide TS Saturate ammonia TS with hydrogen sulfide by bubbling hydrogen sulfide gas through the solution for 1 minute. This solution must be freshly prepared. The solution is not rendered turbid either by magnesium sulfate TS or by calcium chloride TS (carbonate). This solution is unstable for

24、 use if an abundant precipitate of sulfur is present. Residue on ignition: not more than 0.05%. Ammonium Thiocyanate TS Dissolve 8 g of ammonium thiocyanate in water to make 100 mL. Ammonium Vanadate TS Dissolve 2.5 g of ammonium vanadate in 500 mL of boiling water, cool, and add 20 mL of nitric aci

25、d. Mix, cool, and add water to make 1 L. Store in polyethylene containers. Anthrone TS Within 12 hours of use, rapidly dissolve 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 room temperature, and filter through glass wool. Allow t

26、he solution to stand at room temperature for 30 minutes before use. Antimony Trichloride TS Dissolve 20 g of antimony trichloride in chloroform to make 100 mL. Filter if necessary. Barium Chloride TS Dissolve 12 g of barium chloride in water to make 100 mL. Barium Hydroxide TS A saturated solution o

27、f barium hydroxide in recently boiled water. Prepare the solution fresh. Barium Nitrate TS Dissolve 6.5 g of barium nitrate in water to make 100 mL. Betanaphthol TS See 2-Naphthol TS. 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 10

28、00-mL volumetric flask. Add 300 mL of carbonate-free sodium hydroxide solution (1 in 10), dilute with carbonate-free sodium hydroxide solution (1 in 10) to 1000 mL, and mix. Blue Tetrazolium TS Dissolve 500 mg of blue tetrazolium in alcohol to make 100 mL. Brilliant Blue G TS Transfer 25 mg of brill

29、iant blue G to a 100-mL volumetric flask, add 12.5 mL of alcohol and 25 mL of phosphoric acid, dilute with water to volume, and mix. Bromine TS (Bromine Water) A saturated solution of bromine, prepared by agitating 2 to 3 mL of bromine with 100 mL of cold water in a glass-stoppered bottle, the stopp

30、er of which should be lubricated with petrolatum. Store it in a cold place, protected from light. BromineSodium Acetate TS Dissolve 100 g of sodium acetate in 1000 mL of glacial acetic acid, add 50 mL of bromine, and mix. p-Bromoaniline TS Add 8 g of p-bromoaniline to a mixture of 380 mL of thiourea

31、-saturated glacial acetic acid, 10 mL of sodium chloride solution (1 in 5), 5 mL of oxalic acid solution (1 in 20), and 5 mL of dibasic sodium phosphate solution (1 in 10) in a low-actinic glass bottle. Mix, and allow to stand overnight before using. Protect from light, and use within 7 days. Bromoc

32、resol Blue TS Use Bromocresol Green TS. Bromocresol Green TS Dissolve 50 mg of bromocresol green in 100 mL of alcohol, and filter if necessary. Bromocresol GreenMethyl Red TS Dissolve 0.15 g of bromocresol green and 0.1 g of methyl red in mL of alcohol, and dilute with water to 200 mL. Bromocresol P

33、urple TS Dissolve 250 mg of bromocresol purple in 20 mL of 0.05 N sodium hydroxide, and dilute with water to 250 mL. Bromophenol Blue TS Dissolve 100 mg of bromophenol blue in 100 mL of diluted alcohol, and filter if necessary. Bromothymol Blue TS Dissolve 100 mg of bromothymol blue in 100 mL of dil

34、uted alcohol, and filter if necessary. Buffered Acetone TS See Acetone, Buffered, TS. Calcium Chloride TS Dissolve 7.5 g of calcium chloride in water to make 100 mL. Calcium Hydroxide TS Use Calcium Hydroxide Topical Solution (USP monograph). Calcium Sulfate TS A saturated solution of calcium sulfat

35、e in water. Ceric Ammonium Nitrate TS Dissolve 6.25 g of ceric ammonium nitrate in 10 mL of 0.25 N nitric acid. Use within 3 days. Chloral Hydrate TS Dissolve 50 g of chloral hydrate in a mixture of 15 mL of water and 10 mL of glycerin. Chlorine TS (Chlorine Water) A saturated solution of chlorine i

36、n water. Place the solution in small, pletely filled, light-resistant containers. Chlorine TS, even when kept from light and air, is apt to deteriorate. Store it in a cold, dark place. For full strength, prepare this solution fresh. Chromotropic Acid TS Dissolve 50 mg of chromotropic acid or its dis

37、odium salt in 100 mL of 75% sulfuric acid, which may be made by cautiously adding 75 mL of sulfuric acid to 33.3 mL of water. CobaltUranyl Acetate TS Dissolve, with warming, 40 g of uranyl acetate in a mixture of 30 g of glacial acetic acid and sufficient water to make 500 mL. Similarly, prepare a s

38、olution containing 200 g of cobaltous acetate in a mixture of 30 g of glacial acetic acid and sufficient water to make 500 mL. Mix the two solutions while still warm, and cool to 20. Maintain the temperature at 20 for about 2 hours to separate the excess salts from solution, and then pass through a

39、dry filter. Cobaltous Chloride TS Dissolve 2 g of cobaltous chloride in 1 mL of hydrochloric acid and sufficient water to make 100 mL. Congo Red TS Dissolve 500 mg of congo red in a mixture of 10 mL of alcohol and 90 mL of water. m-Cresol Purple TS Dissolve 0.10 g of metacresol purple in 13 mL of 0.

40、01 N sodium hydroxide, dilute with water to 100 mL, and mix. Cresol Red TS Triturate 100 mg of cresol red in a mortar with 26.2 mL of 0.01 N sodium hydroxide until solution is plete, then dilute the solution with water to 250 mL. Cresol RedThymol Blue TS Add 15 mL of thymol blue TS to 5 mL of cresol

41、 red TS, and mix. Crystal Violet TS Dissolve 100 mg of crystal violet in 10 mL of glacial acetic acid. Cupric Acetate TS Dissolve 100 mg of cupric acetate in about 5 mL of water to which a few drops of acetic acid have been added. Dilute to 100 mL, and filter, if necessary. Cupric Acetate TS, Strong

42、er (Barfoeds Reagent) Dissolve 13.3 g of cupric acetate in a mixture of mL of water and 5 mL of acetic acid. Cupric-Ammonium Sulfate TS To cupric sulfate TS add ammonia TS, dropwise, until the precipitate initially formed is nearly but not pletely dissolved. Allow to settle, and decant the clear sol

43、ution. Prepare this solution fresh. Cupric Citrate TS Dissolve 25 g of cupric sulfate, 50 g of citric acid, and 144 g of anhydrous sodium carbonate in water, and dilute with water to 1000 mL. Cupric Citrate TS, Alkaline With the aid of heat, dissolve 173 g of dihydrated sodium citrate and 117 g of m

44、onohydrated sodium carbonate in about 700 mL of water, and filter through paper, if necessary, to obtain a clear solution. In a separate container dissolve 17.3 g of cupric sulfate in about 100 mL of water, and slowly add this solution, with constant stirring, to the first solution. Cool the mixture

45、, add water to make 1000 mL, and mix. Cupric Citrate TS 2, Alkaline With the aid of heat, dissolve about 173 g of sodium citrate dihydrate and 117 g of sodium carbonate monohydrate in about 700 mL of water, and filter. In a second flask, dissolve about 27.06 g of cupric sulfate (Cu2O45H2O) in about

46、100 mL of water. Slowly bine the two solutions while stirring, and dilute with water to 1000 mL. Cupric Iodide TS, Alkaline Dissolve 7.5 g of cupric sulfate (CuSO45H2O) in about 100 mL of water. In a separate container dissolve 25 g of anhydrous sodium carbonate, 20 g of sodium bicarbonate, and 25 g

47、 of potassium sodium tartrate in about 600 mL of water. With constant stirring, add the cupric sulfate solution to the bottom of the alkaline tartrate solution by means of a funnel that touches the bottom of the container. Add 1.5 g of potassium iodide, 200 g of anhydrous sodium sulfate, 50 to 150 m

48、L of 0.02 M potassium iodate, and sufficient water to make 1000 mL. Cupric Oxide, Ammoniated, TS (Schweitzers Reagent)Dissolve 10 g of cupric sulfate in 100 mL of water, add sufficient sodium hydroxide solution (1 in 5) to precipitate the copper hydroxide, collect the latter on a filter, and wash free from sulfate with cold water. Dissolve the precipitate, which must be kept wet during the entire process, in the minimum quantity of ammonia T