Add 116 mL of glacial acetic acid to sufficient water to make 1000 mL after cooling to room temperature.

Dissolve about 8 g of ammonium thiocyanate in 1000 mL of water, and standardize the solution as follows.

Accurately measure about 30 mL of 0.1 N silver nitrate VS into a glass-stoppered flask. Dilute with 50 mL of water, then add 2 mL of nitric acid and 2 mL of ferric ammonium sulfate TS, and titrate with the ammonium thiocyanate solution to the first appearance of a red-brown color.

If desirable, 0.1 N ammonium thiocyanate may be replaced by 0.1 N potassium thiocyanate where the former is directed in various tests and assays.

Dissolve 3 g of potassium bromate and 15 g of potassium bromide in water to make 1000 mL, and standardize the solution as follows.

Accurately measure about 25 mL of the solution into a 500-mL iodine flask, and dilute with 120 mL of water. Add 5 mL of hydrochloric acid, insert the stopper in the flask, and shake it gently. Then add 5 mL of potassium iodide TS, again insert the stopper, shake the mixture, allow it to stand for 5 minutes, and titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the endpoint is approached.

Preserve in dark amber-colored, glass-stoppered bottles.

Dissolve 2.75 g of ceric ammonium nitrate in 1 N nitric acid to obtain 100 mL of solution, and filter. Standardize the solution as follows.

Accurately measure 10 mL of freshly standardized 0.1 N ferrous ammonium sulfate VS into a flask, and dilute with water to about 100 mL. Add 1 drop of nitrophenanthroline TS, and titrate with the ceric ammonium nitrate solution to a colorless endpoint.

Use commercially available volumetric standard solution. Standardize the solution as follows.

Accurately weigh about 0.2 g of sodium oxalate, primary standard, previously dried for 2 hours at 105, and dissolve in 75 mL of water. Add, with stirring, 2 mL of sulfuric acid that has previously been mixed with 5 mL of water, mix well, add 10 mL of hydrochloric acid, and heat to between 70 and 75. Titrate with 0.1 N ceric sulfate to a permanent slight yellow color. Each 6.700 mg of sodium oxalate is equivalent to 1 mL of 0.1 N ceric sulfate.

Dissolve 23.3 g of cupric nitrate 2.5 hydrate, or 24.2 g of the trihydrate, in water to make 1000 mL. Standardize the solution as follows.

Transfer 20.0 mL of the solution to a 250-mL beaker. Add 2 mL of 5 M sodium nitrate, 20 mL of ammonium acetate TS, and sufficient water to make 100 mL. Titrate with 0.05 M edetate disodium VS. Determine the endpoint potentiometrically using a cupric ion-double junction reference electrode system. Perform a blank determination, and make any necessary correction.

To 50 mg of 2,6-dichlorophenol–indophenol sodium that has been stored in a desiccator over soda lime add 50 mL of water containing 42 mg of sodium bicarbonate, shake vigorously, and when the dye is dissolved, add water to make 200 mL. Filter into an amber, glass-stoppered bottle. Use within 3 days and standardize immediately before use. Standardize the solution as follows.

Accurately weigh 50 mg of USP Ascorbic Acid RS, and transfer to a glass-stoppered, 50-mL volumetric flask with the aid of a sufficient volume of metaphosphoric–acetic acids TS to make 50 mL. Immediately transfer 2 mL of the ascorbic acid solution to a 50-mL conical flask containing 5 mL of the metaphosphoric–acetic acids TS, and titrate rapidly with the dichlorophenol–indophenol solution until a distinct rose-pink color persists for at least 5 seconds. Perform a blank titration by titrating 7 mL of the metaphosphoric–acetic acids TS plus a volume of water equal to the volume of the dichlorophenol solution used in titrating the ascorbic acid solution. Express the concentration of the standard solution in terms of its equivalent in mg of ascorbic acid.

Dissolve 18.6 g of edetate disodium in water to make 1000 mL, and standardize the solution as follows.

Accurately weigh about 200 mg of chelometric standard calcium carbonate, previously dried at 110 for 2 hours and cooled in a desiccator, transfer to a 400-mL beaker, add 10 mL of water, and swirl to form a slurry. Cover the beaker with a watch glass, and introduce 2 mL of diluted hydrochloric acid from a pipet inserted between the lip of the beaker and the edge of the watch glass. Swirl the contents of the beaker to dissolve the calcium carbonate. Wash down the sides of the beaker, the outer surface of the pipet, and the watch glass with water, and dilute with water to about 100 mL. While stirring the solution, preferably with a magnetic stirrer, add about 30 mL of the edetate disodium solution from a 50-mL buret. Add 15 mL of sodium hydroxide TS and 300 mg of hydroxy naphthol blue, and continue the titration with the edetate disodium solution to a blue endpoint.

Dissolve 50 g of ferric ammonium sulfate in a mixture of 300 mL of water and 6 mL of sulfuric acid, dilute with water to 1000 mL, and mix. Standardize the solution as follows.

Accurately measure about 40 mL of the solution into a glass-stoppered flask, add 5 mL of hydrochloric acid, mix, and add a solution of 3 g of potassium iodide in 10 mL of water. Insert the stopper, allow to stand for 10 minutes, then titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the endpoint is approached. Correct for a blank run on the same quantities of the same reagents.

Store in tight containers, protected from light.

Dissolve 40 g of ferrous ammonium sulfate in a previously cooled mixture of 40 mL of sulfuric acid and 200 mL of water, dilute with water to 1000 mL, and mix. On the day of use, standardize the solution as follows.

Accurately measure 25 to 30 mL of the solution into a flask, add 2 drops of orthophenanthroline TS, and titrate with 0.1 N ceric sulfate VS until the red color is changed to pale blue.

Dilute 85 mL of hydrochloric acid with water to 1000 mL. Standardize the solution as follows.

Accurately weigh about 5.0 g of tromethamine, previously dried at 105 for 3 hours. Dissolve in 50 mL of water, and add 2 drops of bromocresol green TS. Titrate with 1 N hydrochloric acid to a pale yellow endpoint. Each 121.14 mg of tromethamine is equivalent to 1 mL of 1 N hydrochloric acid.

To a 1000-mL volumetric flask containing 40 mL of water slowly add 43 mL of hydrochloric acid. Cool, and add water to volume. Standardize the solution as follows.

Accurately weigh about 2.5 g of tromethamine, previously dried at 105 for 3 hours. Proceed as directed under Hydrochloric Acid, Normal (1 N), beginning with “Dissolve in 50 mL of water.”

To a 1000-mL volumetric flask containing 40 mL of water slowly add 43 mL of hydrochloric acid. Cool, and add methanol to volume. Standardize the solution as follows.

Accurately weigh about 2.5 g of tromethamine, previously dried at 105 for 3 hours. Proceed as directed under Hydrochloric Acid, Normal (1 N), beginning with “Dissolve in 50 mL of water.”

Dissolve about 14 g of iodine in a solution of 36 g of potassium iodide in 100 mL of water, add 3 drops of hydrochloric acid, dilute with water to 1000 mL, and standardize the solution as follows.

Transfer 25.0 mL of the iodine solution to a 250-mL flask, dilute with water to 100 mL, add 1 mL of 1 N hydrochloric acid, swirl gently to mix, and titrate with 0.1 N sodium thiosulfate VS until the solution has a pale yellow color. Add 2 mL of starch TS and continue titrating until the solution is colorless.

Preserve in amber-colored, glass-stoppered bottles.

Dissolve about 1.4 g of iodine in a solution of 3.6 g of potassium iodide in 100 mL of water, add 3 drops of hydrochloric acid, dilute with water to 1000 mL, and standardize the solution as follows.

Transfer 100.0 mL of iodine solution to a 250-mL flask, add 1 mL of 1 N hydrochloric acid, swirl gently to mix, and titrate with 0.1 N sodium thiosulfate VS until the solution has a pale yellow color. Add 2 mL of starch TS, and continue titrating until the solution is colorless.

Preserve in amber-colored, glass-stoppered bottles.

Dissolve 46 g of lead perchlorate in water, and dilute with water to 1000.0 mL. Accurately weigh about 150 mg of sodium sulfate, previously dried at 105 for 4 hours, and dissolve in 50 mL of water. Add 50 mL of a mixture of water and formaldehyde (1:1), and stir for about 1 minute. Determine the endpoint potentiometrically using a lead ion selective electrode. Perform a blank determination, and make any necessary corrections. Each 14.204 mg of sodium sulfate is equivalent to 1 mL of 0.1 M lead perchlorate.

Accurately pipet 100 mL of commercially available 0.1 M lead perchlorate solution into a 1000-mL volumetric flask, add a sufficient quantity of water to make 1000 mL, and standardize the solution as follows.

Accurately pipet 50 mL of 0.01 M lead perchlorate solution, as prepared above, into a 250-mL conical flask. Add 3 mL of aqueous hexamethylenetetramine solution (2.0 g per 100 mL) and 4 drops of 0.5% xylenol orange indicator prepared by adding 500 mg of xylenol orange to 10 mL of alcohol and diluting with water to 100 mL. (Omit the alcohol if the sodium salt of the indicator is used). Titrate with 0.05 M edetate disodium VS to a yellow endpoint.

Dissolve 0.12 g of freshly cut lithium metal in 150 mL of methanol, cooling the flask during addition of the metal. When the reaction is complete, add 850 mL of methanol, and mix. Store the solution preferably in the reservoir of an automatic delivery buret suitably protected from carbon dioxide and moisture. Standardize the solution by titration against benzoic acid as described under Sodium Methoxide, Tenth-Normal (0.1 N) (in Toluene), but use only 100 mg of benzoic acid. Each 2.442 mg of benzoic acid is equivalent to 1 mL of 0.02 N lithium methoxide.

Dissolve 500 mg of freshly cut lithium metal in 150 mL of methanol, cooling the flask during addition of the metal. When reaction is complete, add 850 mL of chlorobenzene. If cloudiness or precipitation occurs, add sufficient methanol to clarify the solution. Store preferably in the reservoir of an automatic delivery buret suitably protected from carbon dioxide and moisture. Standardize the solution by titration against benzoic acid as described under Sodium Methoxide, Tenth-Normal (0.1 N) (in Toluene).

Dissolve 500 mg of freshly cut lithium metal in 150 mL of methanol, cooling the flask during addition of the metal. When reaction is complete, add 850 mL of methanol. If cloudiness or precipitation occurs, add sufficient methanol to clarify the solution. Store preferably in the reservoir of an automatic delivery buret suitably protected from carbon dioxide and moisture. Standardize the solution by titration against benzoic acid as described under Sodium Methoxide, Tenth-Normal (0.1 N) (in Toluene).

Dissolve 500 mg of freshly cut lithium metal in 150 mL of methanol, cooling the flask during addition of the metal. When reaction is complete, add 850 mL of toluene. If cloudiness or precipitation occurs, add sufficient methanol to clarify the solution. Store preferably in the reservoir of an automatic delivery buret suitably protected from carbon dioxide and moisture. Standardize the solution by titration against benzoic acid as described under Sodium Methoxide, Tenth-Normal (0.1 N) (in Toluene).

Dissolve about 35 g of mercuric nitrate in a mixture of 5 mL of nitric acid and 500 mL of water, and dilute with water to 1000 mL. Standardize the solution as follows.

Transfer an accurately measured volume of about 20 mL of the solution to a conical flask, and add 2 mL of nitric acid and 2 mL of ferric ammonium sulfate TS. Cool to below 20, and titrate with 0.1 N ammonium thiocyanate VS to the first appearance of a permanent brownish color.

Dissolve 6.45 g of oxalic acid in water to make 1000 mL. Standardize by titration against freshly standardized 0.1 N potassium permanganate VS as directed under Potassium Permanganate, Tenth-Normal (0.1 N).

Preserve in glass-stoppered bottles, protected from light.

Mix 8.5 mL of perchloric acid with 500 mL of glacial acetic acid and 21 mL of acetic anhydride, cool, and add glacial acetic acid to make 1000 mL. Alternatively, the solution may be prepared as follows. Mix 11 mL of 60 percent perchloric acid with 500 mL of glacial acetic acid and 30 mL of acetic anhydride, cool, and add glacial acetic acid to make 1000 mL.

Allow the prepared solution to stand for 1 day for the excess acetic anhydride to be combined, and determine the water content by Method I (see Water Determination 921), except to use a test specimen of about 5 g of the 0.1 N perchloric acid that is expected to contain approximately 1 mg of water and the Reagent (see Reagent under Method Ia in Water Determination 921) diluted such that 1 mL is equivalent to about 1 to 2 mg of water. If the water content exceeds 0.5%, add more acetic anhydride. If the solution contains no titratable water, add sufficient water to obtain a content of between 0.02% and 0.5% of water. Allow the solution to stand for 1 day, and again titrate the water content. The solution so obtained contains between 0.02% and 0.5% of water, indicating freedom from acetic anhydride.

Standardize the solution as follows.

Accurately weigh about 700 mg of potassium biphthalate, previously crushed lightly and dried at 120 for 2 hours, and dissolve it in 50 mL of glacial acetic acid in a 250-mL flask. Add 2 drops of crystal violet TS, and titrate with the perchloric acid solution until the violet color changes to blue-green. Deduct the volume of the perchloric acid consumed by 50 mL of the glacial acetic acid. Each 20.42 mg of potassium biphthalate is equivalent to 1 mL of 0.1 N perchloric acid.

Mix 8.5 mL of perchloric acid with sufficient dioxane to make 1000 mL. Standardize the solution as follows.

Accurately weigh about 700 mg of potassium biphthalate, previously crushed lightly and dried at 120 for 2 hours, and dissolve in 50 mL of glacial acetic acid in a 250-mL flask. Add 2 drops of crystal violet TS, and titrate with the perchloric acid solution until the violet color changes to bluish green. Carry out a blank determination. Each 20.42 mg of potassium biphthalate is equivalent to 1 mL of 0.1 N perchloric acid.

Dissolve 4.9455 g of arsenic trioxide primary standard, previously dried at 105 for 1 hour, in 75 mL of 1 N potassium hydroxide. Add 40 g of potassium bicarbonate, dissolved in about 200 mL of water, and dilute with water to 1000.0 mL.

Dissolve 2.784 g of potassium bromate in water to make 1000 mL, and standardize the solution as follows.

Transfer an accurately measured volume of about 40 mL of the solution to a glass-stoppered flask, add 3 g of potassium iodide, and follow with 3 mL of hydrochloric acid. Allow to stand for 5 minutes, then titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the endpoint is approached. Correct for a blank run on the same quantities of the same reagents, and calculate the normality.

Dissolve 2.78 g of potassium bromate (KBrO3) and 12.0 g of potassium bromide (KBr) in water, and dilute with water to 1000 mL. Standardize by the procedure set forth for Potassium Bromate, Tenth-Normal (0.1 N).

Dissolve about 5 g of potassium dichromate in 1000 mL of water. Standardize the solution as follows.

Transfer 25.0 mL of this solution to a glass-stoppered, 500-mL flask, add 2 g of potassium iodide (free from iodate), dilute with 200 mL of water, add 5 mL of hydrochloric acid, allow to stand for 10 minutes in a dark place, and titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the endpoint is approached. Carry out a blank determination.

Dissolve about 17 g of potassium ferricyanide in water to make 1000 mL. Standardize the solution as follows.

Transfer 50.0 mL of this solution to a glass-stoppered, 500-mL flask, dilute with 50 mL of water, add 10 mL of potassium iodide TS and 10 mL of dilute hydrochloric acid, and allow to stand for 1 minute. Then add 15 mL of zinc sulfate solution (1 in 10), and titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the endpoint is approached.

Protect from light, and restandardize before use.

Dissolve 68 g of potassium hydroxide in about 950 mL of water. Add a freshly prepared saturated solution of barium hydroxide until no more precipitate forms. Shake the mixture thoroughly, and allow it to stand overnight in a stoppered bottle. Decant the clear liquid, or filter the solution in a tight, polyolefin bottle, and standardize by the procedure set forth for Sodium Hydroxide, Normal (1 N).

Dissolve about 34 g of potassium hydroxide in 20 mL of water, and add aldehyde-free alcohol to make 1000 mL. Allow the solution to stand in a tightly stoppered bottle for 24 hours. Then quickly decant the clear supernatant into a suitable, tight container, and standardize the solution as follows.

Accurately measure about 25 mL of 0.5 N hydrochloric acid VS. Dilute with 50 mL of water, add 2 drops of phenolphthalein TS, and titrate with the alcoholic potassium hydroxide solution until a permanent, pale pink color is produced.

Dilute 20 mL of 0.5 M alcoholic potassium hydroxide to 100.0 mL with aldehyde-free alcohol.

Dissolve about 6.8 g of potassium hydroxide in 4 mL of water, and add methanol to make 1000 mL. Allow the solution to stand in a tightly stoppered bottle for 24 hours. Then quickly decant the clear supernatant into a suitable, tight container, and standardize the solution as follows.

Accurately measure about 25 mL of 0.1 N hydrochloric acid VS. Dilute with 50 mL of water, add 2 drops of phenolphthalein TS, and titrate with the methanolic potassium hydroxide solution until a permanent, pale pink color is produced.

Dissolve 10.700 g of potassium iodate, previously dried at 110 to constant weight, in water to make 1000.0 mL.

Dissolve about 3.3 g of potassium permanganate in 1000 mL of water in a flask, and boil the solution for about 15 minutes. Insert the stopper in the flask, allow it to stand for at least 2 days, and filter through a fine-porosity, sintered-glass crucible. If necessary, the bottom of the sintered-glass crucible may be lined with a pledget of glass wool. Standardize the solution as follows.

Accurately weigh about 200 mg of sodium oxalate, previously dried at 110 to constant weight, and dissolve it in 250 mL of water. Add 7 mL of sulfuric acid, heat to about 70, and then slowly add the permanganate solution from a buret, with constant stirring, until a pale pink color, which persists for 15 seconds, is produced. The temperature at the conclusion of the titration should be not less than 60. Calculate the normality. Each 6.700 mg of sodium oxalate is equivalent to 1 mL of 0.1 N potassium permanganate.

Since potassium permanganate is reduced on contact with organic substances such as rubber, the solution must be handled in apparatus entirely of glass or other suitably inert material. It should be frequently restandardized. Store in glass-stoppered, amber-colored bottles.

Dissolve about 17.5 g of silver nitrate in 1000 mL of water, and standardize the solution as follows.

Transfer about 100 mg, accurately weighed, of reagent-grade sodium chloride, previously dried at 110 for 2 hours, to a 150-mL beaker, dissolve in 5 mL of water, and add 5 mL of acetic acid, 50 mL of methanol, and about 0.5 mL of eosin Y TS. Stir, preferably with a magnetic stirrer, and titrate with the silver nitrate solution.

Transfer 4.9455 g of arsenic trioxide, which has been pulverized and dried at 100 to constant weight, to a 1000-mL volumetric flask, dissolve it in 40 mL of 1 N sodium hydroxide, and add 1 N sulfuric acid or 1 N hydrochloric acid until the solution is neutral or only slightly acid to litmus. Add 30 g of sodium bicarbonate, dilute with water to volume, and mix.

Dissolve 162 g of sodium hydroxide in 150 mL of carbon dioxide-free water, cool the solution to room temperature, and filter through hardened filter paper. Transfer 54.5 mL of the clear filtrate to a tight, polyolefin container, and dilute with carbon dioxide-free water to 1000 mL.

Accurately weigh about 5 g of potassium biphthalate, previously crushed lightly and dried at 120 for 2 hours, and dissolve in 75 mL of carbon dioxide-free water. Add 2 drops of phenolphthalein TS, and titrate with the sodium hydroxide solution to the production of a permanent pink color. Each 204.2 mg of potassium biphthalate is equivalent to 1 mL of 1 N sodium hydroxide.

Restandardize the solution frequently.

To 250 mL of alcohol add 2 mL of a 50% (w/w) solution of sodium hydroxide.

Dissolve about 200 mg of benzoic acid, accurately weighed, in 10 mL of alcohol and 2 mL of water. Add 2 drops of phenolphthalein TS, and titrate with the alcoholic sodium hydroxide solution until a permanent pale pink color is produced.

Cool in ice-water 150 mL of methanol contained in a 1000-mL volumetric flask, and add, in small portions, about 2.5 g of freshly cut sodium metal. When the metal has dissolved, add toluene to make 1000 mL, and mix. Store preferably in the reservoir of an automatic delivery buret suitably protected from carbon dioxide and moisture. Standardize the solution as follows.

Accurately weigh about 400 mg of primary standard benzoic acid, and dissolve in 80 mL of dimethylformamide in a flask. Add 3 drops of a 1 in 100 solution of thymol blue in dimethylformamide, and titrate with the sodium methoxide to a blue endpoint. Correct for the volume of the sodium methoxide solution consumed by 80 mL of the dimethylformamide. Each 12.21 mg of benzoic acid is equivalent to 1 mL of 0.1 N sodium methoxide.

Weigh 11.5 g of freshly cut sodium metal, and cut into small cubes. Place about 0.5 mL of anhydrous methanol in a round-bottom, 250-mL flask equipped with a ground-glass joint, add 1 cube of the sodium metal, and, when the reaction has ceased, add the remaining sodium metal to the flask. Connect a water-jacketed condenser to the flask, and slowly add 250 mL of anhydrous methanol, in small portions, through the top of the condenser. Regulate the addition of the methanol so that the vapors are condensed and do not escape through the top of the condenser. After addition of the methanol is complete, connect a drying tube to the top of the condenser, and allow the solution to cool. Transfer the solution to a 1-L volumetric flask, dilute with anhydrous methanol to volume, and mix. Standardize the solution as follows.

Accurately measure about 20 mL of freshly standardized 1 N hydrochloric acid VS into a 250-mL conical flask, add 0.25 mL of phenolphthalein TS, and titrate with the sodium methoxide solution to the first appearance of a permanent pink color.

Dissolve 7.5 g of sodium nitrite in water to make 1000 mL, and standardize the solution as follows.

Accurately weigh about 500 mg of USP Sulfanilamide RS, previously dried at 105 for 3 hours, and transfer to a suitable beaker. Add 20 mL of hydrochloric acid and 50 mL of water, stir until dissolved, and cool to 15. Maintaining the temperature at about 15, titrate slowly with the sodium nitrite solution, placing the buret tip below the surface of the solution to preclude air oxidation of the sodium nitrite, and stir the solution gently with a magnetic stirrer, but avoid pulling a vortex of air beneath the surface. Use the indicator specified in the individual monograph, or, if a potentiometric procedure is specified, determine the endpoint electrometrically, using platinum–calomel or platinum–platinum electrodes. When the titration is within 1 mL of the endpoint, add the titrant in 0.1-mL portions, and allow 1 minute between additions. Each 17.22 mg of sulfanilamide is equivalent to 1 mL of 0.1000 M sodium nitrite.

Dissolve an amount of sodium tetraphenylboron, equivalent to 6.845 g of NaB(C6H5)4, in water to make 1000 mL, and standardize the solution as follows.

Pipet two 75-mL portions of the solution into separate beakers, and to each add 1 mL of acetic acid and 25 mL of water. To each beaker add, slowly and with constant stirring, 25 mL of potassium biphthalate solution (1 in 20), and allow to stand for 2 hours. Filter one of the mixtures through a filtering crucible, and wash the precipitate with cold water. Transfer the precipitate to a container, add 50 mL of water, shake intermittently for 30 minutes, filter, and use the filtrate as the saturated potassium tetraphenylborate solution in the following standardization procedure. Filter the second mixture through a tared filtering crucible, and wash the precipitate with three 5-mL portions of saturated potassium tetraphenylborate solution. Dry the precipitate at 105 for 1 hour. Each g of potassium tetraphenylborate is equivalent to 955.1 mg of sodium tetraphenylboron.

Dissolve about 26 g of sodium thiosulfate and 200 mg of sodium carbonate in 1000 mL of recently boiled and cooled water. Standardize the solution as follows.

Accurately weigh about 210 mg of primary standard potassium dichromate, previously pulverized and dried at 120 for 4 hours, and dissolve in 100 mL of water in a glass-stoppered, 500-mL flask. Swirl to dissolve the solid, remove the stopper, and quickly add 3 g of potassium iodide, 2 g of sodium bicarbonate, and 5 mL of hydrochloric acid. Insert the stopper gently in the flask, swirl to mix, and allow to stand in the dark for exactly 10 minutes. Rinse the stopper and the inner walls of the flask with water, and titrate the liberated iodine with the sodium thiosulfate solution until the solution is yellowish green in color. Add 3 mL of starch TS, and continue the titration until the blue color is discharged. Perform a blank determination.

Restandardize the solution as frequently as supported by laboratory stability data. In the absence of such data, restandardize the solution weekly.

Add slowly, with stirring, 13.9 mL of sulfuric acid to a sufficient quantity of dehydrated alcohol to make 1000 mL. Cool, and standardize against tromethamine as described under Hydrochloric Acid, Half-Normal (0.5 N) in Methanol.

Add slowly, with stirring, 30 mL of sulfuric acid to about 1020 mL of water, allow to cool to 25, and determine the normality by titration against tromethamine as described under Hydrochloric Acid, Normal (1 N).

Dissolve 40 g of tetra-n-butylammonium iodide in 90 mL of anhydrous methanol in a glass-stoppered flask. Place in an ice bath, add 20 g of powdered silver oxide, insert the stopper in the flask, and agitate vigorously for 60 minutes. Centrifuge a few mL, and test the supernatant for iodide (see Iodide 191). If the test is positive, add an additional 2 g of silver oxide, and continue to allow to stand for 30 minutes with intermittent agitation. When all of the iodide has reacted, filter through a fine-porosity, sintered-glass funnel. Rinse the flask and the funnel with three 50-mL portions of anhydrous toluene, adding the rinsings to the filtrate. Dilute with a mixture of three volumes of anhydrous toluene and 1 volume of anhydrous methanol to 1000 mL, and flush the solution for 10 minutes with dry, carbon dioxide-free nitrogen. [NOTE—If necessary to obtain a clear solution, further small quantities of anhydrous methanol may be added.] Store in a reservoir protected from carbon dioxide and moisture, and discard after 60 days. Alternatively, the solution may be prepared by diluting a suitable volume of commercially available tetrabutylammonium hydroxide solution in methanol with a mixture of 4 volumes of anhydrous toluene and 1 volume of anhydrous methanol. [NOTE—If necessary to obtain a clear solution, further small quantities of methanol may be added.]

Standardize the solution on the day of use as follows.

Dissolve about 400 mg of primary standard benzoic acid, accurately weighed, in 80 mL of dimethylformamide, add 3 drops of a 1 in 100 solution of thymol blue in dimethylformamide, and titrate to a blue endpoint with the tetrabutylammonium hydroxide solution, delivering the titrant from a buret equipped with a carbon dioxide absorption trap. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N tetrabutylammonium hydroxide is equivalent to 12.21 mg of benzoic acid.

Prepare as described for Tetrabutylammonium Hydroxide, Tenth-Normal (0.1 N) using isopropyl alcohol instead of toluene, and standardize as described. Alternatively, the solution may be prepared by diluting a suitable volume of commercially available tetrabutylammonium hydroxide solution in methanol with 4 volumes of anhydrous isopropyl alcohol.

Dissolve 15.41 g of tetramethylammonium bromide in water to make 1000 mL, and standardize the solution as follows.

Transfer an accurately measured volume of about 40 mL of the solution to a beaker, add 10 mL of diluted nitric acid and 50.0 mL of 0.1 N silver nitrate VS, and mix. Add 2 mL of ferric ammonium sulfate TS, and titrate the excess silver nitrate with 0.1 N ammonium thiocyanate VS.

Dissolve 10.96 g of tetramethylammonium chloride in water to make 1000 mL, and standardize the solution as follows.

Transfer an accurately measured volume of about 40 mL of the solution to a flask, add 10 mL of diluted nitric acid and 50.0 mL of 0.1 N silver nitrate VS, and mix. Add 5 mL of nitrobenzene and 2 mL of ferric ammonium sulfate TS, shake, and titrate the excess silver nitrate with 0.1 N ammonium thiocyanate VS.

Add 75 mL of titanium trichloride solution (1 in 5) to 75 mL of hydrochloric acid, dilute to 1000 mL, and mix. Standardize the solution as follows, using the special titration apparatus described.

Apparatus—Store the titanium trichloride solution in the reservoir of a closed-system titration apparatus in an atmosphere of hydrogen.

Use a wide-mouth, 500-mL conical flask as the titration vessel, and connect it by means of a tight-fitting rubber stopper to the titration buret, an inlet tube for carbon dioxide, and an exit tube. Arrange for mechanical stirring. All joints must be air-tight. Arrange to have both the hydrogen and the carbon dioxide pass through wash bottles containing titanium trichloride solution (approximately 1 in 50) to remove any oxygen.

If the solution to be titrated is to be heated before or during titration, connect the titration flask with an upright reflux condenser through the rubber stopper.

Standardization—Place an accurately measured volume of about 40 mL of 0.1 N ferric ammonium sulfate VS in the titration flask, and pass in a rapid stream of carbon dioxide until all the air has been removed. Add the titanium trichloride solution from the buret until near the calculated endpoint (about 35 mL), then add through the outlet tube 5 mL of ammonium thiocyanate TS, and continue the titration until the solution is colorless.

Dissolve 14.4 g of zinc sulfate in water to make 1 L. Standardize the solution as follows.

Accurately measure about 10 mL of 0.05 M edetate disodium VS into a 125-mL conical flask, and add, in the order given, 10 mL of acetic acid–ammonium acetate buffer TS, 50 mL of alcohol, and 2 mL of dithizone TS. Titrate with the zinc sulfate solution to a clear, rose-pink color.