1. DEFINITIONS
1.1 Normal solutions:
![]() N = equivalent/L
N = weight (g)/equivalent weight (g) × L
Normal solutions and solutions bearing a specific relationship to normal solutions, and used in volumetric determinations, are designated as follows:
1 N = normal
2 N = double normal
0.5 N = half-normal
0.1 N = tenth-normal
0.02 N = fiftieth normal
0.01 N = hundredth-normal
0.001 N = thousandth-normal
1.2 Molar solutions:
![]() M = mol/L
M = weight (g)/mol weight × L
Solutions containing one-tenth of a gram-molecule of the compound in 1 L are designated tenth-molar, 0.1 M; and other molarities are similarly indicated.
1.3 Correction factor:
![]() The concentration of the volumetric solution does not differ from the prescribed one by more than 10%. The correction factor is determined by an appropriate number of replicates. The repeatability does not exceed 0.2% (relative standard deviation). The correction factor should be redetermined frequently.
1.4 Blank determinations:
![]()
2. PREPARATION AND STANDARDIZATION
2.1 Scope
When solutions of a reagent are used in different concentrations, the details of the preparation and standardization are usually given for the concentration most frequently required. Stronger or weaker solutions are prepared and standardized in the same general manner as described, using proportionate amounts of the reagent.
2.2 Preparation by dilution
It is possible in many instances to prepare lower concentrations accurately by making an exact dilution of a stronger solution.
Volumetric solutions prepared by dilution should be restandardized as directed for the stronger solution, using proportionate amounts of reagents.
Dilute solutions that are not stable, as, for instance, potassium permanganate 0.01 N, are preferably prepared by exactly diluting the higher normality with thoroughly boiled and cooled water on the same day they are required for use.
2.3 Standardization
The following directions give only one method for standardization, but other methods of standardization, capable of yielding at least the same degree of accuracy, may be used.
The values obtained in the standardization of volumetric solutions are valid for all Pharmacopeial uses of these solutions, regardless of the instrumental or chemical indicators used in the individual monographs.
Where the apparent normality or molarity of a titrant depends upon the special conditions of its use, the individual monograph sets forth the directions for standardizing the reagent in the specified context.
For those salts that usually are available as certified primary standards or that are available as highly purified salts of primary standard quality, it is permissible to prepare solutions by accurately weighing a suitable quantity of the salt and dissolving it to produce a specific volume of solution of known concentration. Acetic, hydrochloric, and sulfuric acids may be standardized against a sodium hydroxide solution that recently has been standardized against a certified primary standard.
2.4 Temperature
All volumetric solutions, if practicable, are to be prepared, standardized, and used at the standard temperature of 25
![]() If a titration is carried out with the volumetric solution at a markedly different temperature, standardize the volumetric solution used as the titrant at that different temperature, or make a suitable temperature correction.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
Acetic Acid, Double-Normal (2 N)
C2H4O2,
![]() ![]() ![]() 120.10 g in 1000 mL
Add 116 mL of glacial acetic acid to sufficient water to make 1000 mL after cooling to room temperature.
Ammonium Thiocyanate, Tenth-Normal (0.1 N)
NH4SCN,
![]() ![]() ![]() 7.612 g in 1000 mL
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.
Bismuth Nitrate, 0.01 M
Bi(NO3)3·5H2O,
![]() ![]() ![]() 1000 mL of this solution contains 4.851 g of bismuth nitrate pentahydrate
Dissolve 4.86 g of bismuth nitrate pentahydrate in 60 mL of dilute nitric acid, add 0.01 N nitric acid to make 1000 mL, and standardize the solution as follows.
Accurately measure 25 mL of the prepared bismuth nitrate solution, add 50 mL of water and 1 drop of xylenol orange TS, and titrate the solution with 0.01 M edetate disodium VS until the red color changes to yellow. Calculate the molarity factor.
Bromine, Tenth-Normal (0.1 N)
Br,
![]() ![]() ![]() 7.990 g in 1000 mL
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.
Ceric Ammonium Nitrate, Twentieth-Normal (0.05 N)
Ce(NO3)4·2NH4NO3,
![]() ![]() ![]() 2.741 g in 100 mL
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.
Ceric Sulfate, Tenth-Normal (0.1 N)
Ce(SO4)2,
![]() ![]() ![]() 33.22 g in 1000 mL
Use commercially available volumetric standard solution. Standardize the solution as follows.
Accurately weigh about 0.2 g of sodium oxalate, primary standard, dried according to the instructions on its label, 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
![]() ![]() Cupric Nitrate, Tenth-Normal (0.1 N)
Cu(NO3)2·2.5H2O,
![]() ![]() ![]() 23.26 g in 1000 mL
Cu(NO3)2·3H2O,
![]() ![]() ![]() 24.16 g in 1000 mL
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.
Cupric Tartrate, Alkaline, Solution (Fehling's Solution)
Copper solution (Solution A)
Transfer 34.639 g of cupric sulfate to a 500-mL volumetric flask, and dissolve in and dilute with water to volume. Filter, if necessary.
Alkaline tartrate solution (Solution B)
Transfer 173 g of potassium sodium tartrate and 50 g of sodium hydroxide to a 500-mL volumetric flask, and dissolve in and dilute with water to volume. Filter, if necessary.
Just before use, prepare Cupric tartrate, alkaline, solution by mixing equal volumes of Solution A and Solution B. Standardize this solution as follows.
Standard stock solution
Transfer 9.5 g of sucrose to a 1-L volumetric flask, dissolve in 100 mL of water, add 5 mL of hydrochloric acid, and store 3 days at 20
![]() ![]()
Invert sugar solution
Immediately before use in standardizing the Cupric tartrate, alkaline, solution, transfer 25 mL of Standard stock solution to a 100-mL volumetric flask, and dilute with water to volume.
Procedure
Apparatus
Mount a ring support on a ring stand 12 inches above a gas burner, and mount a second ring 67 inches above the first. Place 6-inch open-wire gauze on the lower ring to support a 400-mL conical flask, and place a 4-inch watch glass with a center hole on the upper ring to deflect heat. Attach a 50-mL buret to the ring stand so that the tip just passes through the watch glass centered above the flask. Place an indirectly lighted white surface behind the assembly for observing the endpoint.
Standardization
Transfer 20.0 mL of the Cupric tartrate, alkaline, solution to a 400-mL flask containing a few boiling chips, and add 15 mL of water and 39.0 mL of Invert sugar solution. Mix by swirling at ambient temperature, and immediately place the flask on the wire gauze of the Apparatus. Adjust the burner so that the boiling point of the solution is reached in about 2 min. Boil gently but steadily for 2 min. As boiling continues, add 34 drops of methylene blue solution (1 in 100). Complete the titration within 1 min by adding the Invert sugar solution dropwise until the blue color disappears. Allow a 5-s reaction time between drops at the end of titration. Adjust the Cupric tartrate, alkaline, solution for the correct amount of copper (equivalent to 100 mg of invert sugar), and restandardize if the total volume of Invert sugar solution is more or less than 40.0 mL.
Standard DichlorophenolIndophenol Solution
To 50 mg of 2,6-dichlorophenolindophenol 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 metaphosphoricacetic 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 metaphosphoricacetic acids TS, and titrate rapidly with the dichlorophenolindophenol solution until a distinct rose-pink color persists for at least 5 seconds. Perform a blank titration by titrating 7 mL of the metaphosphoricacetic 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.
Edetate Disodium, Twentieth-Molar (0.05 M)
C10H14N2Na2O8·2H2O,
![]() ![]() ![]() 18.61 g in 1000 mL
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
![]() Ferric Ammonium Sulfate, Tenth-Normal (0.1 N)
FeNH4(SO4)2·12H2O,
![]() ![]() ![]() 48.22 g in 1000 mL
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.
Ferrous Ammonium Sulfate, Tenth-Normal (0.1 N)
Fe(NH4)2(SO4)2·6H2O,
![]() ![]() ![]() 39.21 g in 1000 mL
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.
Hydrochloric Acid, Alcoholic, Tenth-Molar (0.1 M)
HCl,
![]() ![]() ![]() Dilute 9.0 mL of hydrochloric acid to 1000 mL with aldehydefree alcohol.
Hydrochloric Acid, Half-Normal (0.5 N)
HCl,
![]() ![]() ![]() 18.23 g in 1000 mL
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, dried according to the label instructions or, if this information is not available, dried at 105
![]() Hydrochloric Acid, Half-Normal (0.5 N) in Methanol
HCl,
![]() ![]() ![]() 18.23 g in 1000 mL
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, dried according to the label instructions or, if this information is not available, dried at 105
![]() Hydrochloric Acid, Normal (1 N)
HCl,
![]() ![]() ![]() 36.46 g in 1000 mL
Dilute 85 mL of hydrochloric acid with water to 1000 mL. Standardize the solution as follows.
Accurately weigh about 5.0 g of tromethamine, dried according to the label instructions or, if this information is not available, dried at 105
![]() Iodine, Tenth-Normal (0.1 N)
I,
![]() ![]() ![]() 12.69 g in 1000 mL
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.
Iodine, Twentieth-Normal (0.05 N)
I,
![]() ![]() ![]() 6.33 g in 1000 mL
Dissolve about 6.5 g of iodine in a solution of 18 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 50.0 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.
Iodine, Hundredth-Normal (0.01 N)
I,
![]() ![]() ![]() 1.269 g in 1000 mL
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.
Lead Nitrate, Hundredth-Molar (0.01 M)
Pb (NO3)2,
![]() ![]() ![]() 3.312 g in 1000 mL
Xylenol Orange Triturate
Triturate 1 part of xylenol orange with 99 parts of potassium nitrate.
0.1 M Lead Nitrate
Dissolve 33 g of lead nitrate in 1000 mL of water. Standardize the solution as follows. To 20.0 mL of the lead nitrate solution add 300 mL of water. Add about 50 mg of Xylenol Orange Triturate, and add methenamine until the solution becomes violet-pink. Titrate with 0.1 M edetate disodium VS to the yellow endpoint. Calculate the molarity.
Dilute 50.0 mL of 0.1 M Lead Nitrate to 500.0 mL with water.
Lead Perchlorate, Tenth-Molar (0.1 M)
Pb(ClO4)2·3H2O,
![]() ![]() ![]() 46.01 g in 1000 mL
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
![]() Lead Perchlorate, Hundredth-Molar (0.01 M)
Pb(ClO4)2,
![]() ![]() ![]() 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.
Change to read:
Lithium Methoxide, Fiftieth-Normal (0.02 N) in Methanol
CH3LiO,
![]() ![]() ![]() 759.6 mg in 1000 mL
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.
[NoteRestandardize the solution frequently. ]
Change to read:
Lithium Methoxide, Tenth-Normal (0.1 N) in Chlorobenzene
CH3OLi,
![]() ![]() ![]() 3.798 g in 1000 mL
Dissolve 700 mg 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 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.
[NoteRestandardize the solution frequently. ]
Change to read:
Lithium Methoxide, Tenth-Normal (0.1 N) in Methanol
CH3OLi,
![]() ![]() ![]() 3.798 g in 1000 mL
Dissolve 700 mg 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. 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.
[NoteRestandardize the solution frequently. ]
Change to read:
Lithium Methoxide, Tenth-Normal (0.1 N) in Toluene
CH3OLi,
![]() ![]() ![]() 3.798 g in 1000 mL
Dissolve 700 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.
[NoteRestandardize the solution frequently. ]
Magnesium Chloride, 0.01 M
MgCl2·6H2O,
![]() ![]() ![]() 2.0330 g in 1000 mL
Dissolve about 2.04 g of magnesium chloride in 1000 mL of freshly boiled and cooled water, and standardize the solution as follows.
Accurately measure 25 mL of the prepared magnesium chloride solution. Add 50 mL of water, 3 mL of ammoniaammonium chloride buffer TS and 0.04 g of eriochrome black Tsodium chloride reagent. Titrate with 0.05 M edetate disodium VS until the red-purple color of the solution changes to blue-purple.
Mercuric Nitrate, Tenth-Molar (0.1 M)
Hg(NO3)2,
![]() ![]() ![]() 32.46 g in 1000 mL
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
![]() Oxalic Acid, Tenth-Normal (0.1 N)
H2C2O4·2H2O,
![]() ![]() ![]() 6.303 g in 1000 mL
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.
Change to read:
Perchloric Acid, Tenth-Normal (0.1 N) in Dioxane
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
![]() ![]() ![]() Perchloric Acid, Tenth-Normal (0.1 N) in Glacial Acetic Acid
HClO4,
![]() ![]() ![]() 10.05 g in 1000 mL
[NoteWhere called for in the tests and assays, this volumetric solution is specified as 0.1 N perchloric acid. Thus, where 0.1 N or other strength of this volumetric solution is specified, the solution in glacial acetic acid is to be used, unless the words in dioxane are stated. (See also Perchloric Acid, Tenth-Normal (0.1 N) in Dioxane.) ]
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% 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
![]() ![]() ![]() ![]() Standardize the solution as follows.
Accurately weigh about 700 mg of potassium biphthalate, previously crushed lightly and dried at 120
![]() Potassium Arsenite, Tenth-Normal (0.1 N)
KAsO2,
![]() ![]() ![]() 7.301 g in 1000 mL
Dissolve 4.9455 g of arsenic trioxide primary standard, previously dried at 105
![]() Potassium Bromate, Tenth-Normal (0.1 N)
KBrO3,
![]() ![]() ![]() 2.784 g in 1000 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.
Potassium BromideBromate, Tenth-Normal (0.1 N)
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).
Potassium Dichromate, Tenth-Normal (0.1 N)
K2Cr2O7,
![]() ![]() ![]() 4.903 g in 1000 mL
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.
Potassium Ferricyanide, Twentieth-Molar (0.05 M)
K3Fe(CN)6,
![]() ![]() ![]() 16.46 g in 1000 mL
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.
Potassium Hydroxide, Alcoholic, Half-Normal (0.5 N)
28.06 g in 1000 mL
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.
[NoteStore in tightly stoppered bottles, protected from light. ]
Potassium Hydroxide, Alcoholic, Tenth-Molar (0.1 M)
KOH,
![]() ![]() ![]() Dilute 20 mL of 0.5 M alcoholic potassium hydroxide to 100.0 mL with aldehyde-free alcohol.
Potassium Hydroxide, Methanolic, Tenth-Normal (0.1 N)
5.612 g in 1000 mL
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.
[NoteStore in tightly stoppered bottles, protected from light. ]
Potassium Hydroxide, Normal (1 N)
KOH,
![]() ![]() ![]() 56.11 g in 1000 mL
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).
Potassium Iodate, Twentieth-Molar (0.05 M)
KIO3,
![]() ![]() ![]() 10.70 g in 1000 mL
Dissolve 10.700 g of potassium iodate, previously dried at 110
![]() Potassium Permanganate, Tenth-Normal (0.1 N)
KMnO4,
![]() ![]() ![]() 3.161 g in 1000 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, dried according to the instructions on its label, and dissolve it in 250 mL of water. Add 7 mL of sulfuric acid, heat to about 70
![]() ![]() 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.
Potassium Thiocyanate, Tenth-Normal (0.1 N)
KSCN,
![]() ![]() ![]() 9.72 g in 1000 mL
Weigh exactly 9.72 g of potassium thiocyanate, previously dried for 2 hours at 110
![]() Silver Nitrate, Tenth-Normal (0.1 N)
AgNO3,
![]() ![]() ![]() 16.99 g in 1000 mL
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
![]() Sodium Arsenite, Twentieth-Molar (0.05 M)
NaAsO2
![]() ![]() ![]() 6.496 g in 1000 mL
Transfer 4.9455 g of arsenic trioxide, which has been pulverized and dried at 100
![]() Sodium Hydroxide, Alcoholic, Tenth-Normal (0.1 N)
NaOH,
![]() ![]() ![]() To 250 mL of alcohol add 2 mL of a 50% (w/v) 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.
Sodium Hydroxide, Normal (1 N)
NaOH,
![]() ![]() ![]() 40.00 g in 1000 mL
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
![]()
[Note(1) Solutions of alkali hydroxides absorb carbon dioxide when exposed to air. They should be preserved in bottles having well-fitted, suitable stoppers, provided with a tube filled with a mixture of sodium hydroxide and lime (soda-lime tubes) so that air entering the container must pass through this tube, which will absorb the carbon dioxide. (2) Prepare solutions of lower concentration (e.g., 0.1 N, 0.01 N) by quantitatively diluting accurately measured volumes of the 1 N solution with sufficient carbon dioxide-free water to yield the desired concentration. ]
Restandardize the solution frequently.
Sodium Methoxide, Half-Normal (0.5 N) in Methanol
CH3ONa,
![]() ![]() ![]() 27.01 g in 1000 mL
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.
Sodium Methoxide, Tenth-Normal (0.1 N) in Toluene
CH3ONa,
![]() ![]() ![]() 5.402 g in 1000 mL
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.
[Note(1) To eliminate any turbidity that may form following dilution with toluene, add methanol (25 to 30 mL usually suffices) until the solution is clear. (2) Restandardize the solution frequently. ]
Sodium Nitrite, Tenth-Molar (0.1 M)
NaNO2,
![]() ![]() ![]() 6.900 g in 1000 mL
Dissolve 6.9 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
![]() ![]() ![]() Sodium Tetraphenylboron, Fiftieth-Molar (0.02 M)
NaB(C6H5)4,
![]() ![]() ![]() 6.845 g in 1000 mL
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
![]()
[NotePrepare this solution just before use. ]
Sodium Thiosulfate, Tenth-Normal (0.1 N)
Na2S2O3·5H2O,
![]() ![]() ![]() 24.82 g in 1000 mL
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
![]() Restandardize the solution as frequently as supported by laboratory stability data. In the absence of such data, restandardize the solution weekly.
Sulfuric Acid, Half-Normal (0.5 N) in Alcohol
H2SO4,
![]() ![]() ![]() 24.52 g in 1000 mL
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.
Sulfuric Acid, Normal (1 N)
H2SO4,
![]() ![]() ![]() 49.04 g in 1000 mL
Add slowly, with stirring, 27 mL of sulfuric acid to a sufficient quantity of water to make 1000 mL. Cool and standardize against tromethamine as described under Hydrochloric Acid, Normal (1 N).
Tetrabutylammonium Hydroxide, Tenth-Normal (0.1 N)
(C4H9)4NOH,
![]() ![]() ![]() 25.95 g in 1000 mL
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
![]() ![]() 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.
Tetrabutylammonium Hydroxide in Methanol/Isopropyl Alcohol, 0.1 N
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.
Tetramethylammonium Bromide, Tenth-Molar (0.1 M)
(CH3)4NBr,
![]() ![]() ![]() 15.41 g in 1000 mL
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.
Tetramethylammonium Chloride, Tenth-Molar (0.1 M)
(CH3)4NCl,
![]() ![]() ![]() 10.96 g in 1000 mL
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.
Titanium Trichloride, Tenth-Normal (0.1 N)
TiCl3,
![]() ![]() ![]() 15.42 g in 1000 mL
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.
ApparatusStore 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.
StandardizationPlace 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.
Zinc Sulfate, Twentieth-Molar (0.05 M)
ZnSO4·7H2O,
![]() ![]() ![]() 14.4 g in 1000 mL
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 acidammonium 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.
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