Identification
A:
To 2 mL of a dilution of Oral Solution (1 in 40) add 5 mL of
sodium cobaltinitrite TS: a yellow precipitate is formed immediately (
presence of potassium).
B:
Evaporate 5 mL on a steam bath to dryness: a mineral oil dispersion of the residue so obtained exhibits an IR absorption maximum in the spectral region between 6.2 and 6.25 µm (carboxylic acid salt).
C:
It responds to the tests for
Chloride 191.
Assay for potassium
Potassium stock solution
Dissolve in water 0.9535 g of potassium chloride, previously dried at 105
for 2 hours. Transfer to a 500-mL volumetric flask, dilute with water to volume, and mix. This solution contains 1000 µg of potassium per mL.
Standard preparations
To separate 200-mL volumetric flasks transfer 19.0 mL and 25.0 mL, respectively, of
Potassium stock solution, dilute with water to volume, and mix. The
Standard preparations contain 95.0 µg and 125.0 µg of potassium per mL, respectively.
Assay preparation
Transfer an accurately measured volume of Oral Solution, equivalent to about 782 mg (20 mEq) of potassium, to a 100-mL volumetric flask, dilute with water to volume, and mix. Transfer 7.0 mL of the resulting solution to a 500-mL volumetric flask, dilute with water to volume, and mix.
Procedure
Concomitantly determine the absorbances of the
Standard preparations and the
Assay preparation at the resonance line of 766.5 nm, with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-scattering 851) equipped with a potassium hollow-cathode lamp and an airacetylene flame, using water as the blank. Plot the absorbances of the
Standard preparations versus concentration, in µg per mL, of potassium. From the graph so obtained, determine the concentration,
C, in µg per mL, of potassium in the
Assay preparation. Calculate the quantity, in mg, of potassium in each mL of the Oral Solution taken by the formula:
(50 / 7)(C / V),
in which
V is the volume, in mL, of Oral Solution taken. Each mg of potassium is equivalent to 0.02558 mEq.
Assay for chloride
Ionic strength adjusting solution
Use 5 M sodium nitrate.
Procedure
Transfer an accurately measured volume of Oral Solution, equivalent to about 100 mg (2.8 mEq) of chloride, to a suitable beaker. Add 2.0 mL of Ionic strength adjusting solution and water to make about 100 mL, and titrate with 0.1 N silver nitrate VS, determining the endpoint potentiometrically, using a silver-sulfide specific ion-selective electrode and a double-junction reference electrode containing potassium nitrate solution (1 in 10). Perform a blank determination, and make any necessary correction. Each mL of 0.1 N silver nitrate is equivalent to 3.545 mg of chloride (Cl). Each mg of chloride is equivalent to 0.0282 mEq of Cl.