Assay
Sodium chloride solution
Dissolve 1.8 g of sodium chloride in water, dilute with water to 2000 mL, and mix.
Manganese stock solution
Transfer 1.000 g of manganese to a 1000-mL volumetric flask, dissolve in 20 mL of nitric acid, dilute with 0.1 N hydrochloric acid to volume, and mix. This solution contains 1000 µg of manganese per mL. Store in a polyethylene bottle.
Standard preparations
Pipet 10 mL of the Manganese stock solution into a 500-mL volumetric flask, dilute with water to volume, and mix. Transfer 4.0, 5.0, and 6.0 mL, respectively, of this solution to separate 50-mL volumetric flasks, containing 10 mL of Sodium chloride solution, dilute the contents of each flask with water to volume, and mix. These Standard preparations contain, respectively, 1.6, 2.0, and 2.4 µg of manganese per mL.
Assay preparation
Transfer an accurately measured volume of Injection, equivalent to about 1 mg of manganese, to a 100-mL volumetric flask, dilute with water to volume, and mix. Pipet 10 mL of this solution into a 50-mL volumetric flask. From the labeled amount of sodium chloride, if any, in the Injection, calculate the amount, in mg, of sodium chloride in the initial dilution, and add sufficient Sodium chloride solution to bring the total sodium chloride content in this flask to 9 mg. Dilute with water to volume, and mix.
Procedure
Concomitantly determine the absorbances of the
Standard preparations and the
Assay preparation at the manganese emission line of 279 nm, with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-scattering 851) equipped with a manganese hollow-cathode lamp and an airacetylene flame, using a dilution of
Sodium chloride solution (1:5) as the blank. Plot the absorbances of the
Standard preparations versus concentration, in µg per mL, of manganese, and draw the straight line best fitting the three plotted points. From the graph so obtained, determine the concentration, in µg per mL, of manganese in the
Assay preparation. Calculate the quantity, in mg, of manganese in each mL of the Injection taken by the formula:
0.5C / V,
in which
C is the concentration, in µg per mL, of manganese in the
Assay preparation; and
V is the volume, in mL, of Injection taken.