Identification
The
Assay preparation, prepared as directed in the
Assay, exhibits an absorption maximum at about 196 nm when tested as directed for
Procedure in the
Assay.
Assay
Selenium stock solution
Dissolve about 1 g of metallic selenium, accurately weighed, in a minimum volume of nitric acid. [CautionSelenium is toxic; handle it with care.] Evaporate to dryness, add 2 mL of water, and evaporate to dryness. Repeat the addition of water and the evaporation to dryness three times. Dissolve the residue in 3 N hydrochloric acid, transfer to a 1000-mL volumetric flask, dilute with 3 N hydrochloric acid to volume, and mix. This solution contains about 1000 µg of selenium per mL.
Standard preparations
Transfer 3.0, 4.0, and 5.0 mL, respectively, of Selenium stock solution to separate 100-mL volumetric flasks, dilute the contents of each flask with water to volume, and mix. These Standard preparations contain, respectively, about 30, 40, and 50 µg of selenium per mL.
Assay preparation
Using water as the diluent, quantitatively dilute an accurately measured volume of Injection to obtain a solution containing about 40 µg of selenium per mL.
Procedure
Concomitantly determine the absorbances of the
Standard preparations and the
Assay preparation at the selenium emission line of 196 nm, with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-scattering 851) equipped with a selenium electrodeless discharge lamp and an airacetylene flame, using water as the blank. Plot the absorbances of the
Standard preparations versus concentration, in µg per mL, of selenium, and draw the straight line best fitting the three plotted points. From the graph so obtained, determine the concentration
C, in µg per mL, of selenium in the
Assay preparation. Calculate the quantity, in mg, of selenium in each mL of the Injection taken by the formula:
LC / D,
in which
L is the labeled quantity, in mg per mL, of selenium in the Injection taken, and
D is the concentration, in µg of selenium per mL, of the
Assay preparation on the basis of the labeled quantity in the Injection and the extent of dilution.