Identification
The
Assay preparation,prepared as directed in the
Assay,exhibits an absorption maximum at about 196nm when tested as directed for
Procedurein the
Assay.
Assay
Selenium stock solution
Dissolve about 1g of metallic selenium,accurately weighed,in a minimum volume of nitric acid.[CautionSelenium is toxic;handle it with care.]Evaporate to dryness,add 2mLof water,and evaporate to dryness.Repeat the addition of water and the evaporation to dryness three times.Dissolve the residue in 3Nhydrochloric acid,transfer to a 1000-mLvolumetric flask,dilute with 3Nhydrochloric acid to volume,and mix.This solution contains about 1000µg of selenium per mL.
Standard preparations
Transfer 3.0,4.0,and 5.0mL,respectively,of Selenium stock solutionto separate 100-mLvolumetric flasks,dilute the contents of each flask with water to volume,and mix.These Standard preparationscontain,respectively,about 30,40,and 50µg 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 40µg of selenium per mL.
Procedure
Concomitantly determine the absorbances of the
Standard preparationsand the
Assay preparationat the selenium emission line of 196nm,with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-scattering á851ñ)equipped with a selenium electrodeless discharge lamp and an airacetylene flame,using water as the blank.Plot the absorbances of the
Standard preparationsversus 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 mLof the Injection taken by the formula:
LC/D,
in which
Lis the labeled quantity,in mg per mL,of selenium in the Injection taken,and
Dis the concentration,in µg of selenium per mL,of the
Assay preparationon the basis of the labeled quantity in the Injection and the extent of dilution.