Dissolve 40.0 mg of metallic selenium in 100 mL of dilute nitric acid (1 in 2) in a 1000-mL volumetric flask, warming gently on a steam bath if necessary to effect solution, add water to volume, and mix. Pipet 5 mL of this solution into a 200-mL volumetric flask, add water to volume, and mix. Each mL of the resulting solution contains the equivalent of 1 µg of selenium (Se).
Dissolve 100 mg of 2,3-diaminonaphthalene and 500 mg of hydroxylamine hydrochloride in 0.1 N hydrochloric acid to make 100 mL. Prepare this solution fresh on the day of use.
Pipet 6 mL of Stock Solution into a 150-mL beaker, and add 25 mL of dilute nitric acid (1 in 30) and 25 mL of water.
Clean combustion of the test material is an important factor in conducting the test. For compounds that burn poorly and produce soot, the addition of magnesium oxide usually results in more thorough combustion and reduces soot formation. Where the need to add magnesium oxide has been identified, it is specified in the individual monograph. Using a 1000-mL combustion flask and using 25 mL of dilute nitric acid (1 in 30) as the absorbing liquid, proceed as directed under Oxygen Flask Combustion 471
, using a test specimen weighing 100 to 200 mg, unless directed otherwise in the individual monograph. Upon completion of the combustion, place a few mL of water in the cup, loosen the stopper, and rinse the stopper, the specimen holder, and the sides of the flask with about 10 mL of water. Transfer the solution with the aid of about 20 mL of water to a 150-mL beaker, and heat gently to the boiling temperature. Boil for 10 minutes, and allow the solution to cool to room temperature.
Treat the Standard Solution, the Test Solution, and the reagent blank consisting of 25 mL of dilute nitric acid (1 in 30) and 25 mL of water, concomitantly and in parallel, as follows. Add ammonium hydroxide solution (1 in 2) to adjust to a pH of 2.0 ± 0.2. Dilute with water to 60 mL, and transfer to a low-actinic separator with the aid of 10 mL of water, adding the 10 mL of rinsings to the separator. Add 200 mg of hydroxylamine hydrochloride, swirl to dissolve, immediately add 5.0 mL of Diaminonaphthalene Solution, insert the stopper, and swirl to mix. Allow the solution to stand at room temperature for 100 minutes. Add 5.0 mL of cyclohexane, shake vigorously for 2 minutes, and allow the layers to separate. Discard the aqueous layer, and centrifuge the cyclohexane extract to remove any dispersed water. Determine the absorbances of the cyclohexane extracts of the Test Solution and the Standard Solution in a 1-cm cell at the wavelength of maximum absorbance at about 380 nm, with a suitable spectrophotometer, using the cyclohexane extract of the reagent blank as the blank, and compare the absorbances: the absorbance of the Test Solution is not greater than that of the Standard Solution where a 200-mg test specimen has been taken, or is not greater than one-half that of the Standard Solution where a 100-mg test specimen has been taken.