The Determination of Impurities in Nuclear Grade Sodium by Louis Silverman

By Louis Silverman

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Volumetric flask and dilute to the mark with water. This is the standard carbon solution. 1 ml = 10 fig C. Pseudo-standards mentioned under Part A, Carbon. Phosphoric acid. p. Sulfuric acid. p. Fuming sulfuric acid. 15% excess S 0 . Sulfur trioxide, solid. ) Chromic acid. C r 0 . Oxidizing acid (Van Slyke-type reagent). In the first 500-ml Erlenmeyer flask with ground glass mouth, place 350 ml of cone, sulfuric acid and 25 g of chromic acid. Attach a glass tube about 1 ft long, which has a ground glass end to fit the flask, and a right-angle bend at the other end; the bent end is attached to a "calcium chloride drying tube" which is charged with anhydrone.

Acetylene and carbon monoxide may be retained in silica gel, and then determined by colorimetric methods. Sample size. 1-2 g are usually sufficient. Interferences. Hydrogen sulfide interferes. If suspected, insert a KOH wash bottle. Reagents. Dithizone solution. 5 /xg per 100 ml of carbon tetrachloride. Standard acetylenic carbon {silver nitrate) solution. 7 mg of silver nitrate in water, and dilute to 11. with water. 1 ml = 10 /xg C (acetylenic). This is the stock solution. Transfer by pipette, 10 ml to a 100-ml volumetric flask, and dilute to the mark with water.

Hydrogen sulfide interferes. If suspected, insert a KOH wash bottle. Reagents. Dithizone solution. 5 /xg per 100 ml of carbon tetrachloride. Standard acetylenic carbon {silver nitrate) solution. 7 mg of silver nitrate in water, and dilute to 11. with water. 1 ml = 10 /xg C (acetylenic). This is the stock solution. Transfer by pipette, 10 ml to a 100-ml volumetric flask, and dilute to the mark with water. This is the standard carbon solution. 1 ml == 1 /xg of carbon (acetylenic). ^ Solution A: mix 3 g of cupric chloride, 9 g of ammonium chloride and 40 ml of cone, ammonium hydroxide; dilute to 100 ml with water.

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