By Louis Silverman
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Additional info for The Determination of Impurities in Nuclear Grade Sodium Metal
Example text
Preparation of the standard curve for the determination of elemental carbon. 0 ml) of the standard carbon (sucrose) solution are added to the reaction flasks and evaporated to dryness. 5 g of the ignited sodium sulfate. Follow the procedure from the point ® . Preparation of the sample. ) Elemental carbon only. Obtain the sodium sample. Cut away oil, dirt, rust and extraneous materials that are not part of the sample. Select a sample size of about 2 g for carbon content less than 30 fig', 1 g for samples containing more than 30 ^g of carbon; up to 5-g samples of sodium may be used.
Absorbance as ordinate for the cyanide carbon standard curve. Procedure. Dissolve 1 g of sodium metal in cold water, under a protective blanket of nitrogen. Transfer the solution to a 50- or 100-ml evaporating dish and add 2-3 mg of precipitated sulfur. Evaporate to the appearance of solids, then cool. Add 15 ml of water to dissolve the solids, and cool. Add 2 ml of ferric perchlorate and neutralize with perchloric acid (about 4 ml), at which time the ferric hydroxide dissolves. Add 5 ml of perchloric acid in excess.
Obtain "micrograms, carbon" from the carbon (acetylene, silver) standard curve. 41 CARBON ^ , , . Calculation: i^gj C (as acetylenic carbon) _ , . —— = C (acetylenic) (ppm). wt. of sample (g) v J ; VFF / Discussion. Acetylene is not found in many samples of sodium metal. Silverman and Trego noted its presence using the silver acetylide cloud, as described. It is possible that carbide initiates corrosion more quickly, if present. When the amount of carbide is greater than 50 /xg, the spectrophotometric technique of Gilbert et al.