Sodium hypophosphite as reducing agent for determination of submicrogram quantities of mercury in animal feeds and manures

The reduction of mercury in samples of dairy cattle and chicken feed rations and manures prepared by acid digestion for determination by flameless atomic absorption is rapidly, smoothly, and quantitatively effected by sodium hypophosphite. The reducing agent is air-stable, is effective over a wide range of mercury concentrations, and is useful in the presence of many mineral acids commonly used for wet digestion of these matrices. The accuracy and precision obtained in determinations with this reagent are equivalent to those obtained using stannous chloride at the same conditions. Recovery efficiencies for the total analytical procedure were studied using cattle manure and feed rations spiked to 0.6 ppm Hg as phenylmercuric nitrate; the range of recoveries varied from 93 to 102% (97% average). The absolute detection limit of the method is 10 ng Hg, and the precision varies in the range of 2.2-6% for samples containing 3 ppt-10 ppm Hg. The advantages of sodium hypophosphite lie in the elimination of premature reduction of mercury caused by traces of stannous chloride adhering to the walls of the reaction vessel, the elimination of several wash steps in the determination, and the long shelf life of the reagent.