A rapid high-performance analytical procedure with simultaneous voltammetric determination of toxic trace metals in...

For the monitoring of toxic trace metals in urine a new high-performance trace analytical procedure with simultaneous voltammetric determination is presented. Particular emphasis has been placed on minimizing contamination by reducing the urine sample volume to 1 ml and consequently limiting the needed amount of HNO(3)/HClO(4) and the duration (<20 min) of the wet digestion stage. The procedure consists of three stages. First 20 urine samples (1 ml each) are simultaneously freeze-dried overnight. They then require only a short wet digestion (HClO(4)/HNO(3) 2:1, 20 min, 210 degrees ). They are then adjusted to pH 4.5 with acetate buffer and the trace metals are determined simultaneously by differential pulse anodic-stripping voltammetry at the mercury film electrode, the quartz digestion vessel being used as the voltammetric cell. If precipitates occur in the acidified samples, their trace metal content can be determined in the same manner, avoiding the low results commonly obtained by other methods. The procedure has high sensitivity with fair to good precision, covers a determination range from the sub-mug/l. to the medium mug/l. level and lends itself to automation. It is cheaper and more accurate than atomic absorption. Thus the procedure provides important potentialities for surveillance of occupationally exposed persons as well as for extended ecotoxicological baseline studies in man and cattle.