Rhodium as permanent modifier for atomization of lead from biological fluids usign tungsten filament electrothermal atomic absorption spectrometry

摘要

Rhodium (Rh) was investigated as a permanent modifier for the atomization of Pb from biological fluids in W-filament atomic absorption spectrometry (AAS). Heating the W-filament with a Rh solution provided a protective coating for subsequent determinations of Pb in blood and urine matrices. The W-filament AAS instrumentation used coating for subsequent determinations of Pb in blood and urine matrices. The W-filament AAS instrumentation used was based on a prototype design that utilized self-reversal background correction scheme and peak area measurements. We found that Rh not only stabilized Pb during the pryolysis step, but also facilitated the removal of carbonaceous residues during the cleaning step, requiring much less power than with phosphate modifier. Thus, the filament lifetime was greatly extended to over 300 firings. Periodic reconditioning with Rh was necessary every 30 firings or so. Conditioning the filament with Rh also permitted direct calibration using simple aqueous Pb standards. The method detection limit for blood Pd was approximately 1.5 #mu#g dl~(-1), similar to that reported previously. Potential interferences from concomitants such as N,a K, Ca and Mg were evaluated. Accuracy was verified using lead reference materials from the National Institute of Standards and Technology and the New York State Department of Health. Blood lead results below 40 #mu#g dl~(-1) were within +-1 #mu#g dl~(-1) of certified values, and within +=10% above 40 #mu#g dl~(-1); within run precision was +- 10% or better. Additional validation was reported using proficiency test materials and human blood specimens. All blood lead results were within the acceptable limits established by regulatory authorities in the US. When measuring Pb in urine, sensitivity was reduced and matrix-matched calibration became necessary. The method of detection limit was 27 #mu#g l~(-1) for urine Pb. Urine lead results were also validated using an acceptable range comparable to that established for blood lead by US regulatory agencies.