Separation and enrichment of palladium and gold in biological and environmental samples, adapted to the determination by total reflection X-ray fluorescence

Abstract

The reductive co-precipitation of trace and ultra-trace elements together with mercury followed by complete evaporation of the mercury makes it possible to determine palladium and gold by total reflection X-ray fluorescence. Both elements can be detected without interferences at optimal sensitivity in the pg range. Thus, detection limits of, e.g., 2.5 ng L-1 for palladium and 2.0 ng L-1 for gold, in urine, were obtained. The precision was determined to 0.04 at a palladium concentration of about 200 ng L-1 urine and to 0.19 at a gold concentration of only 18 ng L-1. The recovery for a urine sample spiked with known amounts of palladium and gold amounted to > 95%. Results of the combined procedure are given for the determination of palladium and gold in the urine of non-exposed and occupationally exposed persons and in some other environmentally relevant samples.

Palladium [Biomonitoring Methods in German language, 2008]

“…Spektrale Interferenzen störten das Palladiumsignal und führten zu falsch positiven Werten [7,8]. Erst in den letzten 3 Jahren gelang es unter großen analytischen Anstrengungen, Nachweismethoden zu entwickeln, die zur Analyse der Hintergrundbelastung der Allgemeinbevölkerung mit Palladium geeignet waren [12][13][14]20]. In Tabelle 11 Literatur…”

Synthesis of 5,6-Diphenyl-2,3-dihydro-1,2,4-triazine-3-thione as a New Reagent for Spectrophotometric Determination of Palladium

“…Thus due to the urgent need for specific monitoring of Pd ion in many industrial, environmental, and food samples there have been a number of reports on Flame Atomic Absorption Spectroscopy (FAAS) 11,12 , (ETAAS) 13 , Inductively Coupled Plasma Mass Spectrometry 10,14 and x-ray fluorescence spectrometry 15 in the literature.…”

Separation and preconcentration trace amounts of gold by using modified organo nanoclay closite 15A

“…Other sensitive techniques such as neutron activation analysis 9 or total reflection X-ray fluorescence spectrometry (TXRF) 10 are less often applied in gold analysis due to the complexity and cost of the required instrumentation. In environmental, geological and biological samples, the low concentration of gold together with the high concentration of interfering matrix components often require an enrichment step combined with a matrix separation.…”