| Abstrakt: |
Flow-injection hydride generation and in situ concentration of As, Sb and Bi hydrides in graphite furnace atomic absorption spectrometry can be automated by means of a long-term stable trapping reagent replacing the Pd modifier. In a systematic study, carbide-forming elements (Zr, Nb, Ta, W) and noble metals (Ir, Ir/Mg, Pd/Ir) were investigated as stable adsorbers which require only a single application. Trapping temperature curves indicate high signals for trapping of As at 750-800 degrees C, Sb at 450-8000 degrees C and Bi at 100-500 degrees C on Zr-coated tubes. Ir- and Ir/Mg-coated tubes showed a high response for Sb and Bi at lower temperatures, but based on signal stability and reproducibility (over 400 trapping and atomization cycles tested) the better performance was found with the Zr-coated tubes. The radiotracers Sb-125 and Bi-207 were used to measure the hydride generation (>95% for both elements) and trapping efficiency (91% for Sb and 56% for Bi) on the Zr-coated tube. An adsorptive "carry-over effect" was observed with Sb and Bi but not with As, and trapping temperatures above 450 degrees C with Sb and 350 degrees C with Bi (the "critical temperatures") can lead to errors in absorbance values. On a Zr-coated tube the characteristic mass was about 16 pg for As, 15 pg for Sb and 9 pg for Bi (peak height) and the detection limits (3 sigma) were about 0.015, 0.010 and 0.027 ng, respectively, with a 1 ml sample loop. The method was tested by the determination of the elements in NIST low-alloy steel certified reference materials. |
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