The sequential determination of arsenic, selenium, germanium and tin as their hydrides by gas - solid chromatography with an atomic absorption detector.
Hahn-MH; Mulligan-KJ; Jackson-ME; Caruso-JA
Anal Chim Acta 1980; 118(1):115-122
A method was described for the sequential determination of hydrides of arsenic (7440382), germanium (7440564), selenium (7782492), and tin (7440315) in a single run by atomic absorption spectrometry. The hydrides were generated and determined using gas chromatography with an atomic absorption detector. The plug of vaporized hydrides was split into two approximately equal portions. One of these was introduced directly into the flame and analyzed for selenium. The other passed through a chromatographic column which served to separate arsenic, germanium and tin hydrides. While the method resulted in a two fold decrease in sensitivity for each analyte, it avoided separation problems associated with the marked chromatographic overlap of selenium and tin hydrides. The periodic step variation in flow rate during the chromatographic separation provided sufficient time for the necessary manipulations and yet preserved peak shape and minimized the analysis time. Detection limits ranged from 3 parts per billion (ppb) for arsenic to 13ppb for germanium with linear dynamic ranges of about 1.5 orders of magnitude. Relative standard deviations evaluated in the middle of the working range varied from 2 to 11 percent. Manual lamp selection and monochromator adjustment were facilitated by the chromatographic parameters chosen. The time for analysis was 5 minutes.
NIOSH-Publication; NIOSH-Grant; Grants-other; Analytical-methods; Chemical-analysis; Chromatographic-analysis; Metalloids
Chemistry University of Cincinnati Department of Chemistry Cincinnati, Ohio 45221
7440-38-2; 7440-56-4; 7782-49-2; 7440-31-5
Other Occupational Concerns; Grants-other
Analytica Chimica Acta
University of Cincinnati, Cincinnati, Ohio