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Germanium – Bestimmung von Germanium und seinen nichtflüchtigen, anorganischen Verbindungen in der Luft am Arbeitsplatz mittels Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)

2023/12/19 by Pitzke, Katrin, Wippich, Cornelia, Woznica, Anita +3
#543 Analytical chemistry #543 Analytische Chemie #571.95 Toxicology #571.95 Toxikologie #616.9803 Betriebs- und Arbeitsmedizin #616.9803 Industrial and occupational medicine #Analysenmethode #Arbeitsplatzmessung #Bestimmungsgrenze #GSP Sammelkopf #GSP sampling head #Gefahrstoff #Germanium #Germanium dioxide #Germanium(IV) oxide #Germanium(IV)oxid #Germaniumdioxid #ICP-MS #Interner Standard #Luft #Luftanalysen #Massenspektrometrie mit induktiv gekoppeltem Plasma #Membranfilter #Messbereich #Mikrowellengestützter Druckaufschluss #Probenahme #Präzision #Selektivität #Wiederfindung #air #air analyses #analytical method #einatembare Partikel #hazardous substance #inductively coupled plama mass spectrometry #inductively coupled plasma mass spectrometry #inhalable particles #internal standard #limit of quantification #measurement range #membrane filter #microwave-assisted pressure digestion #precision #recovery #sampling #selectivity #workplace measurement

paper · doi:10.34865/am744056d8_4or

Abstract

This analytical method is a validated measurement procedure for the determination of germanium [7440-56-4] and its non-volatile compounds in workplace air in a concentration range of one tenth up to twice of the currently valid Occupational Exposure Limit Value (OELV) in Germany of 0.85 mg/m3 as germanium in the inhalable dust fraction. For sampling, a defined volume of air is drawn through a membrane filter (cellulose nitrate). The flow rate is 10 l/min and sampling duration is 2 hours. Germanium is digested with a mixture of hydrofluoric and nitric acid in a microwave-assisted pressure digestion. The samples are subsequently analysed using mass spectrometry with inductively coupled plasma (ICP-MS). The quantitative determination is based on a calibration function. The limit of quantification is 0.004 µg/m3 for an air sample volume of 1200 l and 20 ml digestion volume. The mean recovery is 97.2% for germanium and 97.9% for germanium dioxide. The expanded uncertainty for the validation range of 0.085 to 1.7 mg/m3 is 35.7 to 24.4%.

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