Determination of Fluorine and Chlorine by Pyrohydrolysis and Ion Chromatography: Comparison with Alkaline Fusion Digestion and Ion Chromatography

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Abstract

A method to determine F and Cl in silicate materials by employing pyrohydrolysis and ion chromatography (IC) is described. Pyrohydrolysis involved mixing a pulverised sample (~ 40 mg) with V2O5 (~ 160 mg) and heating to 1100 °C under a wet oxygen flow in a quartz tube. Recovery yields of F and Cl were ~ 97% using a NaF + NaCl standard solution. Detection limits of the pyrohydrolysis-IC method for silicate samples were 0.36 and 0.69 μg g-1 for F and Cl, respectively. Fluorine and Cl concentrations were determined in the reference materials JB-2, JB-3 and JA-1 from the GSJ; BCR-2, BHVO-1, BHVO-2, AGV-1 and AGV-2 from the USGS; and NIST SRM 610, 612 and 614 glasses. Precisions (RSD) for determinations of F were 1-13% (except NIST SRM 614) and 2-19% for Cl, and were dependent on the concentration and blank correction. Most results obtained in this study were in good agreement with those of previous studies. In comparison, the Na2CO3 + ZnO fusion method at 900 °C showed that the yields of F and Cl by alkaline fusion systematically decreased with fusion duration time. The yields were 84% and 83% for JB-3, inferring that F and Cl were lost in this alkaline fusion.

Original languageEnglish
Pages (from-to)175-183
Number of pages9
JournalGeostandards and Geoanalytical Research
Volume34
Issue number2
DOIs
Publication statusPublished - Jun 1 2010

Keywords

  • Alkaline fusion
  • Chlorine
  • Fluorine
  • Ion chromatography
  • Pyrohydrolysis
  • Silicate reference materials

ASJC Scopus subject areas

  • Geology
  • Geochemistry and Petrology

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