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 2010

Fingerprint

Ion chromatography
Fluorine
ion chromatography
Chlorine
fluorine
digestion
chlorine
Fusion reactions
Silicates
silicate
Quartz
glass
quartz
heating
oxygen
Oxygen
Heating
Recovery
Glass
method

Keywords

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

ASJC Scopus subject areas

  • Geochemistry and Petrology
  • Geology

Cite this

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title = "Determination of Fluorine and Chlorine by Pyrohydrolysis and Ion Chromatography: Comparison with Alkaline Fusion Digestion and Ion Chromatography",
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.",
keywords = "Alkaline fusion, Chlorine, Fluorine, Ion chromatography, Pyrohydrolysis, Silicate reference materials",
author = "Qiaoyun Wang and Akio Makishima and Eizou Nakamura",
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T1 - Determination of Fluorine and Chlorine by Pyrohydrolysis and Ion Chromatography

T2 - Comparison with Alkaline Fusion Digestion and Ion Chromatography

AU - Wang, Qiaoyun

AU - Makishima, Akio

AU - Nakamura, Eizou

PY - 2010/6

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N2 - 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.

AB - 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.

KW - Alkaline fusion

KW - Chlorine

KW - Fluorine

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KW - Silicate reference materials

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