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 language | English |
|---|---|
| Pages (from-to) | 175-183 |
| Number of pages | 9 |
| Journal | Geostandards and Geoanalytical Research |
| Volume | 34 |
| Issue number | 2 |
| DOIs | |
| Publication status | Published - Jun 2010 |
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Keywords
- Alkaline fusion
- Chlorine
- Fluorine
- Ion chromatography
- Pyrohydrolysis
- Silicate reference materials
ASJC Scopus subject areas
- Geochemistry and Petrology
- Geology
Cite this
Determination of Fluorine and Chlorine by Pyrohydrolysis and Ion Chromatography : Comparison with Alkaline Fusion Digestion and Ion Chromatography. / Wang, Qiaoyun; Makishima, Akio; Nakamura, Eizou.
In: Geostandards and Geoanalytical Research, Vol. 34, No. 2, 06.2010, p. 175-183.Research output: Contribution to journal › Article
}
TY - JOUR
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
Y1 - 2010/6
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
KW - Ion chromatography
KW - Pyrohydrolysis
KW - Silicate reference materials
UR - http://www.scopus.com/inward/record.url?scp=77956247643&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=77956247643&partnerID=8YFLogxK
U2 - 10.1111/j.1751-908X.2010.00043.x
DO - 10.1111/j.1751-908X.2010.00043.x
M3 - Article
VL - 34
SP - 175
EP - 183
JO - Geostandards and Geoanalytical Research
JF - Geostandards and Geoanalytical Research
SN - 0150-5505
IS - 2
ER -