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首页> 外文期刊>Geostandards and geoanalytical research >Determination of Fluorine and Chlorine by Pyrohydrolysis and Ion Chromatography: Comparison with Alkaline Fusion Digestion and Ion Chromatography
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Determination of Fluorine and Chlorine by Pyrohydrolysis and Ion Chromatography: Comparison with Alkaline Fusion Digestion and Ion Chromatography

机译：热水解和离子色谱法测定氟和氯：与碱性融合消解和离子色谱法比较

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摘要

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 lg 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 Na_2CO_3 + 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.
机译：描述了一种通过热解和离子色谱法（IC）测定硅酸盐材料中F和Cl的方法。热解包括将粉碎的样品（约40 mg）与V2O5（约160 mg）混合，并在石英管中的湿氧气流下加热至1100°C。使用NaF + NaCl标准溶液，F和Cl的回收率约为97％。对于硅酸盐样品，热解-IC法的检出限分别为F和Cl为0.36和0.69 lg g〜（-1）。 GSJ的参考材料JB-2，JB-3和JA-1中的氟和Cl浓度已确定;来自USGS的BCR-2，BHVO-1，BHVO-2，AGV-1和AGV-2; NIST SRM 610、612和614眼镜。测定F的精密度（RSD）为1-13％（NIST SRM 614除外），Cl的准确度为2-19％，这取决于浓度和空白校正。在这项研究中获得的大多数结果与以前的研究非常吻合。相比之下，在900°C的Na_2CO_3 + ZnO熔融方法显示，碱熔融产生的F和Cl的产量随熔融持续时间的增加而系统地降低。 JB-3的收率分别为84％和83％，这表明F和Cl在这种碱性熔融过程中损失了。

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