电感耦合等离子体发射光谱法同时测定地质样品中次量钨锡钼
Simultaneous Determination of Minor Tungsten, Tin and Molybdenum in Geological Samples by Inductively Coupled Plasma- Atomic Emission Spectrometry
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摘要: 研究了电感耦合等离子体发射光谱同时测定地质样品中次量钨、锡、 钼的方法。为了避免基体干扰,采用氢氟酸低温分解试样,蒸干除硅,硅以四氟化硅的形式挥发除去。为了减小盐分,用少量过氧化钠熔融未被分解完全的试样残渣,热水提取,盐酸酸化,电感耦合等离子体发射光谱法同时测定钨、锡、 钼。方法相对标准偏差(RSD,n=12)为钨<10.80％,锡<6.67％,钼<8.33％。标准曲线线性浓度上限为:三氧化钨30.0 mg/L,锡40.0 mg/L,钼40.0 mg/L。方法经国家一级标准物质验证,分析结果与标准值相符。Abstract: A method for the simultaneous determination of tungsten, tin and molybdenum in geological samples by inductively coupled plasma-atomic emission spectrometry (ICP-AES) have been developed. In order to eliminate the matrix interference from coexist elements on the determination, the sample preparation method was studied. Samples were digested by HF at low temperature to remove silicon as volatile SiF4 and the residues were decomposed by alkali fusion with Na2O2 followed by extraction with hot water and acidification with diluted HCl. W, Sn and Mo in the sample solution were then determined by ICP-AES. The linear ranges of the calibration curves for each element are 0~30 mg/L for W, 0~40.0 mg/L for Sn and 0~40.0 mg/L for Mo. The precision (RSD, n=12) of the method are <10.80%, <6.67% and <8.33% for W, Sn and Mo, respectively. The method has been applied to the determination of tungsten, tin and molybdenum in National Standard Reference materials and the results are in agreement with the certificated values.
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Key words:
- tungsten /
- tin /
- molybdenum /
- inductively /
- coupled /
- plasma-atomic
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