敞口酸溶-电感耦合等离子体质谱法同时测定地质样品中45个元素
Determination of Elemental Content in Geological Samples by One-Time Acid Dissolution and Inductively Coupled Plasma-Mass Spectrometry
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摘要: 改进了三酸(HCl-HNO3-HF)或四酸(HCl-HNO3-HF-HClO4)溶矿对难溶元素分解不彻底及对易挥发元素测定结果不稳定的现象,建立了地质样品中15个稀土元素及其常规微量元素一次溶矿、一次测定的分析方法,提高了分析质量。采用HCl-HNO3-HF-HClO4-H2SO4混合酸一次分解样品,用50%的逆王水复溶提取后定容,以Rh为内标元素,三通在线进样方式,电感耦合等离子体质谱法同时测定地质样品中45个元素的含量。讨论了分解方法对易挥发元素、难溶元素的影响,对岩石标准物质(GBW07106)、水系沉积物标准物质(GBW07303)和土壤标准物质(GBW07429)的测定值与标准值相一致,方法精密度为0.03%~4.97%。方法准确度高,简单、快捷、实用。
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关键词:
- 敞口酸溶 /
- 电感耦合等离子体质谱法 /
- 地质样品 /
- 元素测定
Abstract: The methods of HCl-HNO3-HF and HCl-HNO3-HF-HClO4 were improved to overcome the incomplete decomposition of refractory elements and bad replication results of volatile elements. A new analysis method has been developed for 15 rare earth elements and common trace elements by ore dissolution and determination. Analytical quality and efficiency have been greatly improved. Geological samples were dissolved with mixed acids of HCl-HNO3-HF-HClO4-H2SO4 in 30 mL teflon crucible on a hot plate. The salts were dissolved and extracted by 50% reverse aqua regia and diluted to constant volume. 45 elements in the samples were determined simultaneously by ICP-MS with 10 ng/mL Rh as the internal standard and three on-line injections. The effect of volatile elements are discussed in detail for the decomposition method. The certified reference material of rock (GBW07106), stream sediment (GBW07303) and soil (GBW07429) were analyzed to test the method. Results are in good agreement with certified values. Standard deviations of the method are 0.03%-4.97%. This method is rapid, simple and practical with high precision.-
Keywords:
- opening /
- acid /
- dissolution /
- inductively
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