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王小强. 电感耦合等离子体发射光谱法同时测定长石矿物中钾钠钙镁铝钛铁[J]. 岩矿测试, 2012, 31(3): 442-445.
引用本文: 王小强. 电感耦合等离子体发射光谱法同时测定长石矿物中钾钠钙镁铝钛铁[J]. 岩矿测试, 2012, 31(3): 442-445.
WANG Xiao-qiang. Simultaneous Quantification of K, Na, Ca, Mg, Al, Ti and Fe in Feldspar Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2012, 31(3): 442-445.
Citation: WANG Xiao-qiang. Simultaneous Quantification of K, Na, Ca, Mg, Al, Ti and Fe in Feldspar Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2012, 31(3): 442-445.

电感耦合等离子体发射光谱法同时测定长石矿物中钾钠钙镁铝钛铁

Simultaneous Quantification of K, Na, Ca, Mg, Al, Ti and Fe in Feldspar Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry

  • 摘要: 样品用HCl-HNO3-HClO4-HF分解,电感耦合等离子体发射光谱法同时测定长石矿物中的K、Na、Ca、Mg、Al、Ti、Fe。对元素的分析谱线、溶解用酸的量等工作条件进行了优化,选择了各元素的最佳分析谱线及背景校正模式,探讨HF的用量,试验加内标和不加内标两种测定方法对测定结果的影响。结果表明,对于样品中含量较高的Al,选用次灵敏线396.152 nm,用内标法补偿非光谱干扰,以长石中含量极低的Au作为内标元素(测定谱线为242.795 nm)可以获得满意的结果,方法检出限为0.45~3.56 μg/g。经国家一级标准物质GBW 03134、GBW 3116验证,测定值的相对误差(RE)为-1.32%~10.0%,ICP-AES法与其他测定方法的测定结果无显著性差异,方法精密度(RSD, n=10)为0.55%~7.2%,能够满足长石矿物中相关组分的准确测定。

     

    Abstract: Feldspar samples were digested with HCl-HNO3-HClO4-HF mixed acids and K, Na, Ca, Mg, Al, Ti and Fe in sample solutions were directly determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES). The conditions for selection of analytical lines and the amount of dissolved acids were optimized. The best determination result was obtained when the sub-sensitive analytical lines were used for the high content elements. For low content elements, the sensitive analytical lines were used. The amount of HF had to be strictly controlled, which greatly impact on the determination of the results. The results were verified by the internal standard method and a non-internal standard method. The sub-sensitive analytical line of 396.152 nm was selected for high Au content samples. The best result was obtained by using an internal standard to calibrate the nonspectral interference, selecting the low content Au in feldspar as the internal standard and analytical line of 242.795 nm. The established method has been applied to the rapid determination of K, Na, Ca, Mg, Al, Ti and Fe in feldspar samples. The determination limits of the method were 3.5 6 μg/g for K2O, 1.25 μg/g for Na2O, 1.93 μg/g for CaO, 1.86 μg/g for MgO, 0.452 μg/g for Al2O3, 2.97 μg/g for TiO2 and 1.57 μg/g for Fe2O3. The relative error (RE) ranged from -1.32% to 10.0% with a precision of 0.55%-7.2% (RSD, n=10). The results were in agreement with the certified values and chemical method. This method provided the advantages of wide dynamic linear range, high efficiency and simple operation. The method has been applied to determine these components in various feldspar samples with accurate and reliable results.

     

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