岩矿测试

文章摘要

王学伟,彭南兰,唐琦平,金婷婷.四酸溶样电感耦合等离子体发射光谱法测定地质样品中的钪[J].岩矿测试,2014,33(2):212-217

WANG Xue-wei,PENG Nan-lan,TANG Qi-ping,JIN Ting-ting.Determination of Sc in Geological Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry with Four-Acid Digestion[J].Rock and Mineral Analysis,2014,33(2):212-217.DOI:

四酸溶样电感耦合等离子体发射光谱法测定地质样品中的钪

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Determination of Sc in Geological Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry with Four-Acid Digestion

投稿时间：2013-08-10 修订日期：2013-08-18

DOI：

中文关键词: 地质样品钪酸溶电感耦合等离子体发射光谱法光谱干扰

英文关键词: geological samples Sc acid digestion Inductively Coupled Plasma-Atomic Emission Spectrometry spectral interference

基金项目:

作者	单位
王学伟	云南省有色地质局测试中心, 云南昆明 650216
彭南兰	云南省有色地质局测试中心, 云南昆明 650216
唐琦平	云南省有色地质局测试中心, 云南昆明 650216
金婷婷	云南省有色地质局测试中心, 云南昆明 650216

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中文摘要:

分析地质样品中钪的含量，国家标准方法是采用过氧化钠熔融，过滤分离后电感耦合等离子体发射光谱法（ICP-AES）测定，过程繁琐，样品前处理引入大量盐类且分析结果精度不高，不能适应当前矿产勘查快速准确检测的需要。本文建立了采用硝酸、盐酸、高氯酸和氢氟酸处理样品，ICP-AES测定地质样品中钪的分析方法。选择5%盐酸为溶液介质，干扰元素含量低于2%时运用干扰因子校正法（IEC）优化谱线强度以及适量稀释溶液降低基体效应，提高了分析的准确度和精密度。方法测定范围宽（0.00003%~10%）；检出限为0.0016 μg/mL，优于国家标准方法检出限（0.004 μg/mL）；方法回收率为97.0%~99.3%，方法精密度（RSD，n=6）为0.4%~2.3%；国家一级标准物质的测定值和标准值吻合，分析结果准确可靠。虽然酸溶法不能完全溶解所有类型的地质样品，但对区域环境条件要求不高、简便快捷，本法以酸溶法替代碱熔法处理样品，避免了待测组分和干扰物质的引入，对ICP-AES测定钪的稳定性有较大改善，适用于批量快速分析地质样品中的钪元素。

英文摘要:

The national standard method for the analysis of scandium in geological samples uses sodium peroxide to fuse samples. After the filtration and separation of the sample solution, Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) is applied to determine scandium. This process is complex, moreover, large amounts of salts are brought in during the pretreatment and the accuracy of the result is not satisfactory, and the procedure is lengthy, making it unsuitable for current mineral exploration. A mixture of four-acid system, which includes nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid, to decompose geological samples has been used and is reported in this paper. The Sc was measured by ICP-AES. Hydrochloric acid of 5% is used as the solution medium. When the interference element content is lower than 2%, the interference factor correction (IEC) is applied to optimize the intensity of the spectral line and the solution is diluted appropriately to reduce the matrix effects. Through these steps, the accuracy and precision of the measurement results of scandium were improved. The detection limit of this new method is 0.0016 μg/mL, which is better than the detection limit (0.004 μg/mL) of the national standard method, and the recovery rate of this method is 97.0%-99.3% with measurement range of 0.00003%-10%. The relative standard deviation (RSD, n=6) is in the range of 0.4%-2.3%. National standard reference materials were analysed by this method, and the test results of scandium agree well with the recommended values. Unlike the alkali fusion method, the acid leaching method can avoid bringing in interfering substances. Hereby, the stability has been improved greatly by using ICP-AES to determine Sc. This method is less demanding on the regional and environmental conditions, is simple and fast and can be applied to a large number of geological samples in laboratories.

主管单位：	中国科学技术协会
主办单位：	中国地质学会岩矿测试技术专业委员会国家地质实验测试中心