Chemistry Department, Lomonosov Moscow State University, 1-3 Leninskie Gory, 1, 119991 Moscow, Russia.
Anal Chim Acta. 2012 Feb 3;713:97-102. doi: 10.1016/j.aca.2011.11.035. Epub 2011 Nov 25.
Different methods of rock sample digestion for final analysis by ICP-MS technique are investigated. It is shown that only basic rocks can be quantitatively digested in a microwave (MW) field with the mixture of HF and HNO(3) acids at 210°C for 60 min. The addition of HCl and H(3)BO(3) provides complete digestion of andesites and some types of granites. Even at maximal temperature in the used MW oven of 210°C syenites, granodiorites and albitized granites are not digested. These types of rocks are not digested in a closed Teflon autoclave for 16 h and can be digested only by fusion with lithium metaborate. The reason for such behavior is discussed. To avoid problems with the introduction of heavily acidic solutions after fusion in ICP the solutions were diluted. To compensate the loss of sensitivity due to the dilution step the REEs (Rare Earth Elements) pre-concentration using aminocarboxylic Pol-DETATA (diethyltriaminetetraacetate) sorbent was tested. The developed scheme is validated by the analysis of a wide range of reference rock materials.
研究了用于 ICP-MS 技术最终分析的不同岩石样品消解方法。结果表明,只有碱性岩石才能在 210°C 下用 HF 和 HNO3 混合酸在微波(MW)场中定量消解 60 分钟。添加 HCl 和 H3BO3 可完全消解安山岩和某些类型的花岗岩。即使在使用的 MW 炉的最高温度 210°C 下,霞石正长岩、花岗闪长岩和钠长石化花岗岩也未被消解。这些类型的岩石不能在封闭的聚四氟乙烯高压釜中 16 小时消解,只能用锂硼酸盐熔融消解。讨论了这种行为的原因。为了避免熔融后引入强酸溶液的问题,将溶液进行了稀释。为了补偿由于稀释步骤导致的灵敏度损失,测试了使用氨基羧酸多-DETATA(二乙三胺五乙酸)吸附剂对稀土元素(REEs)进行预浓缩。通过对广泛的参考岩样的分析验证了所开发的方案。