García de Madinabeitia S, Sánchez Lorda M E, Ibarguchi J I Gil
Servicio de Geocronología y Geoquímica Isotópica, Facultad de Ciencia y Tecnología, Universidad del País Vasco/EHU, Sarriena s/n, 48940 Leioa, Spain.
Anal Chim Acta. 2008 Sep 12;625(2):117-30. doi: 10.1016/j.aca.2008.07.024. Epub 2008 Jul 25.
A method has been developed for the simultaneous quantification of major to ultratrace elements in geological samples using quadrupole ICP-MS techniques. The sample preparation involves fusion with LiBO2 and dilution in HNO3-HF which allows complete decomposition of refractory minerals and quantification of the elements of interest. The effects of high Total Dissolved Solids (TDS) and Li in the solution are minimized using a matrix-tolerant interface and conditioning the instrument with LiBO2 solution. The signal drift is moreover controlled using conventional internal standards and specific Drift Correction Standards (DCS). A key issue of the technique is the external calibration using selected Certified Reference Materials (CRM). Depending on the sample type and analytes of interest three optimized programmable modes are used sequentially: Standard, Collision Cell (CCT) and Kinetic Energy Discrimination (KED) mode. The method allows to quantify more than 40 elements in concentrations from tens-of-percent to <0.1 ppm levels during a single experiment. The method has been validated through the analysis of different CRMs with recovery factors of ca. 100% and typical 2sigma errors of <10%.
已开发出一种使用四极杆电感耦合等离子体质谱技术同时定量地质样品中主要元素至超痕量元素的方法。样品制备包括与LiBO₂熔融并在HNO₃-HF中稀释，这能使难熔矿物完全分解并对感兴趣的元素进行定量。使用耐基质接口并用LiBO₂溶液对仪器进行调节，可将溶液中高总溶解固体（TDS）和Li的影响降至最低。此外，使用常规内标和特定的漂移校正标准（DCS）来控制信号漂移。该技术的一个关键问题是使用选定的有证标准物质（CRM）进行外部校准。根据样品类型和感兴趣的分析物，依次使用三种优化的可编程模式：标准模式、碰撞池（CCT）模式和动能歧视（KED）模式。该方法允许在一次实验中对40多种元素进行定量，浓度范围从百分之几十到<0.1 ppm水平。通过分析不同的CRM对该方法进行了验证，回收率约为100%，典型的2σ误差<10%。
