Kylander M E, Weiss D J, Jeffries T E, Kober B, Dolgopolova A, Garcia-Sanchez R, Coles B J
Department of Earth Science and Engineering, Imperial College London, London, UK.
Anal Chim Acta. 2007 Jan 16;582(1):116-24. doi: 10.1016/j.aca.2006.08.050. Epub 2006 Aug 30.
An analytical protocol for rapid and reliable laser ablation-quadrupole (LA-Q)- and multi-collector (MC-) inductively coupled plasma-mass spectrometry (ICP-MS) analysis of Pb isotope ratios ((207)Pb/(206)Pb and (208)Pb/(206)Pb) in peats and lichens is developed. This technique is applicable to source tracing atmospheric Pb deposition in biomonitoring studies and sample screening. Reference materials and environmental samples were dry ashed and pressed into pellets for introduction by laser ablation. No binder was used to reduce contamination. LA-MC-ICP-MS internal and external precisions were <1.1% and <0.3%, respectively, on both (207)Pb/(206)Pb and (208)Pb/(206)Pb ratios. LA-Q-ICP-MS internal precisions on (207)Pb/(206)Pb and (208)Pb/(206)Pb ratios were lower with values for the different sample sets <14.3% while external precisions were <2.9%. The level of external precision acquired in this study is high enough to distinguish between most modern Pb sources. LA-MC-ICP-MS measurements differed from thermal ionisation mass spectrometry (TIMS) values by 1% or less while the accuracy obtained using LA-Q-ICP-MS compared to solution MC-ICP-MS was 3.1% or better using a run bracketing (RB) mass bias correction method. Sample heterogeneity and detector switching when measuring (208)Pb by Q-ICP-MS are identified as sources of reduced analytical performance.
开发了一种用于泥炭和地衣中铅同位素比值((²⁰⁷)Pb/(²⁰⁶)Pb和(²⁰⁸)Pb/(²⁰⁶)Pb)的快速可靠的激光烧蚀 - 四极杆(LA - Q)和多接收器(MC)电感耦合等离子体质谱(ICP - MS)分析的分析方案。该技术适用于生物监测研究和样品筛选中的大气铅沉积源追踪。参考物质和环境样品经干灰化后压制成颗粒,通过激光烧蚀引入。未使用粘合剂以减少污染。LA - MC - ICP - MS对(²⁰⁷)Pb/(²⁰⁶)Pb和(²⁰⁸)Pb/(²⁰⁶)Pb比值的内部和外部精密度分别<1.1%和<0.3%。LA - Q - ICP - MS对(²⁰⁷)Pb/(²⁰⁶)Pb和(²⁰⁸)Pb/(²⁰⁶)Pb比值的内部精密度较低,不同样品集的值<14.3%,而外部精密度<2.9%。本研究中获得的外部精密度水平足以区分大多数现代铅源。LA - MC - ICP - MS测量值与热电离质谱(TIMS)值的差异在1%或更小,而使用LA - Q - ICP - MS与溶液MC - ICP - MS相比,采用运行括号(RB)质量偏倚校正方法获得的准确度为3.1%或更好。样品的不均匀性以及通过Q - ICP - MS测量(²⁰⁸)Pb时的检测器切换被确定为分析性能下降的原因。