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Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry
Analyst ( IF 3.6 ) Pub Date : 2017-06-22 00:00:00 , DOI: 10.1039/c7an00777a Jay W. Grate 1, 2, 3 , Jhanis J. Gonzalez 3, 4, 5, 6, 7 , Matthew J. O'Hara 1, 2, 3 , Cynthia M. Kellogg 1, 2, 3 , Samuel S. Morrison 1, 2, 3 , David W. Koppenaal 1, 2, 3 , George C.-Y. Chan 3, 4, 5 , Xianglei Mao 3, 4, 5 , Vassilia Zorba 3, 4, 5 , Richard E. Russo 3, 4, 5, 6, 7
Analyst ( IF 3.6 ) Pub Date : 2017-06-22 00:00:00 , DOI: 10.1039/c7an00777a Jay W. Grate 1, 2, 3 , Jhanis J. Gonzalez 3, 4, 5, 6, 7 , Matthew J. O'Hara 1, 2, 3 , Cynthia M. Kellogg 1, 2, 3 , Samuel S. Morrison 1, 2, 3 , David W. Koppenaal 1, 2, 3 , George C.-Y. Chan 3, 4, 5 , Xianglei Mao 3, 4, 5 , Vassilia Zorba 3, 4, 5 , Richard E. Russo 3, 4, 5, 6, 7
Affiliation
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Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.
中文翻译：
熔融基质氟化物盐作为激光烧蚀电感耦合等离子体质谱法的样品制备方法进行固相转化和示踪剂添加
固体采样和分析方法（例如激光烧蚀电感耦合等离子体质谱法（LA-ICP-MS））受到基质效应和校准困难的挑战。很少有用于外部校准的与基质匹配的标准品，很难将尖峰作为内部标准品均匀地分布到固体基质中。尽管可以高精度地测量同一元素的同位素比率，但在采样和分析过程中依赖于基质的效应妨碍了准确的定量和元素比率的确定。在这里，我们介绍了一种潜在的通用固体基质转化方法，该方法需要在熔融的氟化氢铵（ABF）盐中进行化学反应，从而可以引入尖峰作为示踪剂或内标。原理实验证明，在密封的PFA含氟聚合物小瓶中，铀矿石在230°C时分解，冷却后会产生适合通过LA直接采样的新固体。当熔融盐反应中包含尖峰时，随后在几个点进行的LA-ICP-MS采样表明尖峰分布均匀，并且U-235示踪剂显着提高了U-238分析的重现性。精度从U-238信号的17％相对标准偏差提高到样品U-238与尖峰U-235的比率的0.1％，这是两个数量级以上的因数。这些结果介绍了使用ABF进行固体基质转化（SMT）的概念，并为将内标纳入LA-ICP-MS固体的新方法提供了原理证明。这种新方法SMT-LA-ICP-MS 在基于固体的分析中提供了改进校准和定量的机会。展望未来，示踪剂在转化固体中的添加为分析方法学提供了基于洛杉矶的方法，例如标准添加，同位素稀释，与基质匹配的固体标准物的制备，外部校准以及针对外部校准标准的仪器漂移监测。
更新日期：2017-09-08
中文翻译：
熔融基质氟化物盐作为激光烧蚀电感耦合等离子体质谱法的样品制备方法进行固相转化和示踪剂添加
固体采样和分析方法（例如激光烧蚀电感耦合等离子体质谱法（LA-ICP-MS））受到基质效应和校准困难的挑战。很少有用于外部校准的与基质匹配的标准品，很难将尖峰作为内部标准品均匀地分布到固体基质中。尽管可以高精度地测量同一元素的同位素比率，但在采样和分析过程中依赖于基质的效应妨碍了准确的定量和元素比率的确定。在这里，我们介绍了一种潜在的通用固体基质转化方法，该方法需要在熔融的氟化氢铵（ABF）盐中进行化学反应，从而可以引入尖峰作为示踪剂或内标。原理实验证明，在密封的PFA含氟聚合物小瓶中，铀矿石在230°C时分解，冷却后会产生适合通过LA直接采样的新固体。当熔融盐反应中包含尖峰时，随后在几个点进行的LA-ICP-MS采样表明尖峰分布均匀，并且U-235示踪剂显着提高了U-238分析的重现性。精度从U-238信号的17％相对标准偏差提高到样品U-238与尖峰U-235的比率的0.1％，这是两个数量级以上的因数。这些结果介绍了使用ABF进行固体基质转化（SMT）的概念，并为将内标纳入LA-ICP-MS固体的新方法提供了原理证明。这种新方法SMT-LA-ICP-MS 在基于固体的分析中提供了改进校准和定量的机会。展望未来，示踪剂在转化固体中的添加为分析方法学提供了基于洛杉矶的方法，例如标准添加，同位素稀释，与基质匹配的固体标准物的制备，外部校准以及针对外部校准标准的仪器漂移监测。
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