Galler Patrick, Limbeck Andreas, Boulyga Sergei F, Stingeder Gerhard, Hirata Takafumi, Prohaska Thomas
Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, University of Natural Resources and Applied Life Sciences, Muthgasse 18, A-1190 Vienna, Austria.
Anal Chem. 2007 Jul 1;79(13):5023-9. doi: 10.1021/ac070307h. Epub 2007 Jun 1.
This work introduces a newly developed on-line flow injection (FI) Sr/Rb separation method as an alternative to the common, manual Sr/matrix batch separation procedure, since total analysis time is often limited by sample preparation despite the fast rate of data acquisition possible by inductively coupled plasma-mass spectrometers (ICPMS). Separation columns containing approximately 100 muL of Sr-specific resin were used for on-line FI Sr/matrix separation with subsequent determination of (87)Sr/(86)Sr isotope ratios by multiple collector ICPMS. The occurrence of memory effects exhibited by the Sr-specific resin, a major restriction to the repetitive use of this costly material, could successfully be overcome. The method was fully validated by means of certified reference materials. A set of two biological and six geological Sr- and Rb-bearing samples was successfully characterized for its (87)Sr/(86)Sr isotope ratios with precisions of 0.01-0.04% 2 RSD (n = 5-10). Based on our measurements we suggest (87)Sr/(86)Sr isotope ratios of 0.713 15 +/- 0.000 16 (2 SD) and 0.709 31 +/- 0.000 06 (2 SD) for the NIST SRM 1400 bone ash and the NIST SRM 1486 bone meal, respectively. Measured (87)Sr/(86)Sr isotope ratios for five basalt samples are in excellent agreement with published data with deviations from the published value ranging from 0 to 0.03%. A mica sample with a Rb/Sr ratio of approximately 1 was successfully characterized for its (87)Sr/(86)Sr isotope signature to be 0.718 24 +/- 0.000 29 (2 SD) by the proposed method. Synthetic samples with Rb/Sr ratios of up to 10/1 could successfully be measured without significant interferences on mass 87, which would otherwise bias the accuracy and uncertainty of the obtained data.
本研究介绍了一种新开发的在线流动注射(FI)锶/铷分离方法,以替代常用的手动锶/基体批次分离程序。尽管电感耦合等离子体质谱仪(ICPMS)能够快速采集数据,但总分析时间往往受样品制备的限制。使用含有约100μL锶特异性树脂的分离柱进行在线FI锶/基体分离,随后通过多接收ICPMS测定(87)Sr/(86)Sr同位素比值。成功克服了锶特异性树脂所表现出的记忆效应,这是限制这种昂贵材料重复使用的一个主要因素。该方法通过有证标准物质进行了全面验证。一组两个生物样品和六个含锶和铷的地质样品成功地测定了其(87)Sr/(86)Sr同位素比值,精密度为0.01 - 0.04% 2RSD(n = 5 - 10)。基于我们的测量,我们建议NIST SRM 1400骨灰和NIST SRM 1486骨粉的(87)Sr/(86)Sr同位素比值分别为0.713 15±0.000 16(2SD)和0.709 31±0.0