1. Anion-Exchange Chromatographic Separation of Hg for Isotope Ratio Measurements by Multicollector ICPMS.
- Author
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Malinovsky, Dmitry, Sturgeon, Ralph E., and Lu Yang
- Subjects
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ANIONS , *CHROMATOGRAPHIC analysis , *ISOTOPES , *INDUCTIVELY coupled plasma mass spectrometry , *RATIO measurement , *CYSTEINE proteinases , *CHEMICAL purification - Abstract
A procedure is described for precise Hg isotope ratio measurements by solution nebulization multicollector inductively coupled plasma mass spectrometry (MC- ICPMS). Hg was released from geological samples using aqua regia extraction and then separated from other matrix elements with the aid of anion-exchange chromatography using strongly basic Dowex 1-X8 anion-exchange resin. Performance of the chromatographic procedure was evaluated using various types of replacement anions for elution of mercury, including L-cysteine, thiourea, NO3-, and SO42-. A solution of 0.15% L-cysteine in 0.06 M HCl was found to be the most convenient eluent for subsequent MC-ICPMS measurements. The optimized procedure provides separation of Hg from virtually all concomitant matrix elements while maintaining quantitative (>95%) recovery. In addition, band displacement chromatographic experiments were conducted to assess whether the anion-exchange purification can produce Hg isotope fractionation artifacts. No isotope fractionation between the Hg(II)-L-cysteine complex in aqueous solution and Hg ions in the anion-exchange resin was observed. Hg isotope ratio measurements were performed using the bracketing standards approach and on-line correction for instrumental mass discrimination using TI spiking and normalization to the 205Tl/203Tl ratio. The absence of spectral interference during Hg isotope ratio measurements was verified using a three-isotope plot. Uncertainties of Hg isotope ratio measurements for replication of the entire procedure, expressed as two standard deviations, are better than ±0.08‰/amu. The described procedure facilitates study of variations in the isotopic composition of Hg in nature. [ABSTRACT FROM AUTHOR]
- Published
- 2008
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