34S Measurements of Sulfur by Multicollector Inductively Coupled Plasma Mass Spectrometry
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- 作者：Robert Clough ; Peter Evans ; Tim Catterick ; E. Hywel Evans
- 刊名：Analytical Chemistry
- 出版年：2006
- 出版时间：September 1, 2006
- 年：2006
- 卷：78
- 期：17
- 页码：6126 - 6132
- 全文大小：195K
- 年卷期：v.78,no.17(September 1, 2006)
- ISSN：1520-6882
文摘
An accurate and precise method for the determination of
34S measurements by multicollector inductively coupledplasma mass spectrometry has been developed. Fulluncertainty budgets, taking into consideration all theuncertainties of the measurement process, have beencalculated. The technique was evaluated by comparingmeasured values with a range of isotopically enrichedsulfur solutions prepared by gravimetric addition of a 34Sspike. The gravimetric and measured results exhibited acorrelation of R2 >0.999. Repeat measurements werealso made after adding Na (up to 420 
g g-1) and Ca (upto 400 g g-1) salts to the sulfur standard. No significantdeviations in the 34S values were observed. The Russellcorrection expression (Ingle, C.; Sharp, B.; Horstwood,M.; Parrish, R.; Lewis, D. J. J. Anal. At. Spectrom.2003, 18, 219) was used to correct for mass bias on the34S/32S isotope amount ratio from the mass bias observedfor the 30Si/28Si isotope amount ratio. Consistent compensation for instrumental mass bias was achieved.Resolution of the measured 34S values was better than1” after consideration of all uncertainty components. Thetechnique was evaluated for practical applications bymeasurement of 34S for a range of mineral waters bypneumatic nebulization sample introduction and theanalysis of genuine and counterfeit pharmaceuticals usingboth laser ablation sample introduction and liquid chromatography. For the former two cases polyatomic interferences were resolved by operating the MC-ICPMS inmedium resolution, while for the chromatographic analyses polyatomic interferences were minimized by the useof a membrane desolvator, allowing the instrument to beoperated at a resolution of 400.
34S measurements by multicollector inductively coupledplasma mass spectrometry has been developed. Fulluncertainty budgets, taking into consideration all theuncertainties of the measurement process, have beencalculated. The technique was evaluated by comparingmeasured values with a range of isotopically enrichedsulfur solutions prepared by gravimetric addition of a 34Sspike. The gravimetric and measured results exhibited acorrelation of R2 >0.999. Repeat measurements werealso made after adding Na (up to 420 g g-1) and Ca (upto 400 g g-1) salts to the sulfur standard. No significantdeviations in the 34S values were observed. The Russellcorrection expression (Ingle, C.; Sharp, B.; Horstwood,M.; Parrish, R.; Lewis, D. J. J. Anal. At. Spectrom.2003, 18, 219) was used to correct for mass bias on the34S/32S isotope amount ratio from the mass bias observedfor the 30Si/28Si isotope amount ratio. Consistent compensation for instrumental mass bias was achieved.Resolution of the measured 34S values was better than1” after consideration of all uncertainty components. Thetechnique was evaluated for practical applications bymeasurement of 34S for a range of mineral waters bypneumatic nebulization sample introduction and theanalysis of genuine and counterfeit pharmaceuticals usingboth laser ablation sample introduction and liquid chromatography. For the former two cases polyatomic interferences were resolved by operating the MC-ICPMS inmedium resolution, while for the chromatographic analyses polyatomic interferences were minimized by the useof a membrane desolvator, allowing the instrument to beoperated at a resolution of 400.