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采用离子-分子反应的电感耦合等离子体质谱法消除氧化物干扰并测定土壤中的痕量银。

Elimination of oxide interferences and determination of ultra-trace silver in soils by ICP-MS with ion-molecule reactions.

机构信息

Key Laboratory of Biogeology and Environmental Geology of Ministry of Education, Faculty of Earth Sciences, China University of Geosciences, Wuhan 430074, PR China.

出版信息

Sci Total Environ. 2011 Jul 1;409(15):2981-6. doi: 10.1016/j.scitotenv.2011.04.011.

Abstract

Silver is subject to significant spectral interferences caused by high concentrations of Zr, Nb, Mo and Y in inductively coupled plasma mass spectrometry (ICP-MS) analysis for soil or sediment samples. In this study, the Zr, Nb, and Mo based oxide and/or hydroxide polyatomic interferences were successfully eliminated by ion-molecule reactions in a dynamic reaction cell (DRC). These potentially interfering ions ⁹³Nb¹⁶O+, ⁹²Zr¹⁶OH+ and ⁹²Mo¹⁶OH+ on ¹⁰⁹Ag+ were rapidly oxidized to higher oxides ⁹³NbO₂+, ⁹²ZrO₂H+/⁹²ZrO₂H+ and ⁹²MoO₂H+ by O₂ as the reaction gas in DRC. However, interfering ions ⁸⁹Y¹⁸O+ and ⁹¹Zr¹⁶O+ on ¹⁰⁷Ag cannot be removed by this method, because the reaction rates of ZrO+ and YO+ to ZrO₂+/ZrO₃+ and YO₂+/YO₃+ were too low. Under the optimized O₂ flow rate (2.4 mL min⁻¹) and DRC rejection parameter q (Rpq, 0.75), the background signal was reduced by up to 100-fold at m/z 109 and the limit of quantitation (LOQ, 10σ) for ¹⁰⁹Ag was 0.5 ng g⁻¹. The proposed method was used to determine the concentration of Ag in twenty-eight soil standard reference materials (SRMs). The accuracy of the results suggests that the method has great potential for the direct determination of trace or ultra-trace levels of Ag in various environmental samples.

摘要

银在电感耦合等离子体质谱(ICP-MS)分析土壤或沉积物样品时,受到 Zr、Nb、Mo 和 Y 高浓度引起的显著光谱干扰。在这项研究中,通过在动态反应池(DRC)中离子-分子反应成功消除了基于 Zr、Nb 和 Mo 的氧化物和/或氢氧化物多原子干扰。这些潜在的干扰离子 ⁹³Nb¹⁶O+、⁹²Zr¹⁶OH+和 ⁹²Mo¹⁶OH+在 DRC 中迅速被 O₂作为反应气体氧化为更高的氧化物 ⁹³NbO₂+、⁹²ZrO₂H+/⁹²ZrO₂H+和 ⁹²MoO₂H+。然而,这种方法不能去除干扰离子 ⁸⁹Y¹⁸O+和 ⁹¹Zr¹⁶O+,因为 ZrO+和 YO+与 ZrO₂+/ZrO₃+和 YO₂+/YO₃+的反应速率太低。在优化的 O₂流速(2.4 mL min⁻¹)和 DRC 排斥参数 q(Rpq,0.75)下,在 m/z 109 处的背景信号降低了 100 倍,109Ag 的定量限(LOQ,10σ)为 0.5 ng g⁻¹。该方法用于测定 28 个土壤标准参考物质(SRM)中 Ag 的浓度。结果的准确性表明,该方法在直接测定各种环境样品中痕量或超痕量 Ag 方面具有很大的潜力。

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