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Flow injection of slurries of a lithium borate fusion disc for multi-elemental analysis by mixed-gas inductively coupled plasma mass spectrometry
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2021-08-18 , DOI: 10.1039/d1ja00189b Andrew K. Schug 1 , Diane Beauchemin 1
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2021-08-18 , DOI: 10.1039/d1ja00189b Andrew K. Schug 1 , Diane Beauchemin 1
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A method was devised for the direct analysis of slurries of a lithium borate fused disc of SY-4 (Diorite Gneiss) by ICPMS with a mixed-gas plasma and flow injection for the introduction of slurries into the ICP. Various surfactants and concentrations were tested to homogenously suspend the ground particulate in solution. A 4% (m/m) solution of Triton X-100 in 2% v/v HNO3 was found to produce highly reproducible injection peaks. In an attempt to matrix match the calibration solutions, solid flux powder as well as standard solution Li were added to the calibration solutions. However, both additions failed to adequately correct for the observed effects with/without the use of an internal standard, suggesting a sample introduction problem. To test this, the sample uptake rate was halved, and slurry dilution was increased from 3.2% (m/v) to 0.8% and 0.4% (m/v). With the 0.8% (m/v) suspension, the majority of concentrations (for 11 out of 16 elements) measured by external calibration agreed with the certified values at the 95% confidence level when an 76Ar2+ dimer was used as an internal standard.
中文翻译：
混合气体电感耦合等离子体质谱多元素分析用硼酸锂聚变盘浆液的流动注射
设计了一种通过 ICPMS 直接分析 SY-4（闪长岩片麻岩）硼酸锂熔凝盘的浆液的方法，采用混合气体等离子体和流动注射将浆液引入 ICP。测试了各种表面活性剂和浓度以在溶液中均匀悬浮磨碎的颗粒。Triton X-100 在 2% v/v HNO 3 中的4% (m/m) 溶液发现可产生高度重现的进样峰。为了与校准溶液进行基质匹配，将固体助焊剂粉末和标准溶液 Li 添加到校准溶液中。然而，这两种添加都未能充分校正使用/不使用内标时观察到的效果，表明存在样品引入问题。为了测试这一点，将样品吸收率减半，并将浆液稀释度从 3.2% (m/v) 增加到 0.8% 和 0.4% (m/v)。对于 0.8% (m/v) 悬浮液，当使用76 Ar 2 +二聚体作为内部校准时，通过外部校准测量的大多数浓度（16 种元素中的 11 种）与认证值一致，置信度为 95%标准。
更新日期：2021-08-25
中文翻译：
混合气体电感耦合等离子体质谱多元素分析用硼酸锂聚变盘浆液的流动注射
设计了一种通过 ICPMS 直接分析 SY-4（闪长岩片麻岩）硼酸锂熔凝盘的浆液的方法，采用混合气体等离子体和流动注射将浆液引入 ICP。测试了各种表面活性剂和浓度以在溶液中均匀悬浮磨碎的颗粒。Triton X-100 在 2% v/v HNO 3 中的4% (m/m) 溶液发现可产生高度重现的进样峰。为了与校准溶液进行基质匹配，将固体助焊剂粉末和标准溶液 Li 添加到校准溶液中。然而，这两种添加都未能充分校正使用/不使用内标时观察到的效果，表明存在样品引入问题。为了测试这一点，将样品吸收率减半，并将浆液稀释度从 3.2% (m/v) 增加到 0.8% 和 0.4% (m/v)。对于 0.8% (m/v) 悬浮液，当使用76 Ar 2 +二聚体作为内部校准时，通过外部校准测量的大多数浓度（16 种元素中的 11 种）与认证值一致，置信度为 95%标准。
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