National Institute of Metrology, Beijing, 100029, China.
Anal Bioanal Chem. 2018 Nov;410(27):7195-7201. doi: 10.1007/s00216-018-1324-z. Epub 2018 Sep 3.
High-purity silicon power was doped with standard solutions containing 15 elements, and a high-purity indium tablet was prepared by the melting of indium pellets. An In-Si tablet, which is mechanically stable and thus suitable as a calibration sample, was prepared by our pressing the doped silicon power on the high-purity indium tablet. The matrix effect was studied by our investigating the variations of measured mass fractions (standard relative sensitivity factor, StdRSF, calibration) of doped impurities in the In-Si tablet, which provides a series of matrixes with different mass ratios of In to Si. For all the elements, the relative standard deviations of the measured mass fractions of impurities were less than 30%. The RSFs of the glow discharge mass spectrometer (Element GD) were obtained, and the results showed that three RSFs derived from the In-Si tablet with low, intermediate and high mass ratios of In to Si, respectively, agreed with the mean RSF within an uncertainty interval of 30%. The measurement of Fe and Al matrix certified reference materials further demonstrated that the RSFs generated from a matrix can be used for the calibration of another matrix, and the uncertainty was within 30%. Finally, another doped silicon powder was measured with the glow discharge mass spectrometer, which was calibrated by the mean RSFs from the In-Si tablet, and the analytical results obtained by glow discharge mass spectrometry are in good agreement with the analytical results obtained by high-resolution inductively coupled plasma mass spectrometry. Graphical abstract ᅟ.
高纯硅粉经标准溶液掺杂，标准溶液含 15 种元素，铟丸经熔融制备高纯铟片。通过将掺杂硅粉压在高纯铟片上，我们制备了机械稳定的 In-Si 片，可作为校准样品。通过研究掺杂杂质在 In-Si 片中的测量质量分数（标准相对灵敏度因子，StdRSF，校准）的变化，我们研究了基体效应，In-Si 片提供了一系列不同 In 与 Si 质量比的基体。对于所有元素，杂质测量质量分数的相对标准偏差均小于 30%。获得了辉光放电质谱仪（Element GD）的 RSF，结果表明，分别来自 In 与 Si 质量比低、中、高的三个 In-Si 片的三个 RSF 在不确定度间隔 30%内与平均 RSF 一致。Fe 和 Al 基体标准物质的测量进一步证明了来自基体的 RSF 可用于另一个基体的校准，且不确定度在 30%以内。最后，使用辉光放电质谱仪测量了另一种掺杂硅粉，采用 In-Si 片的平均 RSF 进行校准，辉光放电质谱法的分析结果与高分辨率电感耦合等离子体质谱法的分析结果吻合良好。
