We developed a fusion glass disc technique using small-size samples (30 mg) for assaying precious siliceous samples of geochemical reference materials using wavelength-dispersive X-ray fluorescence determination of major (SiO₂, TiO₂, Al₂O₃, TFe₂O₃, MnO, MgO, CaO, Na₂O, K₂O, and P₂O₅) and minor (Ni, Sr, and Zr) elements. The normal-size glass discs (approximately 30 mm in diameter) were prepared using an automatic fluxer, combined with manual preparation, with a flux to sample ratio of 100 : 1. GSR-1 and GSR-3 were selected to evaluate the results obtained using XRF, ICP-OES (fusion), and ICP-OES (acid attack) and to assess the accuracy and precision of the three methods based on Whitty-Léveillé and coworkers' protocol. In the present work, a set of 46 rock certified reference materials (CRMs) was used to calibrate the spectrometer and another set of 16 CRMs was analyzed further to validate the accuracy and precision of the procedure. The homogeneity of the discs was evaluated using the μ-XRF mapping image technique. In general, we obtained good agreement with the recommended values for most determinations. Finally, we summarized the small-size sample methods published in recent years and compared the advantages and disadvantages of these methods in detail.

中文翻译：

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用于地质样品X射线荧光分析的1：100稀释熔融玻璃微珠的定量验证

我们开发了一种使用小尺寸样品（30 mg）的熔融玻璃圆盘技术，用于通过波长色散X射线荧光光谱法测定主要（SiO ₂，TiO ₂，Al ₂ O ₃，TFe ₂ O ₃，MnO，MgO，CaO，Na ₂ O，K ₂ O和P ₂ O ₅）和次要元素（Ni，Sr和Zr）。使用自动助熔剂结合手动制备来制备标准尺寸的玻璃圆盘（直径约30 mm），通量与样品的比率为100：1。选择GSR-1和GSR-3评估获得的结果使用XRF，ICP-OES（融合）和ICP-OES（酸侵蚀），并根据Whitty-L​​éveillé和同事的协议评估这三种方法的准确性和精密度。在当前的工作中，一组46种岩石认证参考材料（CRM）用于校准光谱仪，另一组16种CRMs被进一步分析以验证该方法的准确性和精确性。使用μ-XRF映射图像技术评估光盘的均匀性。通常，对于大多数测定，我们都与推荐值获得了很好的一致性。最后，