The National Institute of Standards and Technology uses borate fusion, wavelength dispersive X‐ray fluorescence (WDXRF) spectrometry and synthetic calibration standards for high performance, quantitative analyses of alloys reacted and partially dissolved for fusion into borate beads. Conversion from metal matrix to low Z glass preserves measurement sensitivity. Synthetic calibration standards closely match fused samples, yielding very low uncertainties in results. This approach was applied to zirconium alloys of ≥90% Zr and 17 elements: Al, Co, Cr, Cu, Fe, Hf, Mn, Mo, Nb, Ni, P, Pb, Sn, Ta, Ti, V, and W. To demonstrate capabilities, it was applied to Standard Reference Material (SRM) 360b Zirconium (Sn‐Fe‐Cr) Alloy, renewal SRM 360c, plus discontinued Zr alloy SRMs: 360, 360a, 1210 through 1215, and 1234 through 1239. Eleven elements exhibit biases ≤5% for these SRMs. Additional validation used comparative test methods of inductively coupled plasma (ICP) mass spectrometry, ICP optical emission spectrometry and prompt gamma‐ray activation analysis. This WDXRF method gives results of high enough quality to certify the valid elements in conjunction with results from one or more independent methods. Several phenomena complicate the approach. Normal Zr dissolution using HNO₃ + HF, forms Zr(NO₃)₄ in solution and concentrates it on drying. Zr(NO₃)₄ sublimes at low temperatures, causing uncontrolled loss of Zr as the temperature exceeds 100°C. Rapidly heated Zr(NO₃)₄ may explode. Digestion with HF alone works well. High‐purity ZrO₂ and LiF were used for matrix matching of calibration standards, requiring determinations of trace elements in the high‐purity ZrO₂.

中文翻译：

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硼酸盐熔融和波长色散X射线荧光光谱法定量分析锆合金

美国国家标准技术研究所使用硼酸盐熔融，波长色散X射线荧光（WDXRF）光谱法和合成校准标准物来获得高性能，对反应和部分溶解以熔合为硼酸盐珠粒的合金进行定量分析。从金属基质到低Z玻璃的转换可保持测量灵敏度。合成校准标样与熔融样品紧密匹配，结果不确定度非常低。此方法适用于Zr≥90％和17种元素的锆合金：Al，Co，Cr，Cu，Fe，Hf，Mn，Mo，Nb，Ni，P，Pb，Sn，Ta，Ti，V和W为了演示其功能，已将其应用于标准参考材料（SRM）360b锆（Sn-Fe-Cr）合金，更新的SRM 360c以及已停产的Zr合金SRM：360、360a，1210至1215和1234至1239。这些SRM的11个元素的偏差≤5％。额外的验证使用了电感耦合等离子体（ICP）质谱，ICP发射光谱和快速伽马射线活化分析的比较测试方法。这种WDXRF方法可提供高质量的结果，以结合一种或多种独立方法的结果对有效元素进行认证。有几种现象使该方法复杂化。使用HNO的正常Zr溶解₃  + HF在溶液中形成Zr（NO ₃）₄并将其浓缩干燥。Zr（NO ₃）₄在低温下升华，当温度超过100°C时会导致Zr的失控损失。快速加热的Zr（NO ₃）₄可能会爆炸。仅用HF进行消化即可。高纯度ZrO ₂和LiF用于校准标准品的基质匹配，需要测定高纯度ZrO _2中的痕量元素。