材料期刊网

应用X射线荧光光谱仪（XRF ）分析金属及合金样品，选择熔融制样有助于获取更准确的样品组成信息。为避免熔融过程中样品腐蚀铂黄坩埚，实验通过在熔融前以酸或碱消解样品的预氧化方式消除隐患，将金属转化为盐类，从而实现安全可靠的熔融操作。酸消解方法中先加入HBr避免样品钝化，随后加入过量 HNO3除Br－并进一步溶解，所得溶液蒸干后即可熔融；某些特定类型的样品如铝制品可考虑碱液消解，以LiOH溶液溶样，HNO3酸化，随后蒸干熔样。所得样片经无标定量分析可获得相对准确的主含量信息，对By1901‐2铜合金样品平行实验（n＝6）显示主含量元素测定结果的相对标准偏差RSD＜7％，同时实验也为建立定量的X射线荧光光谱对金属及合金分析方法提供了思路。

During the analysis of metal and alloy samples by X‐ray fluorescence spectrometry (XRF) ,the sample preparation by fusion method was advantageous to obtain more accurate composition information . In order to avoid the corrosion of platinum‐gold crucible by sample during fusion process ,the sample was pre‐oxidized by acid dissolution or alkali digestion before fusion .The metals were translated to the salts , realizing the safe and reliable fusion operation .In acid dissolution method ,HBr was firstly added to avoid the passivation of sample .Then ,excessive HNO3 was added for the further dissolution and the removal of Br- .The solution was evaporated to dryness followed by fusion .Some special samples such as aluminum products could be digested with alkali solution .The sample was dissolved with LiOH followed by acidifica‐tion with HNO3 .The solution was evaporated to dryness for fusion .The relatively accurate content infor‐mation of major components could be obtained by quantitative analysis without standard sample .The par‐allel experiments of By1901‐2 copper alloy sample (n= 6 ) indicated that the relative standard deviation (RSD) of major components were less than 7% .Meanwhile ,the study provided idea for the quantitative a‐nalysis of metals and alloys by XRF .