光谱分析用GH4169高温合金质量控制样品的研制

目前国内没有高含量P和Nb的GH4169高温合金标准物质用于检测过程的质量控制,研制的GH4169高温合金质控样品中P和Nb最高含量为0.014%和5.37%,能够满足分析过程质量控制的需求。选择美国和中国生产的4种GH4169高温合金原料加工制备质量控制样品。采用火花放电原子发射光谱法对样品进行测试,用t检验考察原料中各元素面分布和纵向分布的一致性,结果表明各元素无偏析;用方差分析法考察质控样品的均匀性,结果表明样品均匀性良好。质控样品由12家有丰富高温合金检测经验的实验室采用湿法分析定值,确定了Nb、P以及Ni、Cr、Mo、Ti等共12个元素的值及扩展不确定度。采用火花放电原子发射光谱法和X射线荧光光谱法考察了质控样品各元素与镍基有证标准物质的成线性,结果表明质控样品和标准物质有良好的线性关系。

Development of quality control sample of GH4169 superalloy for spectrum analysis

At present, there is no domestic GH4169 certified reference materials with high content of P and Nb for quality control in the testing process. The quality control samples of GH4169 superalloy with the highest content of P and Nb of 0.014% and 5.37% respectively were developed, which could meet the requirement of quality control in analysis process. 4 kinds of GH4169 raw materials produced in USA and China were selected to prepare quality control samples. The samples were determined by spark discharge atomic emission spectrometry, and the consistency of surface distribution and longitudinal distribution of each element in the raw material was investigated by t-test. The results showed that there was no segregation of each element。The homogeneity of the quality control samples was checked by variance analysis, and the results showed that the homogeneity of sample is well. The values and the expanded uncertainty of 12 elements,include Nb, P and Ni, Cr, Mo, Ti, etc. were determined by wet analysis method in 12 laboratories with rich experience in superalloy determination. The linearity between the quality control samples and the nickel-based certified reference materials was investigated by spark discharge atomic emission spectrometry and X-ray fluorescence spectrometry, and the results showed that there was a good linear relationship.