Abstract：During the composition analysis by spark discharge atomic emission spectrometry, a test block with the same content and uniform composition is usually required as the control sample to establish the test program. Therefore, it is necessary to conduct the homogeneity test on the selected control sample test block. In order to inspect the homogeneity of control sample of nickel base alloy by variance analysis according to YB/T 4143-2019, the precision of the test method should be further analyzed. The judgement results are only reliable when the method used in the control sample test has the same repeatability as the method used in daily practice. INCONEL 718 was used as an example for homogeneity test. The analysis results showed that the reproducibility variance of the test method was large, and there was a possibility that the non-uniform samples were judged to be uniform.The drift of the test system was corrected by interpolation method, and the uniformity test parameters were recalculated. The results showed that the test results of Fe element before drift correction were uniform,while the test results after drift correction were not uniform.The results of homogeneity test for other elements were relatively uniform except for Fe. The root cause of the inhomogeneity distribution of Fe element as Balance element was discussed. Moreover, this test block was used as a control sample to test the chemical composition of certified reference material GH4169. The accuracy of the test results was accordant with the requirements in GB/T38939-2020 and literatures. The proposed method was suitable for the uniformity test of self-made spark discharge atomic emission spectral control samples in industrial and mining enterprises.
李红. 镍基合金控样均匀性初检探讨[J]. 冶金分析, 2021, 41(11): 15-20.
LI Hong. Investigation on homogeneity initial test of control sample of nickel base alloy. , 2021, 41(11): 15-20.
[1] 赵静,张凯,李乃洁.方差分析法和极值法统计在样本均匀性检验中的应用[J].品牌与标准化,2011,16:42. ZHAO Jing,ZHANG Kai,LI Naijie.Application of analysis of variance and extreme value method in sample uniformity test[J].Brand and Standizaition,2011,16:42. [2] 张勇,贾云海,刘英.光谱分析用标准物质/样品均匀性初检的符合性评价[J].冶金分析,2011,31(8):22-25. ZHANG Yong,JIA Yunhai,LIU Ying.Evaluation of conformity in initial homogeneity in section of certified reference materials/samples for spectral analysis[J].Metallurgical Analysis,2011,31(8):22-25. [3] 张勇,刘英,臧慕文.光谱分析用标准物质/样品均匀性不同检验规则比较及其不确定度评定[J].分析试验室,2011,30(1):76-79. ZHANG Yong,LIU Ying,ZANG Muwen.Comparision of standard practice for testing homogeneity of certified refrence material and its evaluation of uncertainty for spectroscopic analysis[J].Chinese Journal of Analysis Laboratory,2011,30(1):76-79. [4] 顾文佳,张懿翔,许超.运用统计学方法对能力验证定性样品的均匀性和稳定性进行评价[J].食品安全质量检测学报,2019,10(21):7138-7141. GU Wenjia,ZHANG Yixiang,XU Chao.Evaluation of the homogeneity and stability of qualitative samples in the proficiency test with statistical methods[J].Journal of Food Safety and Quality,2019,10(21):7138-7141. [5] 中华人民共和国工业和信息化部.YB/T 4143—2019火花源原子发射光谱法测定固体金属均匀性检验方法[S].北京:冶金工业出版社,2019. [6] 贾云海,孙晓飞.火花放电原子发射光谱分析全流程正确度控制方法研究[J].冶金分析,2020,40(7):1-7. JIA Yunhai,SUN Xiaofei.Research on trueness control method of full process in spark discharge atomic emission spectro metric analysis[J].Metallurgical Analysis,2020,40(7):1-7. [7] 田衎,贺岩涛,张覃.环境标准样品均匀性检验数据漂移校正方法探讨[J].岩矿测试,2020,39(3):425-433. TIAN Kan,HE Yantao,ZHANG Qin.Discussion on the data drift correction method in homogeneity assessment of environmental reference materials[J].Rock and Mineral Analysis,2020,39(3):425-433. [8] 徐永萍.ARL4460金属分析仪中旋转校正法的应用[J].中国化工贸易,2018,10(9):112. XÜ Yongping.Application of rotation correction method in ARL4460 metal analyzer[J].China Chemical Trade,2018,10(9):112.
