钐钴合金中氧元素系列标准样品的研制及定值溯源性探讨  

Development on oxygen element series certified reference material of samarium-cobalt alloy and discussion on traceability of calibration value

作　　者：任旭东[1] 于勇海[1] 常诚[1] 张秀艳[1] REN Xudong;YU Yonghai;CHANG Cheng;ZHANG Xiuyan(Baotou Research Institute of Rare Earths,Baotou 014010,China)

机构地区：[1]包头稀土研究院,内蒙古包头014010

出　　处：《冶金分析》2024年第3期36-45,共10页Metallurgical Analysis

摘　　要：目前,各种样品中的氧元素均采用脉冲熔融红外吸收法进行测定,缺乏基体一致的标准样品进行曲线校正是日常检测更是标准样品研制过程中亟待解决的问题。本文主要探讨了在钐钴合金系列标准样品定值过程中定值检测方法溯源性的问题,验证了不同定值方法对定值结果一致性的影响,从而保证了本文研制系列标准样品定值的准确性。考察了熔融温度对粉末和块状两种形态钐钴合金样品、钛合金标准样品、铜合金标准样品中氧元素释放程度的影响,结果表明,设置仪器功率高于4.4 kW且熔融温度大于1200℃可以保证定值结果的溯源性;采用基准试剂法进行量值溯源性试验,结果满意;分别采用基准试剂法、中子活化法、行业标准XB/T 610.3—2015中的脉冲熔融红外吸收法对本文研制的标准样品进行测定,3种方法的一致性满足标准样品定值要求。在对标准样品的均匀性、稳定性考察的基础上,采用多家实验室协作定值的方式,分别以基准试剂法、中子活化法、行业标准XB/T 610.3—2015中的脉冲熔融红外吸收法为定值方法,确定了所研制的钐钴合金系列标准样品的标准值和扩展不确定度。本文为钐钴合金中氧含量的测定提供实物保障并为其他类型尚无同类标准样品作为定值溯源的氧元素标准样品研制提供了参考。At present,oxygen element in various samples is determined by pulse fusion infrared absorption method.The lack of certified reference materials(CRMs)with consistent matrix for curve correction is an urgent problem for daily detection and the development process of CRMs.This paper mainly focused on the issue of traceability of calibration methods in the calibration process of samarium-cobalt alloy series CRMs.The influence of different calibration methods on the consistency of calibration results was verified to ensure the accuracy of calibration values for series CRMs.The influence of fusion temperature on the degree of oxygen release in powder and bulk samarium-cobalt alloy samples,titanium alloy CRMs,and copper alloy CRMs was investigated.The results showed that the traceability of the calibration results could be guaranteed when the instrument power was above 4.4 kW and the fusion temperature was above 1200℃.The traceability test was conducted by primary reagent method,and the results were satisfactory.The developed CRMs were determined by primary reagent method and neutron activation method,as well as pulse fusion infrared absorption method in industrial standard of XB/T 610.3-2015,respectively.It was found that the consistency of three methods could meet the requirements for CRMs calibration.On the basis of investigating the uniformity and stability of CRMs,the standard values and expanded uncertainties of series CRMs were determined respectively by primary reagent method,neutron activation method,and pulse fusion infrared absorption method in industry standard of XB/T 610.3-2015 as the calibration methods through the collaboration of multiple laboratories.This paper provided a physical guarantee for determination of oxygen element in samarium-cobalt alloy and also provided a reference for the development of oxygen element CRM for other types that had no similar CRMs as calibration value traceability.

关 键 词：钐钴合金 氧元素标准样品 标准样品研制 定值溯源 基准试剂法 中子活化法 脉冲熔融红外吸收法 

分 类 号：O659.2[理学—分析化学] TG146.45[理学—化学]