制定碳素钢火花放电原子发射光谱标准的精密度研究

摘要

The new version of national standard GB/T 4336-2016 Carbon and low-alloy steel—Determination of multi-element contents—Spark discharge atomic emission spectrometric method (routine method) has been implemented in November 1,2016.A significant difference compared with the 2002 version was the narrowed quantitative range,and this change of the new standard was caused by the newest ISO technical report (ISO TR 21074-2016).In order to facilitate the daily analysis work in the laboratory,CSTM social organization standard by spark discharge atomic emission spectrometry was formulated to expand the lower end of the range considering of the characteristics of carbon steel determination of C,Si,Mn,P,S,Cr,Ni,Mo,V,Al,Ti,Cu,Nb,Co,B,Zr,As,Sn,N,Ca and Sb's low content range.In the development process of CSTM standard,the technique of the recalibration to the low content elements was used innovatively,and these requirements in the standard for low content section of elements were strictly stipulated.To the statistic results of the inter-laboratory study,spark discharge atomic emission spectrometric CSTM social organization standard combined the ISO TR 21074-2016 report to determine the quantitative range of standard methods at home and abroad for the first time.How to process the inter-laboratory research according to the relevant rules of ISO standard was described,and the statistic results of the inter-laboratory study were ideal.%新版国家标准GB/T4336-2016《碳素钢和中低合金钢多元素含量的测定火花放电原子发射光谱法(常规法)》已于2016年11月1日实施,相较于2002版标准的显著差异之一是分析范围变窄,而这种变化的产生是由于新版标准是严格按照ISO有关最新技术报告(ISO TR 21074-2016)制定.为便于实验室开展日常分析工作,针对碳素钢中元素碳、硅、锰、磷、硫、铬、镍、钼、钒、铝、钛、铜、铌、钴、硼、锆、砷、锡、氮、钙、锑的低含量范围,制定火花放电原子发射光谱的中国材料与试验团体标准委员会(CSTM)团体标准以拓展国标分析范围下限.团体标准制定过程中,在技术上创新性地采用了元素低含量段二次校正的方法,并在标准中对低含量段火花放电原子发射光谱分析的技术要求作了严格规定;对于共同试验的结果统计,在国内、国际首次根据ISO TR 21074-2016确定标准方法最终测定范围.将团体标准在制定过程中如何按照ISO有关规程进行实验室间研究的过程展开说明,获得了理想的结果.