铜–铬–锆合金光谱分析用标准物质的研制

以电解铜和铜–铬、铜–锆中间合金为原材料,通过真空熔炼和热锻加工工艺,研制了铜–铬–锆合金光谱分析用标准物质。将样品分成4组,每组85块后,采用金相检验和光电直读光谱仪进行均匀性、稳定性和定值分析。从样品中随机抽取15块进行均匀性检验,经F检验表明,在95%的置信区间范围内样品均匀性良好;稳定性考察12个月,结果表明在考察期间内样品稳定性良好;标准物质样品经国内3家具有分析资质的实验室进行协作定值,并评定了定值结果的不确定。铜–铬–锆合金标准物质样品中Cr,Zr元素的相对扩展不确定度分别为0.015%~0.036%,0.019%~0.033%(k=2)。该标准物质达到了国家标准物质的技术要求,可用于有关铜–铬–锆合金产品中铬、锆元素的方法校准和质量控制。

Development of Cu-Cr-Zr-Alloy Certiifed Reference Material for Spectral Analysis

The Cu–Cr–Zr–alloy certified reference material(CRM) for spectral analysis was developed. Using electrolytic copper,Cu–Cr,Cu–Zr master alloys as raw material,the CRM was melted in the vacuum arc furnace,then forged using hot forging process. The Cu–Cr–Zr–alloy was divided into 4 sets and 85 pieces per set. The homogeneity and stability testing and quantitative analysis were evaluated by metallographic test and photoelectric direct reading spectrometer. According to analysis procedure of homogeneity,15 pieces of sample were randomly taken from every 85 pieces,and the results were validated by F-test statistical method. The stability inspection was carried on the short-term(12 months),and the results indicated that the stability was good. A cooperative certification was conducted by 3 qualified laboratories. The relative expanded uncertainty for Cr and Zr elements of Cu–Cr–Zr–alloy reference material was 0.015%–0.036%, 0.019%–0.033%(k=2), respectively. The reference material can conform to the technical requirement of the certified reference material. The reference material was intended for use in the method validation and quality control regarding Cr and Zr elements in the Cu–Cr–Zr–alloy.