含钼、铜、铌、氮不锈钢化学和光谱分析系列标准样品的定值研究

Study on characterisation of stainless steel reference materials containing molybdenum,copper,niobium and nitrogen for chemical and spectral analysis

采用纯金属原材料配制原料,选择合理的冶炼及锻轧工艺进行加工,成功研制出了包括高钼、高铜、高铌、高氮在内的20个元素的不锈钢化学分析及光谱分析用系列标准样品。按材料的不同部位选取20块样品,随机排序用火花源原子发射光谱仪进行均匀性检验,双因素方差分析统计处理数据,结果表明本套不锈钢标准样品有良好的均匀性。9家对标准物质定值有丰富经验的单位协作定值,确定了20个元素的认定值及标准不确定度。经同类不锈钢标准样品稳定性考察,此类标准样品稳定性良好,有效期可定为15年。射频辉光放电发射光谱的分析结果进一步证明:本套不锈钢标准样品的各元素成分含量有良好的梯度分布,对定值元素进行成线性考查,线性关系良好。

A series of stainless steel reference materials containing 20 elements including molybdenum, copper, niobium and nitrogen for chemical and spectral analysis were successfully developed by using pure metal as preparation material and adopting proper smelting and forging process. Twenty pieces of samples were selected from different positions of material to do uniformity test with flame atomic absorption spectrometer in random order. The got datas were treated by two-factor analysis of variance. It was indicated that the prepared stainless steel reference materials had good uniformity. The certified value and standard uncertainty of twenty elements were determined by nine organization with abundant experiences in characterisation of reference materials. The stability test of homogeneous stainless steel reference materials showed that the stability of prepared samples was good, and the effective period could be 15 years. The analytical results of radio frequency glow discharge optical emission spectrometry further proved that the content of each element in this series of stainless steel reference materials had good graded distribution. The linear investigation of characterisation elements indicated that the linearity was also good.