小直径不锈钢棒样品的火花源原子发射光谱分析

Analysis of stainless steel rod sample with small diameter by spark source atomic emission spectrometry

采用自制特制模具制取样品后,把待测样品放入仪器自带的小样品夹具中进行分析,实现了火花源原子发射光谱法对小直径不锈钢棒状样品中碳、硅、锰、磷、硫、铬、镍、钼、铜等元素含量的准确测定。由于目前尚无各种小直径光谱分析标准样品,因此实验从送检的直径6和8mm钢棒中选择表面质量好,经光谱分析检验均匀性良好的棒材,经化学分析定值作为光谱分析的内部控制样品,试验表明应用"控样系数法"修正用块状光谱标样绘制的校准曲线的标准化数据,用以分析棒状样品可消除分析的系统偏差而提高分析的准确度,从而解决了棒状光谱标样绘制校准曲线的困难。对直径6和8mm的不锈钢棒进行精密度考察,结果的相对标准偏差分别在0.51%~2.5%和0.10%~6.3%范围内。对4个小直径不锈钢棒样品进行分析,结果同湿法的测定结果基本一致,且测量误差小于国标GB/T222-2006的标准要求。

After the sample was prepared with a special self-made mode,it was put into the built-in small-sample holder of the analyzer.A spark-source atomic emission spectrometric determination of carbon,silicon,magnesium,phosphorus,sulfur,chromium,nickel,molybdenum,cobalt,etc.in small-diameter stainless steel rod sample was thus established.Because there are no small-diameter reference samples for spectral analysis at present,the rod samples with fine surface quality and homogeneity after spectral detection were selected from the 6nm-and 8nm-diameter steel rods to be sent for detection as internal control sample for spectral analysis after being certified by chemical analysis.It was found that,the system deviation was eliminated and the analysis accuracy was enhanced in the analysis of rod sample by using the standardized data of calibration curve,which was established with block spectral reference sample and corrected by 'control sample coefficient method',thus the difficulty in establishing calibration curve of rod reference sample for spectral analysis was solved.Precision test was conducted on 6nm-and 8nm-diameter stainless steel rods.The relative standard deviation was within 0.51%-2.5% and 0.10%-6.3%,respectively.Four small diameter stainless steel rods samples were analyzed.The results were basically consistent with those obtained by wet methods and the test errors were smaller than the standard requirement of national standard GB/T222-2006.