辉光放电原子发射光谱法测定不锈钢中宽范围含量钴  

Determination of cobalt with wide content range in stainless steel by glow discharge optical emission spectrometry

作　　者：胡维铸 王亚朋 牟英华 唐语 王伟 HU Weizhu;WANG Yapeng;MU Yinghua;TANG Yu;WANG Wei(Technical Center of Ben Gang Group Corporation,National and Local Joint Engineering Laboratory of Advanced Automotive Steel Development and Application Technology,Benxi 117000,China)

机构地区：[1]本钢集团有限公司技术中心,先进汽车用钢开发与应用技术国家地方联合工程实验室,辽宁本溪117000

出　　处：《冶金分析》2023年第5期27-31,共5页Metallurgical Analysis

摘　　要：钴元素含量及其变化直接影响不锈钢材料性能,准确测定不锈钢中钴成分并对其严格控制对保证和提高不锈钢材料性能具有重要意义。通过优化仪器参数,用7块不同钴含量的不锈钢标准物质绘制校准曲线,建立了辉光放电原子发射光谱法(GD-OES)测定不锈钢中宽范围含量钴的方法。考察了仪器参数对钴测定的影响,优化后仪器参数为激发电流45 mA、激发电压1 100 V、预燃时间75 s、积分时间10 s。实验表明,钴在质量分数为0.008%~1.55%范围内与其对应的光谱强度呈良好的线性关系,线性相关系数为0.990 5。方法检出限为1.2μg/g,定量限为4.0μg/g。将实验方法应用于不锈钢标准样品和实际样品中钴含量的测定。结果表明:对于标准样品,测定值与标准值基本一致,测定结果的相对标准偏差(RSD,n=9)为0.71%~1.2%;对于实际样品,钴测定值为1.48%、0.62%、0.128%,与GB/T 223.65—2012中的火焰原子吸收光谱法及GB/T 223.22—1994中的亚硝基R盐光度法基本一致,测定结果的相对标准偏差(RSD,n=9)为1.1%~1.6%。The cobalt content and its variation directly affect the properties of stainless steel.The accurate determination and strict control of cobalt content in stainless steel has important significance to guarantee and improve the properties of stainless steel.The instrumental parameters were optimized.Seven reference materials of stainless steel with different cobalt contents were selected to prepare the calibration curves.A method for the determination of cobalt with wide content range in stainless steel by glow discharge optical emission spectrometry(GD-OES)was established.The influence of instrument parameters on the determination of cobalt was investigated,and the optimized conditions were as follows:the discharge current was 45 mA;the discharge voltage was 1100 V;the pre-burning time was 75 s;the integration time was 10 s.The experimental results showed that there was a good linear relationship between the spectral intensity of cobalt and its mass fraction in the range of 0.008%-1.55%,and the linear correlation coefficient was 0.9905.The limit of detection was 1.2μg/g,and the limit of quantification was 4.0μg/g.The proposed method was applied to the determination of cobalt content in reference materials and actual samples of stainless steel.The results showed that the found results of reference materials were basically consistent with the certified values,and the relative standard deviations(RSD,n=9)were between 0.71%and 1.2%.For the actual samples,the determination results were 1.48%,0.62%and 0.128%,respectively,which were basically consistent with those obtained by flame atomic absorption spectrometry in GB/T 223.65-2012 and the nitroso-R salt spectrophotometry in GB/T 223.22-1994.The RSDs(n=9)of determination results were between 1.1%and 1.6%.

关 键 词：辉光放电原子发射光谱法(GD-OES) 不锈钢 钴 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]