火花放电原子发射光谱法测定铬不锈钢中砷锡锑铅  

Determination of arsenic,tin,antimony and lead in chromium stainless steel by spark discharge atomic emission spectrometry

作　　者：张晨慧 顾春峰[1] 张毅[1] ZHANG Chenhui;GU Chunfeng;ZHANG YiAuthor information-(Central Research Institute,Baoshan Iron and Steel Co.,Ltd.,Shanghai 201900,China)

机构地区：[1]宝山钢铁股份有限公司中央研究院,上海201900

出　　处：《冶金分析》2025年第2期64-69,共6页Metallurgical Analysis

摘　　要：铬不锈钢具有良好的抗氧化性和耐腐蚀性,其中As、Sn、Sb、Pb会影响铬不锈钢材料的塑性和强度,因此As、Sn、Sb、Pb的检测对判断钢材质量具有重要意义。在日常分析中,大多采用原子吸收光谱法(AAS)或电感耦合等离子体原子发射光谱法(ICP-AES)进行测定,但上述方法操作流程复杂、分析周期长且检测范围有限。本文研究了火花放电原子发射光谱法分析铬不锈钢中微量/痕量As、Sn、Sb、Pb的方法,选用国内外铬不锈钢标准物质/样品及内部控制样品建立校准曲线。试验优化了预燃时间和积分时间,当预燃时间为9 s、积分时间为6 s时,As、Sn、Sb、Pb的发射光谱强度最稳定。通过曲线回归扣除干扰元素对各标准曲线的干扰。实验方法中As、Sn、Sb、Pb的定量限分别为0.000 3%、0.001 3%、0.000 5%、0.000 06%(质量分数,下同)。按照实验方法选择了As、Sn、Sb、Pb含量为0.000 4%~0.011%的两个铬不锈钢试样进行精密度试验,结果的相对标准偏差(RSD,n=10)均不超过5%;选择5块铬不锈钢光谱标准物质/样品和3块铬不锈钢样品进行正确度试验,结果表明本方法的测定值与标准物质/样品的认定值/标准值以及石墨炉原子吸收光谱法的测定值具有良好的一致性。Chromium stainless steel has good properties in oxidation resistance and corrosion resistance.The contents of As,Sn,Sb and Pb will affect the plasticity and strength of chromium stainless steel materials,so the detection of As,Sn,Sb and Pb is of great significance for judging the quality of steel.In daily analysis,the atomic absorption spectrometry(AAS)or inductively coupled plasma atomic emission spectrometry(ICP-AES)is mostly used for measurement.However,the above methods have some shortcomings such as complex operation procedure,time-consuming process and limited detection range.In this paper,the determination method of micro/trace As,Sn,Sb and Pb in chromium stainless steel by spark source atomic emission spectrometry was investigated.The calibration curves were prepared using domestic and imported chromium stainless steel standard samples and self-made internal control samples.The pre-burn time and integration time were optimized.It was found that the excitation intensity of As,Sn,Sb and Pb was most stable when the pre-burn time was 9 s and the integration time was 6 s.The interference of elements with the calibration curves was deducted by curvilinear regression.The limit of quantification for As,Sn,Sb and Pb was 0.0003%,0.0013%,0.0005%and 0.00006%(mass fraction,similarly hereinafter),respectively.The samples of chromium stainless steel with As,Sn,Sb and Pb contents in range of 0.0004%-0.011%were selected for precision experiments according to the experimental method.The relative standard deviations(RSD,n=10)of determination results were all less than 5%.Five chromium stainless steel standard samples and three chromium stainless steel samples were selected for accuracy experiments,and the results showed that the measured values of this method were consistent with the standard value/certified value of the standard samples and those obtained by the graphite furnace atomic absorption spectrometry.

关 键 词：火花放电原子发射光谱法 铬不锈钢 五害元素 砷 锡 锑 铅 

分 类 号：O657.31[理学—分析化学]