火花放电原子发射光谱法测定奥氏体易切削不锈钢中高含量硫  

Determination of high content sulfur in austenitic free-cutting stainless steel by spark discharge atomic emission spectrometry

作　　者：张征宇[1,2] 芦飞[1,2] 赵卫星[1,2] ZHANG Zhengyu;LU Fei;ZHAO Weixing(State Key Laboratory of Advanced Stainless Steel Material,Taiyuan Iron&Steel(Group)Co.,Ltd.,Taiyuan 030003,China;Technology Center,Shanxi Taigang Stainless Steel Co.,Ltd.,Taiyuan 030003,China)

机构地区：[1]太原钢铁(集团)有限公司先进不锈钢材料国家重点实验室,山西太原030003 [2]山西太钢不锈钢股份有限公司技术中心,山西太原030003

出　　处：《冶金分析》2022年第1期43-49,共7页Metallurgical Analysis

摘　　要：奥氏体易切削不锈钢中S含量(质量分数,下同)大于0.2%,常规的测量方法有红外吸收法和电感耦合等离子体原子发射光谱法(ICP-AES),而上述分析方法存在制样慢、分析元素种类少等缺点,不能满足炉前炼钢的快速分析要求。实验采用火花放电原子发射光谱法研究了奥氏体易切削不锈钢中高含量S的分析技术。首先通过分析奥氏体易切削不锈钢样品的化学和物理特性,对制样方法进行了考察,然后探讨了火花放电原子发射光谱法的测量条件以及干扰元素对分析结果的影响。研究表明,统一奥氏体易切削不锈钢样品的制样方法,得到相同的测量表面;火花放电原子发射光谱仪使用新激发电极;保持奥氏体易切削不锈钢样品在纯度不低于99.995%的氩气环境中激发,设定预燃时间50 s,测量时间12 s(800 Hz);绘制奥氏体易切削不锈钢0.1%~0.4%含量范围内S的专用校准曲线,能准确得到奥氏体易切削不锈钢样品中高含量S的分析结果。S含量分别为0.122%、0.264%、0.387%的奥氏体易切削不锈钢样品测量结果的相对标准偏差(RSD,n=11)分别为3.8%、1.3%和0.81%,利用t分布临界值(t;=2.262)检验火花放电原子发射光谱法和红外吸收法分析结果,检验结果小于临界值。表明火花放电原子发射光谱法的测定结果与红外吸收法测定结果无明显差异,可以稳定测量奥氏体易切削不锈钢中S。The content of sulfur(mass fraction, similarly hereinafter) in austenitic free-cutting stainless steel is higher than 0.2%. The conventional measurement methods include infrared absorption and inductively coupled plasma atomic emission spectrometry(ICP-AES). However, these methods have some shortcomings such as slow sample preparation speed and few types of analytical elements, which cannot meet the rapid analysis requirements of steelmaking process. The analysis method of high content sulfur in austenitic free-cutting stainless steel by spark discharge atomic emission spectrometry was studied in experiments. The chemical and physical properties of austenitic free-cutting stainless steel sample were firstly analyzed, and the sample preparation method was investigated. Then the effects of measurement conditions and interference elements on the analytical results by spark discharge atomic emission spectrometry were discussed. The results showed that the sample preparation method of austenitic free-cutting stainless steel was unified to obtained the same measurement surface. New excitation electrode was used for the spark discharge atomic emission spectrometer. The austenitic free-cutting stainless steel sample was excited in the argon environment with purity not less than 99.995%. The precombustion time was 50 s and the measurement time was 12 s(800 Hz). The special calibration curve of sulfur with content range of 0.1%-0.4% in austenitic free-cutting stainless steel was drawn. The analytical results of high content sulfur in austenitic free-cutting stainless steel sample could be accurately obtained. For the austenitic free-cutting stainless steel samples with sulfur content of 0.122%, 0.264% and 0.387%, the relative standard deviation(RSD, n=11) of determination results was 3.8%, 1.3% and 0.81%, respectively. The t distribution critical value(t;=2.262) was adopted to check the analytical results of spark discharge atomic emission spectrometry and infrared absorption method, and the inspection result was less than

关 键 词：奥氏体易切削不锈钢 高硫 火花放电原子发射光谱法 熔融法 

分 类 号：O657.31[理学—分析化学] TF764.1[理学—化学]