Abstract: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 (t0.975,9=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 the critical value. It indicated that there was no obvious different between the determination results of spark discharge atomic emission spectrometry and infrared absorption method. The proposed method could be used to stably determine the content of sulfur in austenitic free-cutting stainless steel.
[1] Soon-Tae Kim,Yong-Soo Park.Effects of copper and sulfur additions on machinability behavior of high performance austenitic stainless steel[J].Met. Mater. Int.,2009,15(2):221-230. [2] 徐建平,程德翔.电感耦合等离子体原子发射光谱法测定钢中硫时空白与背景[J].冶金分析,2016,36(11):71-75. XU Jianping,CHENG Dexiang.Blank and background during determination of sulfur in steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(11):71-75. [3] 刘伟洪,向懋笔,杨峰.基于硝酸-氯酸钠溶样体系-电感耦合等离子体发射光谱法测定地质样品中的总硫[J].化学世界,2019,60(11):14-18. LIU Weihong,XIANG Maobi,YANG Feng.Determination of total sulfur in geological sample by ICP-OES based on the system of nitric acid,sodium chlorate dissolve sample[J].Chemical World,2019,60(11):14-18. [4] 王艳君,周蕾,蒋晓光.电感耦合等离子体原子发射光谱法测定高硫铜磁铁矿中硫[J].冶金分析,2019,39(12):61-66. WANG Yanjun,ZHOU Lei,JIANG Xiaoguang.Determination of sulfur in high-sulfur copper magnetite by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2019,39(12):61-66. [5] 中国国家标准化管理委员会.GB/T 20123—2006钢铁总碳硫含量的测定 高频感应炉燃烧后红外吸收法(常规方法)[S].北京:中国标准出版社,2006. [6] 李岩,翟金鸥,仇慧群.红外碳硫仪测定钢中碳、硫含量的不确定度评定研究[J].中国化工贸易(China Chemical Trade),2013(10):251-252. [7] 中国国家标准化管理委员会.GB/T 11170—2008不锈钢 多元素含量的测定 火花放电原子发射光谱法(常规法)[S].北京:中国标准出版社,2008. [8] 宋祖峰,牟新玉,程坚平,等.火花源原子发射光谱法测定钢中超低碳、氮、磷和硫[J].冶金分析,2008,28(10):14-18. SONG Zufeng,MOU Xinyu,CHENG Jianping,et al.Determination of ultra-low carbon,nitrogen,phosphorus and sulfur in steel by spark source atomic emission spectrometry[J].Metallurgical Analysis,2008,28(10):14-18. [9] 赵兰季.光电直读光谱仪准确分析硫系易切削钢[J].河北冶金,2013(9):20-22. ZHAO Lanji.Accurate analysis of sulphur-series easy-cutting steel with photoelectric direct-reading spectrometer[J].Hebei Metallurgy,2013(9):20-22. [10] 张平根,张水菊,方南辉.光电直读光谱法检测易切削钢中的硫[J].江西冶金,2016,36(5):44-46. ZHANG Pinggen,ZHANG Shuiju,FANG Nanhui.Detection sulfur of free cutting steel by photoelectric direct reading spectrometry[J].Jiangxi Metallurgy,2016,36(5):44-46. [11] 张世欢,李世晶.直读光谱法快速测定易切削钢中高硫含量[J].南方金属,2017(1):30-32. ZHANG Shihuan,LI Shijing.Quick determination of sulfur content in free cutting steel by direct reading spectrometry[J].Southern Metals,2017(1):30-32. [12] 中国国家标准化管理委员会.GB/T 223.4—2008 钢铁及合金 锰含量的测定 电位滴定和可视滴定法[S].北京:中国标准出版社,2008. [13] 中国国家标准化管理委员会.GB/T 223.5—2008 钢铁 酸溶硅和全硅含量的测定 还原型硅钼酸盐分光光度法[S].北京:中国标准出版社,2008. [14] 中国国家标准化管理委员会.GB/T 223.23—2008 钢铁及合金 镍含量的测定 丁二酮肟分光光度法[S].北京:中国标准出版社,2008. [15] 中国国家标准化管理委员会.GB/T 223.59—2008 金属及合金 磷含量的测定 铋磷钼蓝分光光度法和锑磷钼蓝分光光度法[S].北京:中国标准出版社,2008. [16] 中国国家标准化管理委员会.GB/T 223.11—2008 钢铁及合金 铬含量的测定 可视滴定或电位滴定法[S].北京:中国标准出版社,2008. [17] 中国国家标准化管理委员会.GB/T 20124—2006 钢铁 氮含量的测定 惰性气体熔融热导法(常规方法)[S].北京:中国标准出版社,2008. [18] 曹晨巍,张盼盼,胡绍晖,等.硫系,碲系,铅系易切削钢组织及硫化物对比分析[J].冶金分析,2020,40(7):8-15. CAO Chenwei,ZHANG Panpan,HU Shaohui,et al.Structure and sulfide comparative analysis of sulfur,tellurium and lead free-cutting steels [J].Metallurgical Analysis,2020,40(7):8-15. [19] 张刚,信世奇,李运辉,等.含硫易切削钢硫化物形成机理研究[J].特钢技术,2020(1):49-52. ZHANG Gang,XIN Shiqi,LI Yunhui,et al.Study on formation mechanism of sulfide in free-cutting steel containing sulfur[J].Special Steel Technology,2020(1):49-52. [20] 王英虎,宋令玺.铸态和锻造态钛-硫易切削钢中硫化物形态及力学性能对比[J].机械工程材料,2021,45(2):37-42,48. WANG Yinghu,SONG Lingxi.Comparison of sulfide morphology and mechanical properties of as-cast and forged titamium-sulfur containing free-cutting steel[J].Materials for Mechanical Engineering,2021,45(2):37-42,48.