Abstract：The thickness of material on the top of ball-point pen was only between 0.3-0.4mm, which required very high machining precision. It put forward very high demands to the performance of stainless steel raw material (free-cutting steel). In free-cutting steel, some free-cutting elements such as S, P, Pb and Te were added into steel to improve the cutability of alloy steel. The accurate analysis of these microelements directly influenced on the success of steel smelting. It was found that the analysis of bucket sample had better stability than that of racket sample. Therefore, the sample was prepared from bucket sample with milling machine. The rotation speed of cutting head was controlled at 300r/min and the feeding speed was 250mm/min. The fundamental analysis conditions such as X-ray fluorescence spectrometer crystal, 2θ angle and pulse height were optimized. The certified reference material (CRM) was developed to draw the regression curves for Pb, Te and Bi in free-cutting stainless steel. The standard errors of estimate (SEE) were 0.0034, 0.0027 and 0.0046, respectively. The determination of Pb, Te and Bi in free-cutting stainless steel by X-ray fluorescence spectrometry (XRF) was realized. The detection limits for Pb, Te and Bi were 0.0009%, 0.0012% and 0.0006%, respectively. The proposed method was applied for the determination of Pb, Te and Bi in production sample (Number of 3125). The relative standard deviations (RSD, n=11) of determination results were all not more than 1.1%. The trueness analysis of free-cutting steel production samples was performed. The analytical results were in good agreement with those obtained by chemical wet method and spark discharge atomic emission spectrometry.
李联生,朱荣,郭汉杰,等.含锡易切削钢的冶炼和性能研究[J].特殊钢,2004,25(6):10-12.LI lian-sheng,ZHU Rong,GUO han-jie,et al.A study on smelting and properties of tin-bearing free-cutting steel[J].Special Steel,2004,25(6):10-12.
[2]
罗刚,王辉绵.一种圆珠笔用易切削不锈钢组织及性能分析[J].上海金属,2015,37(6):10-14.LUO Gang,WANG Hui-mian.Microstructure and mechanical properties of a free-cutting staninless steel for ballpoint pen[J].Shanghai Metals,2015,37(6):10-14.
[3]
张志刚,祁旭丞,李方军,等.X射线荧光光谱法分析中低合金钢[J].理化检验:化学分册,2009,45(9):1095-1100.ZHANG Zhi-gang,QI Xu-cheng,LI Fang-jun,et al.Analysis of medium and low alloy steels by XRF spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2009,45(9):1095-1100.
[4]
万双,李先和,赵九轲.X射线荧光光谱法快速测定黑铜中的铜、砷、锑、铋、铅、镍、锌和锡[J].化学分析计量,2017,26(5):93-96.WAN Shuang,LI Xian-he,ZHAO Jiu-ke.Rapid determination of copper,arsenic,antimony,bismuth,lead,nickel,zinc and tin in black copper by X-ray fluorescence spectrometry[J].Chemical Analysis and Meterage,2017,26(5):93-96.
[5]
张蓉,陈映宏,吴兰.X-荧光光谱仪对生铁中“五害”元素分析的探讨[J].特钢技术,2006(2):32-35.ZHANG Rong,CHEN Ying-hong,WU Lan.Analysis on five harmful elements in pig iron using X-fluorescent spectrum[J].Special Steel Technology,2006(2):32-35.
[6]
李强,黄万燕,王勇刚,等.能量色散X射线荧光光谱法测量钢铁中的铅[J].冶金分析,2012,32(7):41-44.LI Qiang,HUANG Wan-yan,WANG Yong-gang,et al.Determination of lead in iron and steel by energy dispersive X-ray fluorescence spectrometry[J].Metallurgical Analysis,2012,32(7):41-44.
[7]
彭光宇,王晶,陈江,等.X射线荧光光谱法测定不锈钢中多种元素[J].分析科学学报,2015,31(5):713-716.PENG Guang-yu,WANG Jing,CHEN Jiang,et al.Determination of multi-elements in stainless steel by wavelength dispersive X-ray fluorescence spectrometry[J].Journal of Analytical Science,2015,31(5):713-716.
[8]
刘晓丽.影响X荧光光谱仪测量准确度的几个因素[J].电子产品可靠性与环境试验,2012,30(1):138-140.LIU Xiao-li.Factors affecting the accuracy of X-ray fluorescence spectrometer[J].Electronic Product Reliability and Environmental Testing,2012,30(1):138-140.
[9]
马晓云,李健,宋鸿印,等.X-射线荧光光谱法测定含铁硫酸渣中的铅锌[J].新疆钢铁,2017(1):58-60.MA Xiao-yun,LI Jian,SONG Hong-yin,et al.Determination of lead and zinc in contain iron pyrite cinder by X-ray flurescence[J].Xinjiang Iron and Steel,2017(1):58-60.
[10]
郭利军.X射线荧光光谱快速分析高碳铬铁中铬、硅、磷[J].河北冶金,2018(3):41-44.GUO Li-jun.Rapid analysis of chromium silicon and phosphorus in high carbon ferrochromium by X-ray fluorescence spectrometry[J].Hebei Metallurgy,2018(3):41-44.
[11]
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):44-49.ZHANG Ping-gen,ZHANG Shui-ju,FANG Nan-hui.Detection sulfur of free cutting steel by photoelectric direct reading spectrometry[J].Jiangxi Metallurgy,2016,36(5):44-49.
[12]
孙琳琳,张磊,迟晓红,等.不锈钢中多元素含量测定的X射线荧光光谱法[J].化学工程师,2016 (3):35-37.SUN Lin-lin,ZHANG Lei,CHI Xiao-hong,et al.X-ray fluorescence spectrometry for elements concent of stainless steel[J].Chemical Engineer,2016(3):35-37.
[13]
芦飞.X射线荧光光谱法测定不锈钢中多种元素[J].冶金分析,2014,34(7):69-73.LU Fei.Determination of multi-element in stainless steel by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(7):69-73.
