Abstract：The sample was dissolved with nitric acid. A determination method of trace acid soluble aluminum (Als) in steel by inductively coupled plasma mass spectrometry (ICP-MS) was established. The determination conditions were also optimized. The experiment showed that the use of purified nitric acid to dissolve sample could reduce the influence on determination results. The matrix effect of high-purity iron could not be ignored, so the calibration curve was prepared by standard addition method with testing sample as matrix to eliminate this effect. The sample was dissolved in quartz beaker, and the determination results were more stable than those conducted in glass beaker. The sample solution of silicon steel certified reference material was diluted to constant volume in plastic volumetric flask, and the determination result was closer to the certified value than that in glass volumetric flask. The sample pretreatment conditions were optimized: the amount of nitric acid was 5mL and the dissolution time was 10min. The determination results of silicon steel certified reference material with 45Sc as internal standard was closer to the certified value than that with 89Y. When the pipe was washed with 2% (volume fraction) nitric acid for 8s, the memory effect could be basically eliminated. The mass concentration of 27Al was used as x-axis, while the response ratio of 27Al to internal standard element was used as y-axis to prepare calibration curve by standard addition method. The correlation coefficient of calibration curve equation was 0.9998. The low limit of determination for the method was 0.00006%. The proposed method was applied for determination of five certified reference materials of steel and two actual samples of alloy steel. The results were basically consistent with the certified values. The relative standard deviations (RSD, n=5) were between 1.6% and 4.5%.
胡文豪,袁永,刘骁,等.酸溶铝在钢中行为的探讨[J].钢铁,2003,38(7):42-44.HU Wen-hao,YUAN Yong,LIU Xiao,et al.On the behavior of soluble aluminum in steel[J].Iron and Steel,2003,38(7):42-44.
[2]
张翠敏.测定钢铁及合金中酸溶铝方法的比较[J].冶金标准化与质量,2008,46(3):48-51.ZHANG Cui-min.Comparison of methods for the determination of acid soluble aluminium in iron and steel and alloys[J].Metallurgical Standardization & Quality,2008,46(3):48-51.
[3]
张玲,李兰群,马爱方.钢中酸溶铝和全铝的光谱测定[J].冶金分析,2001,21(2):49-50.ZHANG Ling,LI Lan-qun,MA Ai-fang.Spectrum deteminnation of acid-aluminium and all-aluminium in steel[J].Metallurgical Analysis,2001,21(2):49-50.
[4]
闫茗,李志鹏,刘元元.多元光谱拟合-电感耦合等离子体原子发射光谱法测定不锈钢中低含量酸溶铝[J].冶金分析,2015,35(5):43-47.YAN Ming,LI Zhi-peng,LIU Yuan-yuan.Determination of low content acid-soluble alumium in stainless steel by multi-component spectral fitting-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2015,35(5):43-47.
[5]
陈学琴,张桂华,高文红,等.ICP-AES法测定酸溶铝和酸不溶铝及全铝[J].理化检验:化学分册,2002,38(1):25-26.CHEN Xue-qin,ZHANG Gui-hua,GAO Wen-hong,et al.ICP-AES determination of acid soluble and acid insoluble aluminum in steel[J].Physical Testing Chemical Analysis Part B:Chemical Analysis,2002,38(1):25-26.
[6]
Chen H,Dabekzlotorzynska E,Rasmussen P E.Evaluation of semiquantitative analysis mode in ICP-MS[J].Talanta,2008,74(6):1547-1555.
[7]
Nicola M,Rosin C,Tousset N,et al.Trace metals analysis in estuarine and seawater by ICP-MS using online preconcentration and matrix elimination with chelating resin[J].Talanta,1999,50(2):433-444.
[8]
Taylor D B,Kingston H M,Nogay D J,et al.On-line solid-phase chelation for the determination of eight metals in environmental waters by inductively coupled plasma mass spectrometry[J].Anal. At. Spectrom.,1996,11(3):187-191.
[9]
刘莹,翟世奎,张爱滨,等. ICP-MS测定海水中溶解态痕量重金属-直接稀释法[J].海洋学报,2008,30(5):151-158.LIU Ying,ZHAI Shi-kui,ZHANG Ai-bin,et al.Determination of dissolved heavy trace metals in seawater on ICP-MS-direct dilution method[J].Acta Oceanologica Sinica,2008,30(5):151-158.
[10]
何小青,刘湘生,陈翁翔,等.电感耦合等离子体质谱技术新进展[J].冶金分析,2004,24(6):26-35.HE Xiao-qing,LIU Xiang-sheng,CHEN Weng-xiang,et al.Advance in inductively coupled plasma mass spectrometry[J].Metallurgical Analysis, 2004,24(6):26-35.
[11]
聂玲清,纪红玲,陈英颖,等.基体未分离高分辨电感耦合等离子体质谱法测定钢中痕量元素[J].冶金分析,2007,27(2):18-23.NIE Ling-qing,JI Hong-ling,CHEN Ying-ying,et al.Determination of trace elements in steel by high resolution inductively coupled plasma mass spectrometry without matrix separation[J].Metallurgical Analysis,2007,27(2):18-23.
