电感耦合等离子体原子发射光谱法测定硼钢铸件中的钆
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摘要
钆对高质量硼钢屏蔽铸件研究有重要意义。试验采用王水和硫磷混酸分解样品,选择分析线Gd376.839 nm,使用电感耦合等离子体原子发射光谱法(ICP-AES)建立了硼钢铸件中钆的测定方法。仪器的工作条件为:发生器功率1.2 kW、冷却气流量20 L/min、辅助气流量0.1 L/min、雾化器压力36PSI、蠕动泵泵速1.40 mL/min。钆质量浓度在0.5～5.0μg/mL范围内与发射强度呈线性,相关系数大于0.999 9,方法检出限为0.024μg/mL。按照试验方法测定三种硼钢材料中的钆,结果相对标准偏差(RSD,n=11)为1.28%～1.52%,加标回收率为95.0%～106.5%。
The determination of gadolinium in boron steel is very important to research the high quality boron steel castings. In this experiment, the boron steel sample was dissolved by HCl: HNO_3(3:1) and H_2SO_4:H_3PO_4:H_2O(1:2:3), and the content of gadolinium in boron steel was measured by inductively coupled plasma atomic emission spectrometry(ICP-AES) with the analytical line of Gd376.839 nm. The working conditions were listed as below: the power of generator was 1.2 kW, flow rate of cooling gas and auxiliary gas were 20 L/min and 0.1 L/min, respectively, the pressure of atomization gas was 36 PSI, and the speed of peristaltic pump was 1.40 mL/min. The mass concentration of gadolinium in the range of 0.5-5.0 μg/mL was linear to the corresponding emission intensity, and the linear correlation coefficient of calibration curve of gadolinium was higher than 0.999 9. The detection limit of the method was 0.024 μg/mL. The proposed method was applied to the determination of gadolinium in three boron steel samples. The relative standard deviation(RSD, n=11)was in the range of 1.28%-1.52%. The recovery ranged from 95.0% to 106.5%.
The determination of gadolinium in boron steel is very important to research the high quality boron steel castings. In this experiment, the boron steel sample was dissolved by HCl: HNO_3(3:1) and H_2SO_4:H_3PO_4:H_2O(1:2:3), and the content of gadolinium in boron steel was measured by inductively coupled plasma atomic emission spectrometry(ICP-AES) with the analytical line of Gd376.839 nm. The working conditions were listed as below: the power of generator was 1.2 kW, flow rate of cooling gas and auxiliary gas were 20 L/min and 0.1 L/min, respectively, the pressure of atomization gas was 36 PSI, and the speed of peristaltic pump was 1.40 mL/min. The mass concentration of gadolinium in the range of 0.5-5.0 μg/mL was linear to the corresponding emission intensity, and the linear correlation coefficient of calibration curve of gadolinium was higher than 0.999 9. The detection limit of the method was 0.024 μg/mL. The proposed method was applied to the determination of gadolinium in three boron steel samples. The relative standard deviation(RSD, n=11)was in the range of 1.28%-1.52%. The recovery ranged from 95.0% to 106.5%.
引文
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[2]贺信莱,褚幼义,柯俊.硼钢淬透性与硼向奥氏体晶界的偏聚[J].金属学报,1983(6):5-12,111-114.
[3]祖荣祥.硼钢的应用与热处理节能[J].金属热处理,1983(12):2-9.
[4]赵定国,马海涛,书桓,等.高硼钢中夹杂物形成热力学及实验研究[J].科学技术与工程,2016(13):162-167.
[5]董占武,魏世忠,张国赏,等.高碳硼钢的组织和性能研究[J].铸造技术,2008(11):1481-1484.
[6]马媛,方卫,王应进,等.ICP-AES测定金合金中钆和铍含量[J].光谱实验室,2008(5):947-950.
[7]张翼明,周凯红,张立锋.ICP-MS法测定钆镁合金中稀土杂质[J].稀土,2013(5):63-68.
[8]黎英,刘鸿,潘建忠,等.电感耦合等离子发射光谱法测定钆铁合金中稀土杂质量[J].有色金属科学与工程,2011(6):93-96.
[9]段双,董文博,金小成,等.电感耦合等离子体原子发射光谱法测定钯钛合金中钯元素[J].铸造,2018,67(7):603-606.
[10]段双,金小成,朱智,等.电感耦合等离子体原子发射光谱法测定水玻璃再生砂中残余氧化钠含量[J].铸造,2016,65(12):1198-1202.
[11]向勇,陈志国,魏祥,等.稀土铈对高碳高硼钢微观组织与性能影响机理的研究(英文)[J].稀有金属材料与工程,2015(6):1335-1339.
[12]蒋军,赵平.高硼钢中B回收率的影响因素分析[J].铸造,2009,58(1):75-76.