Determination of 17 Micro Elements in Aluminum and Aluminum Alloy by ICP-AES
摘 要
在0.050 0 g样品中滴加10滴200 g·L-1氢氧化钠溶液,于150℃加热15 s,待剧烈反应停止后,再加入200 g·L-1氢氧化钠溶液6 mL,于200℃加热40 min。取下烧杯,加入30%(质量分数)过氧化氢溶液2 mL。继续于200℃加热20 min,以分解溶液中过量的过氧化氢。冷却,加入50%(体积分数)硝酸溶液20 mL,盐酸2 mL,于200℃加热至溶液变清亮,冷却,用水稀释至100 mL,供电感耦合等离子体原子发射光谱仪测定其中铁、铜、镁、锌、镍、铬、锆、锡、钛、锶、镓、铍、铅、镉、硅、锰、钒等17种元素含量,设置射频功率为1 300 W,观测高度为12 mm,雾化气流量为0.65 L·min-1。通过优选谱线消除基体干扰中的光谱干扰,基体匹配法和同步背景校正法消除基体干扰中的物理干扰。按照上述方法处理10种标准样品,其中17种元素的质量分数均在一定范围内与其对应的谱线强度呈线性关系,检出限(3s)为0.000 3%~0.027 2%。方法分别用于实际样品以及标准样品的分析,实际样品测定值的相对标准偏差(n=11,RSD)为0.23%~3.1%,标准样品测定值的相对误差为-0.22%~5.0%,RSD (n=11)为0.17%~4.5%。
Abstract
The 10 drops of 200 g·L-1 sodium hydroxide solution was dropped into 0.050 0 g of sample, and the mixture was heated at 150℃ for 15 s. After the violent reaction stoped, another 6 mL of 200 g·L-1 sodium hydroxide solution was added, and the mixture obtained was heated for 40 min at 200℃. After removing the breaker, 2 mL of 30% (mass fraction) hydrogen peroxide solution was added for further reaction at 200℃ for 20 min until the excess hydrogen peroxide was completely decomposed. After cooling, 20 mL of 50% (volume fraction) nitric acid solution and 2 mL of hydrochloric acid were added into the solution, the mixture was heated at 200℃ untill the solution became clear. After cooling, the solution obtained was diluted to 100 mL with water. Elements of Fe, Cu, Mg, Zn, Ni, Cr, Zr, Sn, Ti, Sr, Ga, Be, Pb, Cd, Si, Mn, V in the sample were determined by ICP-AES with radio frequency power of 1 300 W, observation height of 12 mm and atomizing gas flow rate of 0.65 L·min-1. The spectral interference from matrix interference was eliminated by optimizing spectral lines, and the physical interference from matrix interference was eliminated by matrix matching method and synchronous background correction method. The proposed method was applied to the analysis of 10 standard samples, the mass concentrations of 17 elements in the standard sample were linearly related to their corresponding spectral line intensities in definite ranges, with detection limits (3s) in the range of 0.000 3%-0.027 2%. RSDs (n=11) of the determined values of the actual samples were found in the range of 0.23%-3.1%. Relative errors of the standard sample ranged from -0.22% to 5.0%, with RSDs (n=11) of the determined values in the range of 0.17%-4.5%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx202205007
所属栏目 工作简报
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收稿日期 2021/10/4
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备注李晓云,高级工程师,硕士,主要从事钢铁、原材料成分检测工作,664128088@qq.com
引用该论文: LI Xiaoyun,LIU Wenjun,WANG Genfang,ZHANG Genping. Determination of 17 Micro Elements in Aluminum and Aluminum Alloy by ICP-AES[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(5): 535~541
李晓云,刘文俊,王艮芳,张根平. 电感耦合等离子体原子发射光谱法测定铝及铝合金中17种微量元素的含量[J]. 理化检验-化学分册, 2022, 58(5): 535~541
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参考文献
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【3】国家市场监督管理总局,国家标准化管理委员会.铝及铝合金化学分析方法第25部分:元素含量的测定电感耦合等离子体原子发射光谱法:GB/T 20975.25-2020[S].北京:中国标准出版社, 2020.
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【5】戴亚明,马冲先,陶美娟.电感耦合等离子体原子发射光谱法测定紫砂壶中12种重金属元素[J].理化检验-化学分册, 2015,51(5):642-646.
【6】张殿英,刘伟.ICP-AES法测定硅铝钡铁合金中Al、Ba等9种元素含量[J].山东冶金, 2011,33(5):115-117.
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【8】高树峰,张海岩,张玉平,等.电感耦合等离子体原子发射光谱法测定氮化钒铁中8种杂质元素[J].理化检验-化学分册, 2014,50(7):842-844.
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