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氢化物发生-原子荧光光谱法测定镁及镁合金中砷

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随着镁及镁合金应用领域的深入,对其中有害元素砷的检测需求越来越多.本文先分次加入硝酸低温加热溶解样品,后用盐酸调节酸度,加入10 mL硫脲-抗坏血酸溶液使As(V)还原为As(Ⅲ),建立了氢化物发生-原子荧光光谱法(HG-AFS)对镁及镁合金中微量砷的测定方法.考虑镁及镁合金具有多种产品组别,如镁铝系、镁锌系、镁锰系、镁锂系、镁稀土系,试验考察了不同量镁基体及这些该镁合金组别内铝、锌、锰、铜、镍、锂、镧、铈、镨、钕、钆、钇、铒、镝等元素在最大量存在时对砷测定的影响.结果表明,镁基体与镁合金中主要合金元素对砷测定产生的干扰均可忽略.实验表明,在砷质量浓度为1.00~10.00 μg/L范围内,砷质量浓度与其对应的荧光强度呈线性关系,校准曲线的相关系数为0.999 7.方法检出限为0.001 4 μg/g,定量限为0.004 2 μg/g.按照实验方法测定3个镁合金样品,并分别加入砷标准溶液进行加标回收试验.测定结果的相对标准偏差(RSD,n=6)在2.4%~5.3%之间,加标回收率在98%~106%之间.方法比对试验表明,实验方法测定结果与电感耦合等离子体质谱法(ICP-MS)相符.
Determination of arsenic in magnesium and magnesium alloy by hydride generation atomic fluorescence spectrometry
With the increasing application of magnesium and magnesium alloy,there are more and more re-quirements for the determination of harmful element arsenic.The sample was dissolved in nitric acid in batches by heating at low temperature.Then the acidity was adjusted with hydrochloric acid followed by adding 10 mL of thiourea-ascorbic acid solution in order to reduce As(Ⅴ)to As(Ⅲ).Thus,a method for determination of trace arsenic in magnesium and magnesium alloy was established by hydride generation a-tomic fluorescence spectrometry(HG-AFS).Since there are many product types and groups of magnesium and magnesium alloy,such as magnesium-aluminum series,magnesium-zinc series,magnesium-manganese series,magnesium-lithium series and magnesium-rare earth series,the effects of magnesium matrix as well as the maximum content of aluminum,zinc,manganese,copper,nickel,lithium,lanthanum,cerium,praseodymium,neodymium,gadolinium,yttrium,erbium and dysprosium in magnesium alloy on the de-termination of arsenic were investigated.The results showed that the interference of magnesium matrix and major alloying elements in magnesium alloy with the determination of arsenic could be ignored.It was found that the mass concentration of arsenic in range of 1.00-10.00 μg/L had linear relationship with its corresponding fluorescence intensity.The correlation coefficient of calibration curve was 0.999 7.The lim-it of detection of method was 0.001 4 μg/g,and the limit of quantification was 0.004 2 μg/g.Three mag-nesium alloy samples were determined according to the proposed method,and arsenic standard solution was added for recovery test.The relative standard deviations(RSD,n=6)of determination results were between 2.4%and 5.3%,and the recoveries were between 98%and 106%.The method comparison tests indicated that the determination results of the proposed method were basically consistent with those ob-tained by inductively coupled plasma mass spectrometry(ICP-MS).

hydride generation atomic fluorescence spectrometry(HG-AFS)magnesiummagnesium al-loyarsenic

薛宁、孙改华

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中铝检测科技(郑州)有限公司,河南郑州 450041

氢化物发生-原子荧光光谱法(HG-AFS) 镁合金

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(12)