电感耦合等离子体质谱法测定花岗伟晶岩中稀土和稀散元素

doi:10.13228/j.boyuan.issn1000-7571.012236

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摘要稀土和稀散元素是支撑国家战略发展的关键元素,准确测定花岗伟晶岩样品中稀土和稀散元素具有重要意义。采用氟化铵-硝酸-高氯酸溶解法处理样品,将溶液蒸发至近干后,用逆王水(1+1)-0.1%(体积分数)氢氟酸体系复溶以避免Nb、Ta等元素的水解,采用耐氢氟酸的进样系统进样,建立了电感耦合等离子体质谱法(ICP-MS)测定花岗伟晶岩中Rb、Ga、Cs、Nb、Ta及稀土元素的方法。实验表明,各元素质量浓度与其对应的质谱信号强度值呈良好的线性关系,相关系数均不小于0.999 5,方法检出限为0.005～0.042 μg/g,定量限为0.015～0.126 μg/g。采用实验方法测定秦岭花岗岩标准物质和花岗伟晶岩标准物质中Rb、Ga、Cs、Nb、Ta和稀土元素,测定结果与认定值的相对误差(RE)为-8.3%～8.3%,相对标准偏差(RSD,n=12)为0.70%～7.6%。将实验方法应用于花岗伟晶岩样品的测定,测定结果的相对标准偏差(RSD,n=6)为1.1%~7.1%。

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	王书勤
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	赵娜娜
	卢希
	梁倩

关键词 ：花岗伟晶岩, 氟化铵, 电感耦合等离子体质谱法(ICP-MS), 稀土, 稀散元素

Abstract：Rare earth and scattered elements are the key elements to support the development of national strategy. It is of great significance to accurately determine the contents of rare earth and scattered elements in granite pegmatite samples. The sample was treated with ammonium fluoride-nitric acid-perchloric acid. After evaporating the solution to almost dryness, the residue was redissolved with reverse aqua regia (1+1)-0.1% (volume fraction) hydrofluoric acid to avoid the hydrolysis of Nb, Ta, and other elements. The hydrofluoric acid resistant sampling system was employed. Consequently, a method for determination of Rb, Ga, Cs, Nb, Ta and rare earth elements in granite pegmatite was established by inductively coupled plasma mass spectrometry (ICP-MS). The experimental results showed that the mass concentration of each element had a good linear relationship with its corresponding mass spectral signal intensity, and the correlation coefficients were all not less than 0.999 5. The limits of detection of method were between 0.005 μg/g and 0.042 μg/g, and the limits of quantification were between 0.015 μg/g and 0.126 μg/g. The proposed method was applied for determination of Rb, Ga, Cs, Nb, Ta and rare earth elements in certified reference materials of Qinling granite and granite pegmatite. The relative errors (RE) between the measured results and the certified values were between -8.3% and 8.3%, and the relative standard deviations (RSD, n=12) were between 0.70% and 7.6%. The proposed method was applied to determination of granite pegmatite sample, and the relative standard deviations(n=6) of the measured results were between 1.1% and 7.1%.

Key words： granite pegmatite ammonium fluoride inductively coupled plasma mass spectrometry(ICP-MS) rare earth scattered element

收稿日期: 2023-05-24

ZTFLH:	O657.63
	TF843
	TF845

基金资助:河南省国土资源厅2016年度地质科研项目(2015-1992-03)

通讯作者: 梁倩(1970—), 女, 教授级高工, 硕士, 主要从事岩石矿物的光谱和质谱分析研究;E-mail:646905947@qq.com

作者简介: 王书勤(1977—), 女, 高级工程师, 大学本科, 主要从事岩石矿物的分析方法研究; E-mail:dzsycsyjs@126.com

引用本文:

王书勤, 金艳妮, 赵娜娜, 卢希, 梁倩. 电感耦合等离子体质谱法测定花岗伟晶岩中稀土和稀散元素[J]. 冶金分析, 2023, 43(12): 25-32. WANG Shuqin, JIN Yanni, ZHAO Na′na, LU Xi, LIANG Qian. Determination of rare earth and scattered elements in granite pegmatite by inductively coupled plasma mass spectrometry. , 2023, 43(12): 25-32.

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