摘要: |
通过测定条件优化、方法比对等实验建立了一种固相萃取小柱离线螯合富集分离电感耦合等离子体质谱仪测定海水中稀土元素的方法。海水样品通过调节pH后, 进入VAC ELUT SPS24 Agilent圆形固相萃取装置, 其主要基体物质的去除率高于97%; 萃取富集的优化条件是海水样品pH 4.0~7.0, 海水进入萃取柱速率2 mL/min, 硝酸洗脱液浓度为1 mol/L; 方法对稀土元素的加标回收率为83%~108%, 14种稀土元素的检出限为0.057~0.613 ng/L, RSD<10 %; 该方法与氢氧化铁共沉淀法富集稀土元素比对测定结果一致, 方法具有准确度与精密度高、操作简便快速等优点, 可用于海水样品中稀土元素的定量精确测量。 |
关键词: 稀土元素 固相萃取 富集分离 ICP-MS 测定 海水 |
DOI:10.11759/hykx20170315001 |
分类号: |
基金项目:国家自然科学基金项目(No. 41676068; No. 41306070) |
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Determination of trace rare earth elements in seawater by ICP-MS with solid-phase extraction treatment off-line |
LIU Yao,SONG Jin-ming,LIN Qiang,YU Ying,SUN Ling-ling,WEN Ting-yu
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Abstract: |
In this paper, by optimizing the measurement conditions and comparing methods, we determined the presence of 14 trace rare earth elements in seawater by inductively coupled plasma mass spectrometry with solid-phase extraction treatment off-line. The seawater was pumped into a VAC ELUT SPS24 solid-phase extraction device after adjusting the pH value. The removal rate of the main matrix elements in seawater was higher than 97%. We determined the optimum conditions for solid-phase extraction to be of 4.0–7.0 pH value, 2 mL/min sample flow rate, and 1 mol/L nitrate elution concentration. The recovery rate by this method was in the range 83%–108%, and the relative standard deviations (RSDs) were less than 10%. The detection limit of 14 rare earth elements was in the range 0.057–0.613 ng/L. The method proposed in this paper is consistent with the iron hydroxide co-precipitation method for rare earth elements enrichment. The proposed method has high accuracy, good precision, and simple operation, which will meet the requirements for the determination of rare earth elements in seawater. |
Key words: rare earth elements solid-phase extraction enrichment and separation ICP-MS determination seawater |