Analytical procedures for the determination of selected trace elements in peat and plant samples by inductively coupled plasma mass spectrometry
Analytical procedures for the determination of selected trace elements in peat and plant samples by inductively coupled plasma mass spectrometry
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DOI：
10.1016/s0584-8547(02)00068-x
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发表时间：
2002-08-30
影响因子：
3.3
通讯作者：
Shotyk, W
中科院分区：
文献类型：
--
作者：
Krachler, M;Mohl, C;Shotyk, W
采用电感耦合等离子体四极杆质谱法（ICP-QMS），建立了泥炭和植物样品中Ca、V、Cr、Mn、Co、Ni、Cu、Zn、Rb、Ag、Cd、Ba、Tl、Th和U等15种元素的分析方法。在能够同时消化40份样品的微波加热高压灭菌器中，用各种酸混合物溶解约220 mg粉末状样品等分试样。选择适量的消解酸（硝酸、氢氟酸或四氟硼酸）对获得准确的结果至关重要。用于植物和泥炭样品消化的最佳酸混合物由3 ml HNO 3和0.1 ml HBF 4组成。发现具有额外膜去溶剂化单元的超声雾化器有利于测定Co、Ni、Ag、Tl、Th和U，允许将干燥样品气溶胶吸入ICP-QMS中。气动交叉流雾化器作为其他元素的进样装置。所有元素均采用103 Rh进行内标，但Th除外，其ICP-QMS信号由Rh-103和Re-185校正。通过对植物标准物质GBW 07602灌木枝叶的分析，确定了质量控制方法。在几乎所有的情况下，HNO 3单独不能完全从泥炭或植物基质中释放出感兴趣的分析物，可能是因为存在硅酸盐。在向消化混合物中加入少量（0.05-0.1 ml）HF或HBF 4后，通过ICP-QMS定量的浓度通常显著增加，在Rb的情况下高达80%。进一步增加HF或HBF 4的体积，导致几乎所有元素的回收率损失，其中一些达到约60%。成功的分析程序被应用到两个散装泥炭材料的测定。在一般情况下，发现的浓度和实验室间试验或仪器中子活化数据的结果之间的良好协议，得到了支持的适用性开发的分析方法。(C)2002 Elsevier Science B. V.保留所有权利。
A simple, robust and reliable analytical procedure for the determination of 15 elements, namely Ca, V, Cr, Mn, Co, Ni, Cu, Zn, Rb, Ag, Cd, Ba, Tl, Th and U in peat and plant materials by inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS) was developed. Powdered sample aliquots of approximately 220 mg were dissolved with various acid mixtures in a microwave heated high-pressure autoclave capable to digest 40 samples simultaneously. The selection of appropriate amounts of digestion acids (nitric acid, hydrofluoric acid or tetrafluoroboric acid) was crucial to obtain accurate results. The optimized acid mixture for digestion of plant and peat samples consisted of 3 ml HNO3 and 0.1 ml HBF4. An ultrasonic nebulizer with an additional membrane desolvation unit was found beneficial for the determination of Co, Ni, Ag, Tl, Th and U, allowing to aspirate a dry sample aerosol into the ICP-QMS. A pneumatic cross flow nebulizer served as sample introduction device for the other elements. Internal standardization was achieved with 103 Rh for all elements, except for Th whose ICP-QMS signals were corrected by Rh-103 and Re-185. Quality control was ascertained by analysis of the certified plant reference material GBW 07602 Bush Branches and Leaves. In almost all cases HNO3 alone could not fully liberate the analytes of interest from the peat or plant matrix, probably because of the silicates present. After adding small amounts (0.05-0.1 ml) of either HF or HBF4 to the digestion mixture, concentrations quantified by ICP-QMS generally increased significantly, in the case of Rb up to 80%. Further increasing the volumes of HF or HBF4 in turn, resulted in a loss of recoveries of almost all elements, some of which amounted to approximately 60%. The successful analytical procedures were applied to the determination of two bulk peat materials. In general, good agreement between the found concentrations and results from an inter-laboratory trial or from instrumental neutron activation data were obtained, underpinning the suitability of the developed analytical approach. (C) 2002 Elsevier Science B.V. All rights reserved.