碱消解-高效液相色谱-电感耦合等离子体质谱法测定生物样品中的甲基汞和乙基汞

建立了碱消解-高效液相色谱-电感耦合等离子体质谱联用系统测定生物样品中甲基汞(MeHg)与乙基汞(EtHg)的分析方法。为提高灵敏度,选用微流量的PFA雾化器,在优化的检测条件下,MeHg及EtHg检出限可达到0.036μg/L和0.03μg/L;线性范围达到4个数量级,两条工作曲线线性相关系数为1。对1.78μg/L MeHg、1.65μg/L EtHg的混合标准溶液重复测定7次,色谱峰面积的相对标准偏差(RSD)分别为1.79%和1.44%。对标准物质BCR 464(金枪鱼)的分析结果表明,测定值与标准值基本吻合,但略低于标准值;甲基汞和乙基汞的加标回收率分别为85.9%和84.5%。高效液相色谱与质谱联用技术的高灵敏度和低检出限能够满足生物样品中汞形态定量分析的要求。     

微波消解在环境样品分析中的应用

微波消解是近年来兴起的一种样品分析手段,具有快速、高效、试剂用量少、样品不易被沾污、节约能源等优点。对当前微波消解技术在环境样品分析领域的应用和研究现状进行了综述,介绍了微波消解技术的基本原理、特点和设备,尤其对它在环境样品分析中的应用作了较为详细的介绍,并对该技术的应用前景进行了展望。     

黑龙江省中部森林沼泽区 超低密度深穿透地球化学调查采样介质的确定

通过对王水溶矿法与四酸溶矿法的对比,元素在泛滥平原A层、B层沉积物及水系沉积物中的分配,以及这3种介质圈定的异常对比等综合因素的研究,确定了泛滥平原A层沉积物是黑龙江省中部森林沼泽区开展超低密度深穿透地球化学调查的有效采样介质。     

重油凝胶色谱制备样品中痕量镍的分析研究

研究表明微波密闭消解法对重油凝肢色谱制各样品的前处理，不造成易挥发有机金属化合物的损失，对样品无污染。采用消解前定容，配合石墨炉二次进样富集样品，可以测定样品中低至10^—9级的镍。方法应用于镍在渣油中随相对分子质量分布分析中，标准样品对照数据吻合好，相对标准偏差(RSD，n＝11)为8％。     

ROCKS & MINERALS DETERMINATION AND ANALYSIS

正20142093Chen Daohua(Guangzhou Marine Geological Survey,Guangzhou 510075,China);Diao Shaobo The Latest Progress of Geological Marine Testing Technology in China(Rock and Mineral Analysis,ISSN0254-5357,CN11-2131/TD,32(6),2013,p.850-859,105refs.)Key words:chemical analysis,China     

An Investigation of Digestion Methods for Trace Elements in Bauxite and Their Determination in Ten Bauxite Reference Materials Using Inductively Coupled Plasma‐Mass Spectrometry

Trace elements from samples of bauxite deposits can provide useful information relevant to the exploration of the ore‐forming process. Sample digestion is a fundamental and critical stage in the process of geochemical analysis, which enables the acquisition of accurate trace element data by ICP‐MS. However, the conventional bomb digestion method with HF/HNO₃ results in a significant loss of rare earth elements (REEs) due to the formation of insoluble AlF₃ precipitates during the digestion of bauxite samples. In this study, the digestion capability of the following methods was investigated: (a) ‘Mg‐addition’ bomb digestion, (b) NH₄HF₂ open vessel digestion and (c) NH₄F open vessel digestion. ‘Mg‐addition’ bomb digestion can effectively suppress the formation of AlF₃ and simultaneously ensure the complete decomposition of resistant minerals in bauxite samples. The addition of MgO to the bauxite samples resulted in (Mg + Ca)/Al ratios ≥ 1. However, adding a large amount of MgO leads to significant blank contamination for some transition elements (V, Cr, Ni and Zn). The NH₄HF₂ or NH₄F open vessel digestion methods can also completely digest resistant minerals in bauxite samples in a short period of time (5 hr). Unlike conventional bomb digestion with HF/HNO₃, the white precipitates and the semi‐transparent gels present in the NH₄HF₂ and NH₄F digestion methods could be efficiently dissolved by evaporation with HClO₄. Based on these three optimised digestion methods, thirty‐seven trace elements including REEs in ten bauxite reference materials (RMs) were determined by ICP‐MS. The data obtained showed excellent inter‐method reproducibility (agreement within 5% for REEs). The relative standard deviation (% RSD) for most elements was < 6%. The concentrations of trace elements in the ten bauxite RMs showed agreement with the limited certified (Li, V, Cr, Cu, Zn, Ga, Sr, Zr and Pb) and information values (Co, Ba, Ce and Hf) available. New trace element data for the ten RMs are provided, some of which for the first time.     

微波消解―ICP―MS法测土壤和水系沉积物样品中的碘

介绍了用微波消解处理土壤和水系沉积物样品,用电感耦合等离子质谱仪(ICP-MS)快速高效测试碘的方法。方法的检出限为0. 012μg/g。所选的12个土壤和水系沉积物国家一级标准物质12次测定,除GBW07307a的RSD小于10%外,其余RSD值均小于5%,12次测试的平均值和标准值对数差绝对值均小于0. 05。方法加标回收率在98. 6%104. 6%之间。     

微波消解-电感耦合等离子体质谱法测定海泡石中的稀土元素

海泡石是一种纤维状含水的富镁硅酸盐黏土矿,其中的稀土元素含量在1×10~(-7)～1×10~(-5)之间,目前还没有建立海泡石中稀土元素的国家标准分析方法。测定岩石中的稀土元素主要是采用电感耦合等离子体质谱法(ICP-MS),样品前处理一般采用封闭溶矿和碱熔,但这两种处理方法耗时较长,效率不高。本文通过比较硝酸-氢氟酸-过氧化氢、硝酸-氢氟酸、硝酸-过氧化氢三种样品前处理方法,确定使用硝酸-氢氟酸溶矿,然后进行微波消解同时赶去氢氟酸,避免氢氟酸与稀土元素生成难溶的氟化物,再采用ICP-MS法测定15种稀土元素的含量。由于海泡石中的镁含量较高,为降低基体效应,以~(103)Rh和~(185)Re作内标补偿基体效应和校正灵敏度漂移,各元素测定值的准确性显著提高,回收率为91. 2%～110. 9%,检出限为0. 002～0. 011μg/L,精密度≤2. 79%。本方法与封闭酸溶ICP-MS法的分析结果吻合较好,且用酸量少(7 mL),溶矿效率高(1 h),检出限更低。     

MODIS多光谱信息在海上溢油检测中的应用

利用搭载在EOS-Aqua/Terra卫星上的MODIS数据,对长江口溢油、委内瑞拉的马拉开波湖溢油等4次事故进行光谱分析和研究.在对出事海域的卫星数据进行图像处理的基础上,利用MODIS数据的多光谱信息,分析溢油在各个波段的特征,并确定油膜特征比较明显的波段范围,为可见光/近红外卫星监测溢油提供参考.