GGR Critical Review of Analytical Developments in 2004–2005

In 2005 Geostandards and Geoanalytical Research embarked upon a new initiative for its readers. Key researchers in various fields of geoanalytical technique development and their application were identified and invited to provide reviews pertinent to their expertise. As noted in the first of these publications "…instead of revisiting the historical context or decades of development in each analytical technique, the goal here has been to capture a snapshot of "hot topics" across a range of fields as represented in the… literature" (Hergt et al . 2005). Rather than prepare an annual review, a decision was taken earlier this year to provide a biennial summary of progress and accomplishments, in this case for the years 2004–2005. The principal techniques employed in Earth and environmental sciences are covered here, and include laser ablation and multicollector ICP-MS, ICP-AES, thermal ionisation and secondary ion mass spectrometry, as well as neutron activation analysis, X-ray fluorescence and atomic absorption spectrometry. A comprehensive review of the development of reference materials, often essential to these techniques, is also provided. The contributions assembled serve both to keep readers informed of advances they may be unfamiliar with, but also as a means of showcasing examples of the breadth and depth of work being conducted in these fields.     

单道扫描电感耦合等离子体发射光谱法测定珊瑚礁中主量和微量元素

建立了用单道扫描电感耦合等离子体发射光谱法测定珊瑚礁中主量和微量元素的方法。珊瑚礁样品经酸溶解后,直接进行Ca、Mg、K、Na、V、Sr、Ba、Co、Ni、Pb、Li、Rb的测定,方法检出限为0.0004～0.1mg/L,精密度RSD<5%(n=6),样品的加标回收率为97%～105%。测定w(CaO)为50%的样品,结果与传统的EDTA容量法相符。方法经碳酸盐岩石国家一级标准物质验证可行,已用于大批量的珊瑚礁样品的测定。     

南海高钙沉积物中18种常微量元素的ICP-AES测定方法研究

在利用ICP-AES分析南海高钙沉积物中的常微量元素时,钙、镁常常干扰其它元素测试。通过采用优化仪器工作参数、扣除背景值、谱线干扰校正和基体匹配的步骤,消除了元素干扰和钙、镁基体效应,提高了方法的灵敏度和准确度。通过对南海沉积物样品的大量实验和国家一级标准样验证,建立了适宜高钙海洋沉积物元素含量的ICP-AES测试方法。该方法检出限为1.55~271μg/L,相对标准偏差RSD<4.54%(n=6)。     

ICP—AES法分析辉锑矿

本文针对辉锑矿成分复杂、主元素Sb易水解、部分元素易挥发,酸不溶元素的存在以及元素之间的干扰等问题,拟定了酸溶和碱熔分解试样的分析流程。在酸溶系统中结合TBP萃淋树脂和巯基棉分离富集分组,ICP-AES法测定Fe、Ca、Mg、Cu、Mn、Pb、Zn、Co、Ni、Au、Ag、In、Tl、Cd、Bi、Ga、Mo、Se、Te、As等20个元素。碱熔系统不分离主元素,用校正因素校正元素间光谱干扰并采用内标法ICP-AES测定Al、Ti、V、Ba、Sr、Sn、Sc、Cr、Be、Si和Sb等11个元素。试样验证表明,方法可行。     

电感耦合等离子体发射光谱法测定铀矿石尾渣标准物质中9种痕量元素

样品经ＨＦ－ＨＮＯ３－ＨＣｌＯ４分解，在２ｍｏｌ／ＬＨＮＯ３介质中，采用感耦等离子体光电直读光谱法对铀矿石尾标准物质中的Ａｓ、Ｂａ、Ｂｅ、Ｃｄ、Ｃｒ、Ｎｉ、Ｐｂ等和Ｓｎ进行定值分析。同一样品平行测定６次，其各元素的相对标准偏差在２％－１０％。分析结果均落在标准值的置信区间。     

等离子体发射光谱法分析毒砂单矿物

研究了大孔膦酸树脂对毒砂中主、次和痕量元素的吸附行为及洗脱条件,结合巯基棉和TBP柱分离技术,建立了两个分离流程。在J-A1160型多道直读光谱仪上实现了毒砂单矿物中包括主量元素Fe和As在内的20个元素测定。主量元素As和Fe的相对标准偏差(n为5～10)分别为1.03％和0.9％,其它元素在5％～11％范围。流程经实际试样分析验证,结果与化学法相符。     

电感耦合等离子体发射光谱法测试地质样品中的基体效应及校正办法

电感耦合等离子体发射光谱（ICP-AES）法分析速度快、干扰较少并能同时测定多种元素，被广泛应用于地质调查样品的分析测试中，成为通用的无机化学元素分析测试工具.在测定复杂基体样品时，由于基体效应产生的各种干扰也会影响分析测试结果，包括光谱干扰、物理干扰、化学干扰、电离干扰等.以ICAP-6000型号仪器为例，结合仪器特点及实际工作经验，对复杂基体地质样品测定中出现干扰的原因、特点进行分析，探讨基体消除的方法以保障测试结果的准确性.     

贵州织金地区稀土磷块岩矿床中稀土元素赋存状态

以稀土磷块岩矿床为研究对象,采用电感耦合等离子体光谱法和质谱法研究了3个代表性样品的基本化学组成,分析了40多个元素的含量,确定了矿物质量分数和赋存状态,研究了稀土元素在其中的分布特征。结果表明,97%以上的稀土元素呈类质同象状态部分置换磷灰石晶格中的Ca2 存在,只有小于3%的稀土元素呈被粘土质等吸附状态或离子交换(吸附)状态存在。     

Thermo 6300型电感耦合等离子体发射光谱仪常见故障及排除方法

详细介绍了美国Thermo仪器公司生产的Thermo 6300型电感耦合等离子体发射光谱仪在使用过程中不能"引燃"、容易"熄火"、数据稳定性差等常见故障及排除方法,以及其辅助设备的维护维修实例。     

GGR Biennial Review: Atomic Absorption,Inductively Coupled Plasma-Atomic Emission Spectrometry,Neutron Activation Analysis and X-Ray Fluorescence Spectrometry Review for 2008–2009

This review describes developments major and in trace element determination using atomic absorption spectroscopy (AAS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), instrumental neutron activation analysis (INAA), and X-ray fluorescence (XRF) spectrometry that were reported in 2008 and 2009. Publication levels were comparable to those of previous years, except for XRF which showed an increase in the number of articles published in the past 2 years. In terms of number of publications and impact, the most active field was AAS, while INAA was the least active. As expected for well-established and mature methods, novel developments for all four analytical techniques were relatively sparse. For AAS, the most notable publications concerned developments in sample introduction, particularly focussing on solid samples, increasing analyte sensitivity, and higher sample throughput. For ICP-AES, publication of developments in sample introduction, remediation of matrix effects and calibration continues. Compared with past years, there was a clear focus on sample preconcentration methods, but very few publications reporting new hyphenated speciation methods. For INAA, there were several publications exploring the accuracy and robustness of the method, as well as the requirements for INAA to meet criteria for a primary method of measurement. Two other related techniques, delayed neutron activation analysis, and prompt gamma activation analysis, were also described. Hyphenated XRF techniques showed interesting developments in enabling XRF and XRD analysis on the same spot, and further work characterising and calibrating three-dimensional micro-XRF shows promising results for investigating sample heterogeneity.