电感耦合等离子体发射光谱法测定键合用硅铝丝中硅铁铜

采用电感耦合等离子体发射光谱法测定硅铝丝（Al—1％Si）中Si及杂质元素Fe和Cu。确定了最少取样量和样品溶解方法，优化了元素分析谱线和仪器的测量条件。实验表明，方法的加标回收率为99％～1叭％，相对标准偏差（n=6）低于1．4％，Si、Fe、Cu的检出限分别为8．5、1．0和0．4μg／L。该方法应用于快速测定键合硅铝丝中的各种元素，结果满意。     

一种获取包裹体内压的新方法——二氧化碳拉曼光谱法

对CO2的拉曼光谱特征做了介绍，特别指出了CO2费米共振峰随温度和压力的变化特点。利用CO2费米共振峰与密度的关系，结合状态方程对山东昌乐一临朐地区的火山岩包裹体进行了研究，获得了该地区火山岩包裹体的现实内压。结果表明，该地区包裹体的现实内压主要集中在5．75—18．29MPa。简单恢复了包裹体的形成深度，经与前人研究成果对比，显示该方法具有一定的可靠性。这种方法可以作为获取合CO2包裹体内压的一种新方法。     

微波消解-等离子体发射光谱法同时测定水中硅铁钠

讨论使用电感耦合等离子体发射光谱法测定水样中si、Fe、Na时，四种水样前处理方法对测试结果的影响。提出采用HNO3^-HF体系微波消解、H3BO3掩蔽HF的方法前处理水样，用等离子体发射光谱法可同时准确快速地测定水中Si、Fe、Na三种元素的含量。5次测定的相对标准偏差小于4％，加标回收率为89．2％-106％。     

GasBench-IRMS在碳酸盐岩δ^13C和δ^18O在线连续分析中的应用

采用GasBench-IRMS气体质谱分析技术，实现了碳酸盐岩中碳氧同位素的在线连续分析。优化了色谱柱温、离子源参数等工作条件，排除了空气中N2O的干扰。结果表明，色谱柱柱温为40℃、65℃时，方法线性范围较宽，结果准确可靠。方法用于碳酸盐岩国家一级标准物质中δ^13C和δ^18O的测定，结果与标准值一致。     

微波辅助提取-氢化物发生原子荧光光谱法测定土壤中无机砷

建立了微波辅助提取-氢化物发生原子荧光光谱法测定土壤中无机砷的分析方法。用正交试验设计结合单因素试验优化了样品粒度、提取温度、提取时间、固液比等微波提取条件，研究了共存离子对无机砷测定的干扰情况。方法的线性范围为0．25～40．0μg/g，无机砷的检出限为0．05μg/g，样品加标回收率为92．9％～105．0％。方法的精密度（RSD，n=11）为0．3％。与水浴提取法相比，微波辅助提取法具有快速、高效的优势。方法已用于分析3个不同产地有代表性土壤中无机砷含量。     

石墨炉原子吸收光谱法测定农业地质调查土壤样品中镉的不确定度评定

用实例对石墨炉原子吸收光谱法测定土壤样品中镉元素的不确定度进行评定,采用《测量不确定度评定与表示指南》对测量结果进行评估。分析了不确定度的主要来源,包括测量浓度的不确定度、体积的不确定度、称量不确定度及测量重复性引起的不确定度。评估了镉含量的合成标准不确定度和扩展不确定度。对于镉含量为0.42×10-6的土壤样品,其扩展不确定度为0.04×10-6。     

Alternative Validation of a LC-MS/MS-Multi-Method for Pesticides in Drinking Water

The development of instrumental analytics such as the LC-MS/MS has made it possible to quickly determine many component concentrations in a single chromatogram. However, the validation of such multi-methods needs new strategies for robustness and optimization. Statistical execution of analytical tests is one tool that can be utilized to meet this requirement. A Central Composite Design (CCD) was utilized for the validation of an LC-MS/MS multi-method for 84 analytes. The experimental design includes six design variables and two non-design variables (response variables). Concentration, ionization temperature, dwell time, gradient, flow (of eluent), and spraying/curtain gas (continuous design variables) were varied on five different levels; the whole design encompassed 91 runs. To investigate the robustness of a LC-MS/MS method both peak sensitivity and chromatographic separation had to be verified. Therefore, two non-design variables were necessary. The distribution of the peaks over analysis time was applied to describe the quality of the chromatographic separation. The sensitivity was described with the signal to noise ratio (S/N). The evaluation of the measured data was accomplished with the Analysis of Variance (ANOVA) and the Response Surface Methodology (RSM). Three main effects (concentration, ionization temperature, dwell time) and no significant interaction effect were found for the response variable “S/N”. The variables of concentration, ionization temperature, and dwell time had no significant effects for the response variable “S/N”. The ANOVA of the response variable chromatographic separation abandoned no significant effects as well. Therefore, robustness of the method can be guaranteed for all non significant design variables.     

西天山卡拉达湾地区铀及多金属综合找矿方向研究

卡拉达湾地区位于新疆北天山西段,属于中亚造山区,是在前寒武纪基底陆壳裂解的基础上发展起来的陆间型造山带,是铀及多金属成矿的重要区域。本文在前人工作的基础上,依据地面磁测、地面伽玛总量测量结果,总结分析了卡拉达湾地区磁场、放射性场、构造、矿化蚀变特征与铀及多金属成矿的关系,并圈定了铀及多金属找矿有利地段各2处,为西天山卡拉达湾地区的铀及多金属矿找矿工作提供方向。     

碱性体系在线氢化物发生原子荧光光谱法测定铜矿石中痕量砷锑铋

建立了一个碱性体系在线氢化物发生原子荧光光谱法测定铜矿石中痕量砷、锑、铋的分析方法。设计了在线氢化物发生流路及操作程序。选择了碱性体系氢化物发生的各项最佳条件,避免了Ｃｕ、Ｆｅ等大量基体元素的干扰。方法检出限为Ａｓ０．６μｇ／Ｌ,Ｓｂ０．４μｇ／Ｌ,Ｂｉ０．９μｇ／Ｌ,Ａｓ、Ｓｂ、Ｂｉ的工作曲线均在０～４００μｇ／Ｌ内呈良好的线性,经铜矿石国家一级标准物质分析验证,砷锑铋的测定结果与标准值吻合,相对标准偏差（ＲＳＤ,ｎ＝５）在４．２％～８．８％。     

Geological factors influencing the concentration of trace elements in the Philippi peatland, eastern Macedonia, Greece

Six peat samples obtained from the Holocene and the Weichselian of the Philippi peat deposit, eastern Macedonia, Greece, were analyzed for 48 trace elements by Inductively Coupled Plasma–Mass Spectrometry (ICP–MS). The ash contents of these samples were also determined. Most of the trace elements are associated with the minerals in the peat, while Ge, Mo, Pb, Se, Ta, Tl, U, and W display a greater affinity with the organic matter. Compared with crustal averages (Clarke concentrations), the Philippi peat is enriched in some elements (Ag, As, Au, Cd, Mo, Se, Te, U, and W) because of the respective mineralizations in the area. The Philippi peat is also enriched in Cr, Cu, Mo, Pb, Sc, Sn, T, V, Y, and Zn in comparison with typical fen peats, as well as in As, Cr, Mo, Se, and U in comparison with typical coals. Climatic and hydrogeological conditions strongly influenced the peat-forming environment resulting in a differentiation between Holocene and Weichselian peat. Generally, the Holocene peat contains lower concentrations of trace elements in the northern and southern part of the fen, than the Weichselian one. The opposite trend is observed in the fen area close to the western basin margins.