高精度热电离质谱(TIMS)铀系法洞穴沉积物(石笋)年龄的研究

用高精度热电离质谱技术测定石笋的年龄,初步建立了热电离质谱铀系年龄的方法。 4个样品的测定结果复现性较好,铀含量、同位素比值及年龄值与标准值吻合,数据的精度大大提高,显示了质谱铀系年龄方法具有样品量少、时间短、精度高的优点。     

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.     

Damped Lyα absorbers from dwarf galaxy ejecta

It is argued that the formation of a dwarf galaxy causes a massive burst of star formation, resulting in the ejection of most of the available gas from the galaxy as a weakly collimated wind. The ejected gas can give rise to a damped Lyα absorber (DLA). Weakly collimated outflows naturally explain the asymmetric profiles seen in low-ionization absorption lines caused by heavy elements associated with DLAs, where absorption is strongest at one edge of the absorption feature. The shape of the distribution of column densities in the model agrees reasonably well with observations. In particular, the break in slope is caused by external photoionization of the wind. A semi-analytical model for galaxy formation is used to show that, for currently acceptable cosmological parameters, dwarf galaxy outflows can account for the majority of DLA systems and their distribution with redshift. This model also predicts a correlation between velocity structure and metallicity of DLA systems, in qualitative agreement with observations. DLAs do not require many large, rapidly rotating disc galaxies to have formed early on, as in other models for their origin.