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。     

等离子体质谱法测定玄武岩中微量元素三种样品预处理方法的比较

在测定玄武岩的微量元素时,为了保证得到的微量元素结果反映源区特征,需经预处理去除玄武岩的孔洞中充填的碳酸盐等物质。选取雷州半岛新生代玄武岩三个样品,每一个样品用三种预处理方法进行预处理,等离子体质谱法测定其中的微量元素。分析结果表明,用稀硝酸浸泡样品,会导致玄武岩中大多数微量元素严重丢失,得到的数据失真;而用稀盐酸浸泡去除碳酸盐的方法基本不改变玄武岩中微量元素的含量。     

激光拉曼光谱法分析多种显微组分荧光变化及其应用

利用激发488 nm激光的氩离子激光器作为RENISHAW inVia型激光拉曼光谱仪的光源,建立了多种显微组分荧光变化(FAMM)分析方法,并对镜质体反射率明显抑制的东营凹陷有效烃源岩进行了测定。结果表明,东营凹陷有效烃源岩的有机质类型越好,镜质体反射率抑制程度越高,有效烃源岩的真实成熟度应主要处于0.64%~1.30%,而不是实测镜质体反射率所反映的0.37%~1.10%。     

Sulfur isotope measurement of sulfate and sulfide by high-resolution MC-ICP-MS

We have developed a technique for the accurate and precise determination of ³⁴S/³²S isotope ratios (δ³⁴S) in sulfur-bearing minerals using solution and laser ablation multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). We have examined and determined rigorous corrections for analytical difficulties such as instrumental mass bias, unresolved isobaric interferences, blanks, and laser ablation- and matrix-induced isotopic fractionation. Use of high resolution sector-field mass spectrometry removes major isobaric interferences from O₂⁺. Standard-sample bracketing is used to correct for the instrumental mass bias of unknown samples. Background on sulfur masses arising from memory effects and residual oxygen-tailing are typically minor (< 0.2‰, within analytical error), and are mathematically removed by on-peak zero subtraction and by bracketing of samples with standards determined at the same signal intensity (within 20%). Matrix effects are significant (up to 0.7‰) for matrix compositions relevant to many natural sulfur-bearing minerals. For solution analysis, sulfur isotope compositions are best determined using purified (matrix-clean) sulfur standards and sample solutions using the chemical purification protocol we present. For in situ analysis, where the complex matrix cannot be removed prior to analysis, appropriately matrix-matching standards and samples removes matrix artifacts and yields sulfur isotope ratios consistent with conventional techniques using matrix-clean analytes. Our method enables solid samples to be calibrated against aqueous standards; a consideration that is important when certified, isotopically-homogeneous and appropriately matrix-matched solid standards do not exist. Further, bulk and in situ analyses can be performed interchangeably in a single analytical session because the instrumental setup is identical for both. We validated the robustness of our analytical method through multiple isotope analyses of a range of reference materials and have compared these with isotope ratios determined using independent techniques. Long-term reproducibility of S isotope compositions is typically 0.20‰ and 0.45‰ (2σ) for solution and laser analysis, respectively. Our method affords the opportunity to make accurate and relatively precise S isotope measurement for a wide range of sulfur-bearing materials, and is particularly appropriate for geologic samples with complex matrix and for which high-resolution in situ analysis is critical.     

<Superscript>226</Superscript>Ra, <Superscript>232</Superscript>Th and <Superscript>40</Superscript>K activities in soils of Cuihua Mountain National Geological Park,China

Gamma activity from the naturally occurring radionuclides namely, ²²⁶Ra, ²³²Th, the primordial radionuclide ⁴⁰K was measured in the soil of Cuihua Mountain National Geological Park, China using γ-ray spectrometry technique. The mean activity of ²²⁶Ra, ²³²Th and ⁴⁰K were found to be 27.2 ± 6.5, 43.9 ± 6.2 and 653.1 ± 127.6 Bq kg⁻¹, respectively. The concentrations of these radionuclides were compared with the typical world values and the average activities of Chinese soil. The radium equivalent activity, the air absorbed dose rate, the annual effective dose rate, and the external hazard index were evaluated and compared with the internationally approved values. All the soil samples have Ra_eq lower than the limit of 370 Bq kg⁻¹ and H _ex less than unity. The overall mean outdoor terrestrial gamma dose rate is 66.3 nGy h⁻¹ and the corresponding outdoor annual effective dose is 0.081 mSv.     

Si diffusion in zircon

Self-diffusion of Si under anhydrous conditions at 1 atm has been measured in natural zircon. The source of diffusant for experiments was a mixture of ZrO₂ and ³⁰Si-enriched SiO₂ in 1:1 molar proportions; experiments were run in crimped Pt capsules in 1-atm furnaces. ³⁰Si profiles were measured with both Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis with the resonant nuclear reaction ³⁰Si(p,γ)³¹P. For Si diffusion normal to c over the temperature range 1,350–1,550°C, we obtain an Arrhenius relation D = 5.8 exp(−702 ± 54 kJ mol⁻¹/RT) m² s⁻¹ for the NRA measurements, which agrees within uncertainty with an Arrhenius relation determined from the RBS measurements [62 exp(−738 ± 61 kJ mol⁻¹/RT) m² s⁻¹]. Diffusion of Si parallel to c appears slightly faster, but agrees within experimental uncertainty at most temperatures with diffusivities for Si normal to c. Diffusion of Si in zircon is similar to that of Ti, but about an order of magnitude faster than diffusion of Hf and two orders of magnitude faster than diffusion of U and Th. Si diffusion is, however, many orders of magnitude slower than oxygen diffusion under both dry and hydrothermal conditions, with the difference increasing with decreasing temperature because of the larger activation energy for Si diffusion. If we consider Hf as a proxy for Zr, given its similar charge and size, we can rank the diffusivities of the major constituents in zircon as follows: D _Zr < D _Si << D _{O, dry} < D _{O, ‘wet’}.     

江苏潮滩沉积物激光粒度仪与移液管-筛析分析结果的对比

激光粒度仪的广泛应用带来了与历史数据的对比问题,因此需要建立激光粒度仪与早期分析结果之间的关系。根据江苏海岸潮滩沉积物样品的激光粒度仪和移液管-筛析法分析,对粒度参数、粒度组分等进行了对比,对两种方法的差异进行了分析。结果表明,对于江苏潮滩沉积物粒度参数中平均粒径的激光粒度仪与移液管-筛析分析结果之间有良好的线性关系;筛分法测得的粗颗粒物质较激光法偏少,而移液管法法测得的细颗粒物质较激光法偏多;将样品分类之后再进行两种方法所获粒度参数的回归分析,相关性得以提高,说明不同粒度组成的沉积物对分析结果的对比有不同的影响。两种方法之间的换算关系不仅与研究区域有关,而且与沉积物本身的粒度组成有关。     

滑坡体三维地质建模与可视化分析

针对滑坡地质研究的自身特点,提出了面向滑坡地质体三维建模的NURBS-BRep混合数据结构和地质结构单元实体构造技术.通过对滑坡基础地质数据的预处理、滑坡数字地形和滑动面的三维建模、地质结构面的系统构造、地质结构体的生成和显示,形成了一套完整的滑坡三维地质模型的构建方法.将该方法应用于某水库滑坡,建立了相应的三维滑坡地质模型,并基于此模型进行了三维剖切分析、数字钻孔、等值线生成、滑块自动剖分、滑坡失稳可视化动态模拟和滑坡体方量精确计算等一系列实用的可视化分析,为滑坡稳定性的准确计算和客观评价提供了有力的支持.     

1998年夏、冬季南海水团分析

为了解南海水团的特征和分布 ,基于 1 998年夏季和冬季两个航次的实测资料 ,采用聚类分析、判别分析和模糊分析方法 ,对南海的水团进行了分析。结果表明 ,南海外海水可划分为 6个水团 ,即南海表层水团、南海次表层水团、南海次 中层混合水团、南海中层水团、南海深层水团和南海底盆水。越南附近夏季存在一个暖涡 ;1 998年夏季还可鉴别出黑潮表层水团和黑潮次表层水团 ,但在冬季观测期间无黑潮水越过 1 1 9.5°E经线进入南海 ;这些现象可能与厄尔尼诺现象有关联。夏季有苏禄海海水在 5 0— 75m层经由民都洛海峡侵入南海     

Numerical Experiment on Two-Dimensional Line Thermal

The time evolution of a two-dimensional line thermal-a turbulent flow produced by an initial element with signifi-cant buoyancy released in a large water body, is numerically studied with the two-equation k - e model for turbulence closure. The numerical results show that the thermal is characterized by a vortex pair flow and a kidney shaped concentra-tion structure with double peak maxima; the computed flow details and scalar mixing characteristics can be described by self-similar relations beyond a dimensionless time around 10. There are two regions in the flow field of a line thermal: a mixing region where the concentration of tracer fluid is high and the flow is turbulent and rotational with a pair of vortex eyes, and an ambient region where the concentration is zero and the flow is potential and well-described by a model of doublet with strength very close to those given by early experimental and analytical studies. The added virtual mass coeffi-cient of the thermal motion is found to be approximat