Pressurised Extraction Using Dilute Ammonia: A Simple Method for Determination of Iodine in Soil, Sediment and Biological Samples by Inductively Coupled Plasma-Mass Spectrometry

A simple sample treatment method for the accurate and precise determination of iodine in soil, sediment and biological samples by inductively coupled plasma-mass spectrometry (ICP-MS) is described. Iodine in samples was extracted in screw top PTFE-lined stainless steel bombs using a 10% v/v ammonia solution at 185 C for 18 hours (overnight), after which the extract was introduced into the ICP-MS for direct measurement. ¹²⁶Te was employed as the internal standard to compensate for matrix effects and instrument drift. The limit of detection (LOD, three times the standard deviation of the procedural blank solution, expressed as the concentration in the sample solution) was 0.003 ng ml-^-1. The limit of quantitation (LOQ, ten times the standard deviation of the procedural blank solution, expressed as the concentration in the solid samples, dilution factor DF = 100) was 0.01 μg g-^-1 (dry mass). The accuracy and precision of the method were demonstrated by analysing different Chinese geological certified reference materials (soils, stream sediments and a hair sample). The measured concentrations were in a good agreement with the certified values indicating that bias in the method was not significant. The precision (n = 10) for different concentrations ranged from 1.82% to 4.32% RSD. Comparison of the ammonia extraction procedure with a "sintering" method indicated that there was no significant difference in results obtained with the two methods for geological soil and stream sediment samples. However, for biological samples, such as hair, kelp, tea etc., the results obtained by the sintering method were far below those of the ammonia extraction method. The ammonia extraction has advantages, as it is simpler than the "sintering" method, and has a lower procedural blank, better detection limits and reproducibility. Due to the simplicity of the method, a high rate of sample throughput is possible.     

Analytical Developments in Secondary Ion Mass Spectrometry 2003

This annual review of secondary ion mass spectrometry (SIMS) highlights significant progress in the application of the technology for the following areas: U-Pb geochronology (notably in the fields of reference material zircons), sources of uncertainty during analysis and secondary ion yields. Major publications introduced a new zircon reference sample and dealt with an intercomparison study of a suite of established calibrators, some of which have been shown to have certain limitations. Another publication claimed that the principal uncertainty in U-Pb dating is related to variations in the Pb and U relative emission yields over a complete analytical session. 2003 saw the introduction of an automated particle identification procedure applied to the analysis of a chondritic meteorite, as well as new geometries of SIMS hardware (NanoSIMS) and techniques (time-of-flight SIMS). NanoSIMS allows a two to three order of magnitude reduction in sampling volume as a result of a reduced beam diameter, and time-of-flight SIMS allows the study of sample surfaces, and can provide data for elements concurrently.     

流动注射分析及其在地质样品痕量元素测试中的应用

简述了流动注射分析方法的发展及其特点,介绍了流动注射在线分析技术,包括流动注射－原子光谱法、流动注射－分光光度法和流动注射－电化学分析法等联用技术在地质样品分析中的应用情况。     

地质样品中稀土总量的X射线荧光分析法测定

本文研究了稀土元素Ｃｅ的质量分数ｗＣｅ与由Ｃｅ至Ｌｕ１２元素质量分数之和ｗ１２（Ｎｄ除外）间的关系，发现ｗＣｅ和ｗ１２间存在明显一致的线性相关性。回归ｗ１２－ＩＣｅ标准工作曲线，实现了ｗ１２的直接测定。方法采用直接粉末压片制样，光谱仪测定ｗＣｅ，ｗＬａ，ｗＮｄ，ｗＹ，ｗ１２参数条件实现与稀土总量的转换。按本法对标准物质进行单项测定，结果令人满意     

波长色散X射线荧光分析的新发展

除了继续发展波长色散X射线荧光分析装置在主、次量元素分析上高精度、高稳定性的固有特点之外，进一步提高灵敏度，使分析范围扩展到痕量分析；开拓微区面分布的元素成像分析；进一步对传统分析因难的轻元素和中、重金属元素的探讨，开发新的高级次谱线分析方法；适应新材料特别是纳米材料的分析要求，对薄膜分析的开拓等方面，已经有了长足的发展。在介绍商品化的分析装置方面的发展状况的同时，对无标样分析的基本参数法目前发展状况也做了介绍。     

用微波封闭溶样氢醌滴定法快速测定金

采用HNO3—NaCl^--MnO2-NK4HF2溶样体系，在微波场中对矿样进行封闭溶解。实验表明，称样20g，利用聚丙烯溶样瓶，在微波场内只要照射2～3min，即可将矿样中的Au完全分解，以活性炭进行吸附富集，氢醌滴定法进行测定，其分析结果可满足地质找矿和选冶工艺对Au分析的要求。     

On Modelling Discrete Geological Structures as Markov Random Fields

The purpose of this paper is to extend the locally based prediction methodology of BayMar to a global one by modelling discrete spatial structures as Markov random fields. BayMar uses one-dimensional Markov-properties for estimating spatial correlation and Bayesian updating for locally integrating prior and additional information. The methodology of this paper introduces a new estimator of the field parameters based on the maximum likelihood technique for one-dimensional Markov chains. This makes the estimator straightforward to calculate also when there is a large amount of missing observations, which often is the case in geological applications. We make simulations (both unconditional and conditional on the observed data) and maximum a posteriori predictions (restorations) of the non-observed data using Markov chain Monte Carlo methods, in the restoration case by employing simulated annealing. The described method gives satisfactory predictions, while more work is needed in order to simulate, since it appears to have a tendency to overestimate strong spatial dependence. It provides an important development compared to the BayMar-methodology by facilitating global predictions and improved use of sparse data.     

石墨炉原子吸收法测定地质样品中的微量银

研究了石墨炉原子吸收法测定地质样品中微量Ag的方法,探索了以NH4IrCl6做基体改进剂的最佳仪器工作条件。在取样0．2000g,定容25mL的情况下,方法检出限为0．010ug/g,用国家标准物质验证,其准确度（RE％）小于10％,10次测定的精密度（RSD％）小于10％。     

Comparison of methods for calculating annual solute exports from six forested appalachian watersheds

Six methods were compared for calculating annual stream exports of sulfate, nitrate, calcium, magnesium and aluminum from six small Appalachian watersheds. Approximately 250–400 stream samples and concurrent stream flow measurements were collected during baseflows and storm flows for the 1989 water year at five Pennsylvania watersheds and during the 1989–1992 water years at a West Virginia watershed. Continuous stream flow records were also collected at each watershed. Solute exports were calculated from the complete data set using six different scenarios ranging from instantaneous monthly measurements of stream chemistry and stream flow, to intensive monitoring of storm flow events and multiple regression equations. The results for five of the methods were compared with the regression method because statistically significant models were developed and the regression equations allowed for prediction of solute concentrations during unsampled storm flows. Results indicated that continuous stream flow measurement was critical to producing exports within 10% of regression estimates. For solutes whose concentrations were not correlated strongly with stream flow, weekly grab samples combined with continuous records of stream flow were sufficient to produce export estimates within 10% of the regression method. For solutes whose concentrations were correlated strongly with stream flow, more intensive sampling during storm flows or the use of multiple regression equations were the most appropriate methods, especially for watersheds where stream flows changed most quickly. Concentration–stream flow relationships, stream hydrological response, available resources and required level of accuracy of chemical budgets should be considered when choosing a method for calculating solute exports. © 1997 John Wiley & Sons, Ltd.     

切向CT重建算法的研究

在工业CT的检测过程中,由于各种原因可能造成投影数据的不完备.在这种情况下,直接利用传统的解析重建方法(FBP)或者统计重建方法(EM)都不能给出理想的重建结果,从切向CT扫描方式获得的就是典型的不完备投影数据.本文利用迭代算法来改善重建图像的质量,首先通过已有的投影数据合理估计缺失的投影数据,并通过不断的迭代来改善这种估计,从而使得重建图像不断逼近真实物体.