基于正交多项式逼近法的岩土参数概率分布推断

针对岩上参数样本容量较大的情况,基于数值分析中的逼近原理,直接根据试验样本值,运用勒让德正交多项式来拟合岩土参数的概率密度函数,并用K-S检验法从理论上证明所求的密度函数的正确性和实用性。     

Direct Current Plasma Emission Spectrometric Determination of Major, Minor and Trace Elements in Microwave Oven Acid Leachates of Powdered Whole Coal Samples

Major concentrations of Al₂O₃, Fe₂O₃, MgO, CaO, Na₂O and K₂O, minor levels of TiO₂, P₂O₅ and thirty petrologically, geochemically and environmentally significant trace elements have been determined in microwave oven acid leachates of whole powdered coal samples by direct current plasma‐atomic emission spectrometry (DCP‐AES). A single sample preparation procedure was suitable for all the determinations with no additional dilution step for major elements solution. Dried samples (0.5 g) were treated in low‐pressure PFA digestion vessels with HF/HCl/HNO₃/HClO₄ acids to quantitatively extract the analytes from the bulk material, while leaving the major part of organic matrix as a residue. The major constituents of geological samples, in particular the easily ionised elements (EIEs) such as alkali and alkaline earths, may complicate the instrumental determinations in DCP‐AES because of differential enhancements of elemental emission intensities and stray light interferences. Taking account of these factors, the coal matrix is considered to have very low major oxide totals as compared to many other common geo‐environmental and related materials (rocks, sediments, soil, ashes etc.). The sample size employed here, while yielding a relatively concentrated solution to cover a wide range of elemental determinations, provided a sample matrix that significantly diminished interferences for DCP measurements. The need for closely matching the unknowns and calibrators was eliminated except for overall acidity and an excess quantity of caesium for EIE buffering. Calibration of the spectrometer was accomplished by simple aqueous single element solutions as high concentration calibrators in addition to a reagent blank as a low concentration calibrator. Two point working curves were established to allow for the maximum concentrations of each element expected in the unknowns. The precision of determinations under routine conditions as well as the reproducibility of the leaching and precision of instrumental measurements have been evaluated. Relative standard deviations (RSD) were of 1–2% for those elements whose concentrations in solid samples were well above the limits of quantification. Method detection limits in the buffered solutions were also evaluated. To evaluate the accuracy of the microwave oven‐DCP method a suite of eight certified coal reference materials of differing rank, were analysed with good agreement with the certified and/or available published data. Results are presented for the uncertified major oxides in the AR series reference materials.     

粉末压片-X射线荧光光谱法测定盐湖样品中的主次元素

采用粉末样品压片制样,利用波长色散X射线荧光光谱仪对盐湖样品中K、Ca、Na、Mg、Cl、SO_4~(2-)等6个主次元素(组分)含量进行测定。使用化学定值得到的样品作为人工标样,其值作为标准样品参考值,建立了X射线荧光光谱法测定盐湖样品中主次元素的方法。经验证,该分析方法的准确度完全能够满足化学分析的要求,其相对标准偏差RSD7%,分析元素结果与化学法结果的相对误差均小于5%。     

Effect of the Dry Ashing Method on Cadmium Isotope Measurements in Soil and Plant Samples

A dry ashing method is commonly used to remove organic material from samples prior to geochemical analysis. In the course of this study, the Cd isotope ratios of a series of soil and plant reference materials and samples were studied to evaluate the effect of the dry ashing method on measurement results of Cd isotope ratios. The samples were pre‐treated using the dry ashing method and high‐pressure bomb for comparison. The results show that the digestion using high‐pressure bombs did not lead to Cd loss, but using the dry ashing method would cause different proportions of Cd loss. The whole range of Cd isotope difference between two methods was from ?0.07‰ to 3.01‰. There was also an obvious difference in measured Cd isotope ratios from the same leaf sample pre‐treated independently by the dry ashing method, indicating that the amount of Cd loss and the effect on Cd isotope measurement during dry ashing is related to the properties of the samples. Therefore, dry ashing may not be appropriate for the removal of organic material in Cd isotope ratio measurement, especially for samples with high organic contents. The δ^114/110Cd values of reference materials NIST SRM 1573a and GSD‐30 are reported for the first time in this study.     

海水营养盐测定中水样的保存技术

水样的保存和前处理技术直接关系到分析结果的精确度。针对海水氮、磷营养元素测定中影响水样保存期的容器和保存剂的选择进行了讨论 ,通过实验研究探索其行之有效又方便实用的保存方法以提高实验数据的精确度。     

ICP-MS测定生物样品中的微量金属元素

采用SP-60型恒压消解罐消解生物样品,用ICP-MS测定8种金属元素(Mn、Zn、Pb、La、Ce、Mo、Cr和Fe)的质量分数。依据分析结果,比较了消解程序的效果。结果表明,由10.0 mLHNO3对生物样品具有很好的消解能力,各元素的测定值与推荐值相符。     

五酸溶样-电感耦合等离子体质谱法同时测定地质样品中的稀土等28种金属元素

电感耦合等离子体质谱法(ICP-MS)测定大批量地质样品中的稀土和钴铪铟锰铌钽铊铬镉镓锗钒锡等金属元素,主要采用三酸或四酸溶解样品.由于地质样品组分复杂,稀土等金属元素含量低,各元素性质差异大,三酸或四酸溶样经常出现易挥发元素如钒铬镉镓锡的测定结果不稳定、镧铈镨钕等稀土元素溶解不完全的问题.本文在盐酸-硝酸-氢氟酸-高...     

Partial L-moments for the analysis of censored flood samples / Utilisation des L-moments partiels pour l’analyse d’échantillons tronqués de crues

Abstract

Abstract A parameter estimation method is proposed for fitting the generalized extreme value (GEV) distribution to censored flood samples. Partial L-moments (PL-moments), which are variants of L-moments and analogous to ?partial probability weighted moments?, are defined for the analysis of such flood samples. Expressions are derived to calculate PL-moments directly from uncensored annual floods, and to fit the parameters of the GEV distribution using PL-moments. Results of Monte Carlo simulation study show that sampling properties of PL-moments, with censoring flood samples of up to 30% are similar to those of simple L-moments, and also that both PL-moment and LH-moments (higher-order L-moments) have similar sampling properties. Finally, simple L-moments, LH-moments, and PL-moments are used to fit the GEV distribution to 75 annual maximum flow series of Nepalese and Irish catchments, and it is found that, in some situations, both LH- and PL-moments can produce a better fit to the larger flow values than simple L-moments.     

PAN－S光度法测定水和河泥中微量锰

本文研究了ＰＡＮ－Ｓ与锰的显色反应。配合物的最大吸收峰位于５３８ｎｍ波长处，表观摩尔吸光系数为２．９×１０￣４Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１），锰量在０─１．６μｇ／ｍｌ范围内符合比尔定律，方法用于水和河泥中微量锰的测定，结果良好。     

南极乔治王岛环境质量现状调查

本文以１９９２／１９９３年度中国第九次南极考察期间对南极乔治王岛的表土、地衣、苔藓等样品的分析资料为基础，研究探讨了８种无机重金属元素、５种有机污染物的浓度水平。其结果表明，重金属在三种环境样品中的含量分布存在着明显的差异；地衣、苔藓两种植物呈现对不同重金属元素的不同富集能力；∑６６６、∑ＤＤＴ和ＰＣＢｓ及油的沾污亦很明显。本文还对污染物质的来源、南极环境样品历次调查分析的结果以及世界部分地区的背景水平进行了讨论和比较