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

Sandro Fadda 《Geostandards and Geoanalytical Research》2005,29(1):143-156

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.  相似文献   

基于混合回归模型的夏季高温日数预测   总被引：3，自引：2，他引：3       下载免费PDF全文

周后福  王兴荣  翟武全  钱玉萍 《气象科学》2005,25(5):505-512

本文以变化比较激烈的高温日数为对象，通过加权叠加、周期波动以及尺度比较等理论分析提出一种短期气候预测观点，即长周期波动可用当地前期各种气象要素的长周期波动的某种函数表示，而短周期波动依然与大范围周边环境因子的变化有关。采用功率谱分析、逐步回归、方差分析等常用统计手段和二项式平滑方法，建立长周期波动和波动偏差比的预报方程，在此基础上得到高温日数的预报方程。应用该方法对合肥地区的高温日数进行了预测试验，利用滚动预报得到13个预报样本。在13个试测样本中，有11个样本试测较为准确，试测准确率达到84．6％。在试测不准确的2个样本中，误差有5～6d，而且它们出现在高温日数相对较多的年份，因此试测效果令人满意。  相似文献   

Small inflation sources producing seismic and infrasonic pulses during the 2000 eruptions of Miyake-jima, Japan     

Tomokazu Kobayashi  Yoshiaki Ida 《Earth and Planetary Science Letters》2005,240(2):291-301

During the 2000 activity of Miyake-jima volcano, Japan, we detected long period seismic signals with initial pulse widths of 1-2 s, accompanied by infrasonic pulses with almost the same pulse widths. The seismic signals were observed from 13 July 2000, a day before the second summit eruption. The occurrences of the seismic signals were intermittent with a gradual increase in their magnitudes and numbers building toward a significant explosive eruption on 18 August. After the eruption, the seismic and infrasonic events ceased. The results of a waveform inversion show that the initial motions were excited by an isotropic inflation source beneath the south edge of the caldera at a depth of 1.4 km. On the other hand, the sources of the infrasonic pulses were located in the summit caldera area. The times at which the infrasonic pulses were emitted at the surface were delayed by about 3 s from the origin times of the seismic events. It is suggested that small isotropic inflations excited seismic waves in the crust and simultaneously caused acoustic waves that traveled in the conduit and produced infrasonic pulses at the crater bottom. Considering the observed time differences and gas temperatures emitted from the vent, the conduit should have been filled with vapor mixed with SO₂ gas and volcanic ash. The change of the time differences between the seismic and infrasonic signals suggests that the seismic source became shallower within half a day before the August 18 explosive eruption. We interpret the source process as a fragmentation process of magma in which gas bubbles burst and quickly released part of the pressure that had been sustained by the tensional strength of magma.  相似文献   

土壤有机碳同位素样品制备过程的影响因素讨论   总被引：3，自引：1，他引：3  

曹蕴宁  刘卫国  宁有丰  张庆乐  王政 《地球化学》2005,34(4):91-100

土壤有机碳同位素地球化学在气候和植被恢复方面的研究已得到广泛应用,但目前对不同类型、不同时代的土壤总有机碳同位素样品制备过程的系统研究较少.本文选取黄土高原不同地区、不同类型的现代土壤和古土壤,对其有机碳同位素样品制备过程进行了较系统的研究.( 1)去除土壤中无机碳酸盐对有机碳同位素组成的干扰:对于现代土壤样品,在室温条件下,用 0.5～ 6 mol/L HCl反应 1 d去除碳酸盐,均可获得理想数据;在 70 ℃反应条件下,用 0.5～ 2 mol/L HCl反应 2 h去除碳酸盐可获得理想数据,但用 6 mol/L HCl,δ 13C值偏负 0.65‰;( 2)在 850 ℃氧化温度条件下,样品制备加铜丝,对现代土壤及古土壤样品的δ 13C值均没有影响,结果表明在用封管法进行现代土壤及古土壤的有机碳同位素样品制备时,可以不加铜丝;( 3)对于有机碳含量较高的有机碳标准物质、植物和现代土壤样品,在 850 ℃氧化条件下,恒温 2.5 h,足以保证样品有机质氧化完全,不会产生同位素分馏;对于深层黄土和红粘土样品,由于样品体系复杂,在上述氧化条件下难以获得理想数据,合适的氧化条件有待进一步深入研究.  相似文献   

酸性污染物欧拉型输送转化模式的研究   总被引：2，自引：0，他引：2  

高会旺  黄美元 《地球科学进展》1997,12(5):422-427

数值模式是研究酸性污染及其长距离输送特性的一种重要方法。７０年代以来，国内外发展了许多欧拉型的输送转化模式，我国在欧拉型酸性污染物长距离输送模式的研究中也取得了重要进展。主要介绍了国内外的欧拉酸性污染物输送转化模式，并就模式的发展方向进行了讨论。  相似文献   

硅酸盐样品微波加热碱熔分解方法   总被引：1，自引：0，他引：1  

张燮  杨学强 《华东地质学院学报》1997,20(2):126-129

本文研究了硅酸盐样品在常压下，用微波炉进行碱熔分解的熔样时间，试剂用量和滴加水量等情况对分解的影响，确定了最佳实验条件，将此法用于地球化学标准参考样品ＳｉＯ２的测定，取得了满意的结果。  相似文献   

地球化学样品中硒的循序提取技术   总被引：11，自引：0，他引：11  

张忠  周丽沂 《岩矿测试》1997,16(4):255-261

研究开发了一种硒的循序偏提取步骤，将地球化学样品中的硒选择性地循序提取到六个“操作上”定义的相态中：水溶性硒（水提取）；吸附在氧化矿物和粘土矿物上配位可交换的亚硒酸根离子（０．１ｍｏｌ／ＬＫＨ２ＰＯ４提取）；与有机质结合的硒（０．１ｍｏｌ／ＬＮａ４Ｐ２Ｏ７提取）；与铁锰铝氧化物和碳酸盐结合的硒（４．０ｍｏｌ／ＬＨＣｌ提取）；硫化物中的硒（ＫＣｌＯ３＋浓ＨＣｌ提取）；硅酸盐残渣中以副矿物和被硅质包裹的硒微粒存在的硒（ＨＦ＋ＨＮＯ３＋ＨＣｌＯ４强混合酸溶解）。对提取步骤的可行性和实用性作了详细的讨论。  相似文献   

用载炭泡塑吸附原子吸收法测定地质样品中金   总被引：16，自引：0，他引：16  

周红  宋艳合  李红霞  曹丽妍 《黄金地质》2001,7(2):64-66

为达到简便、快速、准确测Au的目的，以泡塑为载体负载一定量的活性炭制成载炭泡塑，研究标准回收、酸度、流速及干扰试验结果，制定用载炭泡塑吸附，火焰原子吸收法测定地质样品中Au的实验方法，对部级含Au标样进行精度分析，并将测定外检样品的结果与活性炭富集及泡塑吸附法的测定结果做对照，表明该法具有较好的精密度和准确度，检出限为0.1ug/g，适合地质样品中Au的测定。  相似文献   

Moment-tensor statistics of the 1997 Long Valley microearthquake swarm     

A. Stroujkova  P.E. Malin 《Journal of Seismology》2002,6(1):69-85

Abstract. A simple, fast, moment-tensor inversion method using bandpass-filtered P-amplitudes was used to study the moment-tensor statistics of Long Valley caldera microearthquakes. The events were recorded in the summer of 1997, during a swarm in the caldera. The swarm was associated with geodetic extension, uplift, and subsequent moderate earthquake activity. The moment tensor solutions for 1,993 events were calculated using the new method. The majority of the resulting focal mechanisms appear to be explained in terms of double couple mechanisms. Since some events did exhibit considerable deviation from double-couples, the moment data were studied for their statistical significance. The moments of the actual data were compared to the moments of synthetic data with varying degrees of random noise in their spectra. The results of this study suggested that unless data from more than 20 stations are used and the earthquake epicenter is located inside or very close to the network area, moment-tensor inversion does not correctly resolve the non-double-couple components of microearthquakes. Analysis of the inversion residuals shows that the average noise in the P-wave spectra was close to 20%. The fluctuations of the volumetric components of the moment-tensor are in good agreement with those of the synthetic pure double-couples with 20% of added noise. Thus the moment-tensor statistics suggests that little if any volume change is required to explain the observed seismic energy release in the swarm. However, the statistics do show that a significant compensated-linear-vector-dipole component maybe present in the bulk of the seismicity. Given the network used in this study, such a component could not be precisely resolved for individual earthquakes. This possibility deserves further investigation because of its bearing on the nature of fluid-fault-earthquake processes in swarms.  相似文献   

Evolution of the fogwater composition in Strasbourg (France) from 1990 to 1999     

Pierre Herckes  Henri Wortham  Philippe Mirabel  Maurice Millet   《Atmospheric Research》2002,64(1-4)

The chemical composition of fogwater has been studied in the city of Strasbourg (France) from 1990 to 1999. During these years, fogwater samples have been collected and analysed for major ions and trace metals. This paper reports on the analysis of the collected dataset. The analysis revealed a significant decrease in acidity of approximately one pH unit over the course of the study. This decrease in acidity appears to be linked to a decrease in SO_2(g) and the resulting SO₄²⁻. Trace metal concentrations have also strongly decreased over the 10-year period. Pb concentrations, following the elimination of leaded gasoline, decreased by more than one order of magnitude.  相似文献