金矿样品的几种溶样方法   总被引：4，自引：0，他引：4  

杨明荣  孙鹏  牟长贤  石爱萍 《黄金地质》2004,10(1):68-70

通过王水、封闭和烧杯敞口及聚乙烯溶样瓶封闭溶样等方法，对含Au矿样的试样分解、溶样体系及各种溶样方法的对比表明，利用聚乙烯溶样瓶，采用HNO3 NaCl KMnO4 NH4HF2溶样体系，在水浴锅中封闭溶样40min，矿样中的Au即可完全分解。经国家标准物质分析验证，结果与标准值相符。封闭溶样可以避免样品外溢、进溅，使分析结果更准确可靠，降低成本，减少环境污染，适用于大批量样品分析。  相似文献   

成都市区域化探深层样品元素异常与物探重、磁异常及遥感解译构造的关系     

唐将  赵琦  沈前斌  雷家立 《物探与化探》2004,28(5):415-417

通过深层样化探异常与物探重力、航磁和遥感解译关系的研究,认为深层样元素异常是由隐伏构造指示元素Au、Hg,与重力负异常有关的酸性岩元素Sn、Be、F、Y,与航磁正异常有关的基性岩元素Fe、Co、Ni、V、Cr和与地层有关元素Cd、C、Tl四部分组成;解释了深层样元素异常的原因,开拓出区域化探与区域物探、遥感解译相结合的新路。  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   

基于正交多项式逼近法的岩土参数概率分布推断   总被引：9，自引：0，他引：9  

宫凤强  李夕兵  邓建 《岩土工程技术》2005,19(3):144-147

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。  相似文献   

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   

土壤样品镉同位素分析中Cd与Sn有效分离方法的改进     

段桂玲  段瑞春  谭娟娟  顾涛  邵长生  路韬 《岩矿测试》2016,35(1):10-16

保证Cd的高回收率以及彻底的Sn干扰去除是获得精确镉同位素组成的前提,目前报道的多种Cd分离与纯化方法获得的Cd回收率有较大差异(42.6%~99.8%),且去除Sn干扰的效果也不同(去除率在87.8%~97.4%之间),Cd回收率和Sn去除率均不理想。本文对前人报道的分离方法进行对比实验,发现0.1 mol/L氢溴酸-0.5 mol/L硝酸是分离Cd和Sn的有效试剂,增加该组混合酸的用量可淋洗出样品中更多的Sn且不会损失Cd,当混合酸的淋洗用量增加至30 mL时,Sn的淋洗率达到99.8%以上,Cd的回收率亦达到99.0%±0.5%,可满足土壤样品镉同位素的测定要求。本工作为获得高精度的镉同位素组成奠定了基础,为研究土壤环境中镉的污染来源提供了技术手段。  相似文献   

电感耦合等离子体质谱法测定铅合金中的微量杂质元素镉和锡   总被引：1，自引：1，他引：0  

郝原芳  刘新  宋丽华  李丽君  徐英奎 《岩矿测试》2016,35(4):378-383

铅合金中的镉和锡由于含量较低,国家标准方法均为单一元素分析,步骤繁琐,检出限高,难以达到理想的检出要求。本文建立了应用电感耦合等离子体质谱法(ICP-MS)测定铅合金中微量级(μg/g级)杂质元素镉和锡的分析方法。采用单一的低浓度硝酸溶解铅合金,用低温慢溶的方式使样品溶解更加完全,减少了多离子对仪器的干扰;通过铅基体匹配和加入酒石酸保证了标准与样品介质的一致性,同时避免了锡的水解;以~(103)Rh作为内标元素,~(111)Cd和~(118)Sn作为测量同位素克服了质谱干扰。方法检出限为镉0.05 ng/g、锡0.04 ng/g,比国家标准方法的检出限(1~6μg/g)低,精密度小于4%。该方法试剂用量少,减少了处理样品的复杂性,实现了合金中微量级元素的准确测定。  相似文献   

粉末压片-X射线荧光光谱法测定盐湖样品中的主次元素          下载免费PDF全文

闵秀云  王德荣  高春亮 《盐湖研究》2016,24(2):32-36

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%。  相似文献   

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     

龚仓  丁洋  陆海川  卜道露  王立华  熊韬  张志翔 《岩矿测试》2021,(3):340-348

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-高氯酸四酸基础上引入硫酸,形成盐酸-硝酸-氢氟酸-高氯酸-硫酸五酸溶样体系,用于水系沉积物、土壤和岩石等不同类型地质样品的一次敞口溶解,采用在线加入~(185)Re和~(103)Rh内标方式,建立了应用ICP-MS同时测定稀土等28种金属元素的方法。钒铬镉镓锡元素的准确度提高了1.4%～14.6%,镧和铈元素的准确度提高了0.2%～8.9%。该方法应用于分析水系沉积物、土壤、岩石标准物质(分别为GBW07301a、GBW07408、GBW07107),其测定值与认定值相一致,相对标准偏差(RSD)为1.14%～9.84%,准确度(△lgC)均≤0.1。该方法分析过程较简单,结果准确可靠,可满足测定大批量地质样品中稀土和钴铪铟锰铌钽等金属元素含量的要求。  相似文献   

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

Wei‐Xin Lv  Hao‐Ming Yin  Meng‐Shu Liu  Fang Huang  Hui‐Min Yu 《Geostandards and Geoanalytical Research》2021,45(1):245-256

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.  相似文献