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1.
葛小燕  佘振宝  张敏  刘静 《世界地质》2013,32(2):412-421
合成并研究了铬黑T 形成树脂分离富集地质标准样品中的钌、铂、铑,获得了最佳实验条件。结果表明: pH = 2. 00 的盐酸溶液作为介质、温度为293 K、流速v≤1. 0 mL·min - 1、柱高h≥10. 0 cm,铂、铑、钌吸附率均在95%以上; 在293 K,使用40 mL 的pH 2. 00 盐酸- 3%硫脲溶液静态洗脱或以1. 0 mL·min - 1的流速进行动态洗脱,洗脱率均在95%以上。树脂对铂、铑、钌的吸附过程符合拟二级动力学模型。实验条件下的标准回收实验,回收率均> 95%。对地质标准样品进行了分析测定,相对误差均< 7%。铂、铑、钌的相对标准偏差分别是铂: 0. 852 0%和0. 325 0%; 铑: 4. 20%和 4. 89%; 钌: 1. 24%和1. 79%。铂、铑、钌的检出限分别为3. 55 × 10 - 6 μg·mL - 1、6. 23 × 10 - 7 μg· mL - 1、1. 92 × 10 - 5μg·mL - 1。该方法的准确度和精密度较高。  相似文献   

2.
采用微色谱柱技术对环境样品中的铀进行分离富集,分析了影响其分离富集的条件,并以ICP-AES为检测仪器,对环境样品中铀的含量进行了准确测定,建立了D293固相萃取分离/ICP-AES在线测定环境样品中铀的方法。实验表明,pH=1.5时,铀可被树脂完全吸附,10mL0.9mol/LNH4NO3-0.1mol/LHNO3可完全解吸铀,浓缩物用ICP-AES进行测定,检出限、相对标准偏差和相对误差分别为0.05μg/mL,0.8%~2.9%和0.4%~9.8%。方法简便、快速、准确,适合于各种环境样品中微量铀的测定。  相似文献   

3.
固相萃取-气相色谱法测定饮用水中的多氯联苯   总被引:2,自引:2,他引:0  
研究了饮用水中84种多氯联苯的气相色谱分析方法。讨论了洗脱曲线、水样的pH值、甲醇加入量、含盐量、萃取流速等实验条件,并与经典的液-液萃取方法进行了对比。确定了样品在pH值为3,以5 mL/min的流速经大体积样品采样器-C18固相萃取柱富集,7 mL丙酮和5 mL乙腈洗脱,氮吹蒸发浓缩后正己烷定容至1.0mL,加入内标后使用电子捕获检测器气相色谱仪测定,并在选定的色谱条件下以选择离子监测方式进行验证。84种多氯联苯的方法检出限为1.2~15.0 ng/L,加标回收率为74.8%~126.8%,相对标准偏差为1.1%~14.8%。由于采用了大体积样品采样器,可实现多个样品的同时萃取富集,方法快速、低污染,低成本,可用于批量水样品中多氯联苯的分析测定。  相似文献   

4.
本文对分离纯化样品过程中铅同位素的分馏进行了评估,并描述了适于MC-ICPMS同位素测定的分离纯化方法。利用AG1-X8阴离子交换树脂分离纯化样品中铅的过程确实导致了铅同位素的质量分馏。尽管分离纯化过程导致的铅同位素分馏程度较小(0.43‰amu-1),但明显超出了仪器的测试误差(0.23‰amu-1),如果样品中铅的回收率太低,会导致铅同位素测试值明显偏离真值。利用AG1-X8阴离子交换树脂,以0.2mL 1mol/L HBr溶液为上样介质,以5mL 1mol/L HBr和0.5mL 2mol/L HCl溶液为淋洗液,1.5mL 6mol/L HCl溶液为洗脱液,利用该分离流程可以保证获得样品中铅同位素的准确值。在本实验研究条件下,相对于过柱前样品,前期淋洗液富集铅的轻同位素(δ208Pb0),后期淋洗液富集铅的重同位素(δ208 Pb0),表明在该实验条件下,铅的重同位素组分比轻同位素更容易和树脂结合,AG1-X8阴离子交换树脂吸附铅的配分系数208 D/204 D大于1。解吸被树脂吸附铅的过程中,铅在不同络合形式间的交换反应可能导致了铅同位素的分馏效应,意味着无机络合物或者有机大分子参与反应的过程可能会导致铅同位素的分馏。  相似文献   

5.
铷作为稀有碱金属具有重大的经济战略意义。卤水中含有大量的铷资源,由于铷与大量与其物理化学性质非常接近的钾共存造成铷分离提取技术难度极大。采用磷钨酸铵-海藻酸钙AWP-CaALG球形复合吸附剂进行卤水中铷钾分离,通过动态吸附实验考察吸附剂的重复性能、流速、高径比、洗脱液浓度等吸附工艺条件对铷钾分离效果的影响。结果表明:在优化的动态吸附条件(流速=2.06BV/h,高径比=6.66)下,对CRb+=1.0g/L,CK+=10g/L,pH=1的溶液进行动态吸附,吸附剂对Rb+的吸附容量为16.34×10-3,穿透体积为7.86BV。以1 mol/L HCl~0.005 mol/L NH4Cl溶液和1 mol/L HCl~0.5mol/L NH4Cl溶液进行梯度洗脱,可得CK+=12.07 mg/L,CRb+=513.84mg/L的富集液,其中RbCl的纯度为96.93%。  相似文献   

6.
汞可以指示矿床或矿化存在,是一种重要的地质过程示踪元素,因此汞的测定是十分重要的。由于汞在地质矿床中丰度较低,直接测定存在困难,需要进行预分离富集处理。目前采用的分离富集手段大多数是离线,自动化程度较低。本文将合成的双硫腙改性氧化石墨烯/壳聚糖复合微球制成固相萃取小柱,考察了溶液pH、吸附剂种类和体积对汞的吸附效果的影响,优化了固相萃取在线采样/洗脱时间和速率对汞的吸附/洗脱效果的影响,建立了固相萃取在线富集-原子荧光光谱法测定地质样品中痕量汞的分析方法。结果表明:溶液pH=3.0时,以5 mL/min的采样速率进样5 min,汞的吸附率大于90%;用20 g/L硫脲-1.0mol/L硝酸混合溶液作洗脱液,以1 mL/min的洗脱速度洗脱1 min,洗脱率大于95%。汞含量在0.050~5.0μg/L范围内线性关系良好,富集因子为22,检出限为0.0019μg/L。采用本方法测定了土壤和沉积物国家标准物质样品,Hg的测定值与参考值的相对误差小于±13%。与离线分析相比,本方法具有灵敏度高、操作简单快速等特点。  相似文献   

7.
汲鹏  佘振宝  李现红  刘静  张敏  张凯 《世界地质》2010,29(1):168-174
采用2-邻胂酸偶氮苯-1, 8-二羟基-3, 6-二磺酸钠(铀试剂) 作为螯合剂制备螯合形成树脂, 并研究了该树脂的性能及对分离富集和测定结果的影响因素。实验发现, 用pH = 1.0的盐酸溶液做淋洗剂、柱高为8 cm、流速为1.00 mL /min、pH = 1.0的3%的硫脲-盐酸40 mL洗脱时, 贵金属离子能和常见的金属离子分离, 定量富集于树脂上。用极谱法测定贵金属元素的标准回收实验表明, 其回收率为94% ~106%。  相似文献   

8.
目前研究萃取分离富集镓大多偏向在强酸性体系中,一定程度上给操作带来安全风险,另需耐酸器皿设备,易污染,空白背景值高。本文开发了一种在弱酸性条件下萃取分离富集痕量镓的方法。以大孔吸附树脂为载体,十六烷基三甲基溴化铵调节其表面极性,热固化负载2-乙基己基磷酸(2-乙基己基)酯,制备了镓的萃取树脂。动态考察了固相萃取镓的吸附容量,优化选择固相萃取分离富集条件,实验表明萃取条件温和,分离富集痕量镓效果理想。当溶液酸度为pH 2.5时,Ga(Ⅲ)达到最大的回收率99%,并确定了掺氧空气乙炔火焰原子吸收光谱法(FAAS)测定镓的最佳参数,提升了常规空气乙炔FAAS测定镓的灵敏度。方法检出限(3σ)为2.6ng/mL,相对标准偏差(RSD,n=7)为2.87%,加标回收率在95.7%~102.0%之间,理论富集倍数为40。本方法已应用于自来水、中药材和水培蔬菜样品中痕量镓的测定,简便、快速、可靠。  相似文献   

9.
矿山企业的冶金废水含有多种污染环境的金属元素,必须经过化学沉淀法处理达标后排放。冶金废水经化学沉淀后引入了大量盐分,使得金属元素含量变得极低给分析测试造成困难。针对此类高盐冶金废水,本文采用巯基棉分离富集其中的金属元素,建立了运用电感耦合等离子体光谱(ICP-AES)测定铅、镉、铜、银的分析方法。通过优化实验表明,巯基棉可有效地分离实际样品中大量存在的硫酸根离子和钠离子基体,富集待测元素的效果显著,硫酸根离子和钠离子回收率均小于0.05%,待测元素的回收率在88.7%~113.0%之间。实验条件方面,待测溶液的pH值对巯基棉吸附有较大的影响,使用巯基棉富集前应将溶液调节至适宜的pH值;待测溶液在富集柱中的流速和洗脱剂盐酸的浓度对分离富集效果也有一定的影响。在最佳实验条件下,本法回收率为95.0%~102.0%,精密度(RSD)为3.1%~9.4%,方法快速简便、准确度高,能够满足冶金废水中痕量金属元素的检测需求。  相似文献   

10.
狄氏剂与多氯联苯均是海洋环境中毒性大、难降解的有机污染物,建立海水中狄氏剂与多氯联苯快速、灵敏、准确的检测方法,具有重要意义。本文采用聚苯乙烯/二乙烯基苯(Cleanert PS)固相萃取柱对海水样品中的狄氏剂与7种多氯联苯进行分离富集,建立了气相色谱-电子捕获检测器(GC-μECD)的分析方法。实验了萃取流速、洗脱液、水样盐度与pH等实验条件对萃取效率的影响,确定样品以5.0 mL/min的流速经Cleanert PS固相萃取柱富集,真空抽干后用5.0 mL丙酮洗脱,挥干洗脱液,用1.0 mL正己烷定容,在选定的色谱条件下进行分析。方法精密度(RSD)为0.9%~4.4%,与《海洋监测规范》GB 17378.4—2007的RSD指标相比,精密度良好;加标回收率为82.1%~123.9%。狄氏剂的检出限(0.0088 μg/L)低于文献的检出限(0.05 μg/L),7种多氯联苯的检出限(0.0012~0.0067 μg/L)低于文献的检出限(0.147~0.289 μg/L)。该方法适合于海水中痕量狄氏剂与多氯联苯的快速分析,具有一定的实用价值。  相似文献   

11.
Pant-y-ffynnon Quarry in South Wales yielded a rich cache of fossils in the early 1950s, including articulated specimens of new species (the small sauropodomorph dinosaur Pantydraco caducus and the crocodylomorph Terrestrisuchus gracilis), but no substantial study of the wider fauna of the Pant-y-ffynnon fissure systems has been published. Here, our overview of existing specimens, a few described but mostly undescribed, as well as freshly processed material, provides a comprehensive picture of the Pant-y-ffynnon palaeo-island of the Late Triassic. This was an island with a relatively impoverished fauna dominated by small clevosaurs (rhynchocephalians), including a new species, Clevosaurus cambrica, described here from a partially articulated specimen and isolated bones. The new species has a dental morphology that is intermediate between the Late Triassic Clevosaurus hudsoni, from Cromhall Quarry to the east, and the younger C. convallis from Pant Quarry to the west, suggesting adaptive radiation of clevosaurs in the palaeo-archipelago. The larger reptiles on the palaeo-island do not exceed 1.5?m in length, including a small carnivorous crocodylomorph, Terrestrisuchus, and a possible example of insular dwarfism in the basal dinosaur Pantydraco.  相似文献   

12.
Lithostratigraphy, physicochemical stratigraphy, biostratigraphy, and geochronology of the 77–70 Ma old series bracketing the Campanian–Maastrichtian boundary have been investigated by 70 experts. For the first time, direct relationships between macro- and microfossils have been established, as well as direct and indirect relationships between chemo-physical and biostratigraphical tools. A combination of criteria for selecting the boundary level, duration estimates, uncertainties on durations and on the location of biohorizons have been considered; new chronostratigraphic units are proposed. The geological site at Tercis is accepted by the Commission on Stratigraphy as the international reference for the stratigraphy of the studied interval. To cite this article: G.S. Odin, C. R. Geoscience 334 (2002) 409–414.  相似文献   

13.
Robert L. Linnen   《Lithos》2005,80(1-4):267-280
The solubilities of columbite, tantalite, wolframite, rutile, zircon and hafnon were determined as a function of the water contents in peralkaline and subaluminous granite melts. All experiments were conducted at 1035 °C and 2 kbar and the water contents of the melts ranged from nominally dry to approximately 6 wt.% H2O. Accessory phase solubilities are not affected by the water content of the peralkaline melt. By contrast, solubilities are affected by the water content of the subaluminous melt, where the solubilities of all the accessory phases examined increase with the water content of the melt, up to 2 wt.% H2O. At higher water contents, solubilities are nearly constant. It can be concluded that water is not an important control of accessory phase solubility, although the water content will affect diffusivities of components in the melt, thus whether or not accessory phases will be present as restite material. The solubility behaviour in the subaluminous and peralkaline melts supports previous spectroscopic studies, which have observed differences in the coordination of high field strength elements in dry vs. wet subaluminous granitic glasses, but not for peralkaline granitic glasses. Lastly, the fact that wolframite solubility increases with increasing water content in the subaluminous melt suggests that tungsten dissolved as a hexavalent species.  相似文献   

14.
Some olistolites reworked in a Tertiary flysch of Mount Parnon (Peloponnesus, Greece) exhibit a Late Permian assemblage, dominated by Paradunbarula (Shindella) shindensis, Hemigordiopsis cf. luquensis and Colaniella aff. minima. This association corresponds to the Late Wuchiapingian (=Late Dzhulfian), a substage whose algae and foraminifera are generally little known. Contemporaneous limestones crop out in the middle part of the Episkopi Formation in Hydra, but they are rather commonly reworked in Mesozoic and Cainozoic sequences. The palaeobiogeographical affinities shared by the foraminiferal markers of Greece, southeastern Pamir, and southern China, are very strong (up to the specific level), and are congruent with the Pangea B reconstructions. To cite this article: E. Skourtsos et al., C. R. Geoscience 334 (2002) 925–931.  相似文献   

15.
PALEONTOLOGY     
正20141596 Liu Yunhuan(School of Earth Sciences and Resources,Chang’an University,Xi’an 710054,China);Shao Tiequan Early Cambrian Quadrapyrgites Fossils of Xixiang Boita in Southern Shaanxi Province(Journal of Earth Sciences and Environment,ISSN1672-6561,CN61-1423/P,35(3),2013,p.39-43,3 illus.,20 refs.)  相似文献   

16.
正20141719 Chen Zhijun(State Key Laboratory of Geological Processes and Mineral Resources,China University of Geosciences,Wuhan 430074,China);Chen Jianguo Automated Batch Mapping Solution for Serial Maps:A Case Study of Exploration Geochemistry Maps(Journal of Geology,ISSN1674-3636,CN32-1796/P,37(3),2013,p.456-464,2 illus.,2 tables,10 refs.)  相似文献   

17.
正20140962 Chen Fenning(Xi’an Institute of Geology and Mineral Resources,Xi’an710054,China);Chen Ruiming Late Miocene-Early Pleistocene Ostracoda Fauna of Gyirong Basin,Southern Tibet(Acta Geologica Sinica,ISSN0001-5717,CN11-1951/P,87(6),2013,p.872-886,6illus.,56refs.)  相似文献   

18.
PETROLOGY     
正1.IGNEOUS PETROLOGY20142008Cai Jinhui(Wuhan Center,China Geological Survey,Wuhan 430205,China);Liu Wei Zircon U-Pb Geochronology and Mineralization Significance of Granodiorites from Fuzichong Pb-Zn Deposit,Guangxi,South China(Geology and Mineral Resources of South China,ISSN1007-3701,CN42-1417/P,29(4),2013,p.271-281,7illus.,  相似文献   

19.
正20141205Cheng Weiming(State Key Laboratory of Resources and Environmental Information System,Institute of Geographic Sciences and Natural Resources Research,CAS,Beijing 100101,China);Xia Yao Regional Hazard Assessment of Disaster Environment for Debris Flows:Taking Jundu Mountain,Beijing as an  相似文献   

20.
正20141266Fan Chaoyan(Guangdong Provincial Key Laboratory of Mineral Resources and Geological Processes,Guangzhou 510275,China);Wang Zhenghai On Error Analysis and Correction Method of Measured Strata Section with Wire Projection Method(Journal of  相似文献   

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