铬铁矿中亚铁的测定方法

采用硫-磷混合酸微波消解对难溶的钒钛磁铁矿进行前处理,用5-溴-PADAP-过氧化氢分光光度法测定矿样中的钒,优化了微波消解的实验条件。加入浓磷酸和40 g/L氟化钠溶液分别消除了共存常量元素铁和钛的干扰。方法检出限为0.004μg/mL,线性范围为0.01~1.0μg/mL。应用于实际钒钛磁铁矿样品中钒的测定,重现性好,检出限较低,灵敏度较高,能够满足简单、快速、批量分析的要求。     

承德钒钛磁铁矿钒和钛物相的联测分析方法

依据承德地区大庙式钒钛磁铁矿床特征,通过人工重砂分离及单矿物化学分析并结合电子探针、岩矿鉴定结果查明了承德钒钛磁铁矿石中的含钒矿物主要是钛磁铁矿和磁铁矿,次要矿物是钛铁矿和硅酸盐;含钛矿物主要是钛铁矿、钛磁铁矿,次要矿物是金红石、榍石。根据承德钒钛磁铁矿石钒和铁呈正比的关系,选取代表性试样进行了钒钛物相分析项目的确定及溶剂选择的实验,最终确定了钒和钛物相分析测定流程。钒物相分析测定项目为磁铁矿和钛磁铁矿中的钒、钛铁矿中的钒、硅酸盐中的钒及总钒四项;钛物相分析测定项目为钛铁矿中的钛、磁铁矿和钛磁铁矿中的钛、金红石中的钛、硅酸盐中的钛及总钛五项。通过本方法测定的各种含钒和钛矿物含量占矿石中总钒和总钛含量的比例与人工重砂分析定量计算的各种含钒和钛矿物含量占矿石中总钒和总钛含量的比例是相互吻合的。对110件钒钛磁铁矿石样品进行了4种含钛矿物及3种含钒矿物物相分析,结果与实际地质成矿组分符合。本方法实现了钒钛磁铁矿中钒矿物和钛矿物的定量分离,确定了钒和钛物相联测分析流程,可以同时测定钒和钛矿物的含量。     

含铀砂岩试样的预处理和铀钍同时测定方法研究

研究了含铀砂岩试样的预处理方法,采用过氧化钠熔融, CTMAB凝聚,有效地消除了硅酸溶胶对铀钍分离富集的影响,与示波极谱法衔接,同时测定铀钍.铀钍的线性范围为0.001～0.500 μg/10 mL,检出限铀为8.63×10-6 μg/mL,钍为5.16×10-6 μg/mL.本法用于砂岩型铀矿中铀钍含量小于5×10-6样品的连续测定,结果满意.     

流动注射在线分离富集分光光度法测定金矿石中金的方法研究

叙述了采用流动注射在线泡塑富集分离、分光光度联用技术快速测定金矿石中微量金的方法.建立了两条工作曲线:其一校正曲线范围为 0.1～1.0 μg/mL,进样频率22 N/h,浓集效率25,检出限2.2×10-8 g/mL;其二校正曲线范围为1.0～9.0 μg/mL,进样频率44 N/h,浓集效率13,检出限1.6×10 -7 g/mL.系统分散系数为3.78,对国家标准管理样GBW(E)-070014平行11次测定,RSD 为1.29%,对所得结果进行t检验,置信度95%时,无系统误差存在.     

微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究

生物样品中微量元素硒的分析检测,经典方法是湿法消解-氢化物发生原子荧光光谱法(HGAFS)。湿法消解处理生物样品需使用大量试剂,并且消解时间长,样品背景值高;HG-AFS的分辨率较低,已经不能满足微量硒的分析需求。解决生物样品的消解过程缓慢、试剂用量大的问题是提高样品中微量元素硒的检出限和分辨率的前提。本文采用湿法消解和微波消解两种消解体系处理样品,对两种方法制备的溶液分别采用HG-AFS和电感耦合等离子体质谱法(ICP-MS)进行测定,通过对比试验确定了微波消解ICP-MS方法可以实现生物样品中微量硒的准确测定。对比试验表明:采用高压密闭微波消解前处理样品技术可以大大缩短消解时间,减少试剂用量,降低了样品背景值;利用ICP-MS直接进行测定,方法检出限为0.01μg/g,精密度(RSD,n=12)小于4%,低于HG-AFS的检出限(0.03μg/g)和精密度(10%)。微波消解ICP-MS方法操作简单快捷,降低了方法检出限,提高了样品分析的准确度和精密度。     

微波消解-氢化物发生原子荧光光谱法测定粉煤灰中的硒

粉煤灰中含有的硒元素较高,有综合利用价值.由于基体的复杂性,并未形成成熟可靠的测定技术.本文参考煤炭样品和土壤样品中硒的原子荧光光谱分析方法,采用氢化物发生-原子荧光光谱法测定粉煤灰中的硒.样品经氢氟酸-硝酸-双氧水体系微波消解得到清亮、透明的消解液,消解液经浓盐酸还原后,加入三价铁盐消除共存元素的干扰,所加的铁盐量不干扰硒的测定.方法检出限为0.020 μg/g;平行测定5份粉煤灰样品,相对标准偏差低于4.2％;加标回收率为94.0％～105.0％.应用建立的方法对煤飞灰标准物质进行分析,测定值与标准值基本相符;对不同地区的实际粉煤灰样品进行分析,证实方法可靠,可用于粉煤灰中硒元素的测定.     

五酸和硝酸微波消解法结合ICP-OES技术测定多金属矿中多种元素的对比研究

快速、准确测定多金属矿中的主次量元素需要根据多金属矿的具体类型选择不同的预处理方法。本文采集我国典型区域的铅锌、锡、钼、钒和铜镍等5种多金属矿,对比了盐酸-硝酸-高氯酸-氢氟酸-硫酸五酸微波消解和硝酸微波消解的溶样效果,应用电感耦合等离子体发射光谱法(ICP-OES)测定铜铅锌锡钨钼锰钛钒9种元素。通过国家标准物质分析验证,五酸微波消解的溶样时间较长,但一次可测定铜铅锌钼锰钒6种元素;硝酸微波消解的溶样时间短,但一次只能测定铜铅锌钼4种元素;两种方法的准确度和精密度高(RSD5%),检出限低(5.3~30 mg/kg),均适合在地质行业推广应用。而由于锡钨钛3种元素不能完全被酸溶解,上述两种消解方法均不适合。     

微波碱消解-电感耦合等离子体发射光谱法测定煤灰中的六价铬

定量分析煤灰中Cr(Ⅵ)含量对于控制煤炭燃烧过程中产生的高毒性Cr(Ⅵ)的排放具有重要意义。现有的Cr(Ⅵ)定量分析方法主要是针对水、土壤、固体废弃物中的高浓度Cr(Ⅵ),前处理方法耗时长,检出限较高,不能有效测定煤灰中的低浓度Cr(Ⅵ)含量,因此有必要建立便捷、有效的煤灰中Cr(Ⅵ)高灵敏度检测方法。本文采用碱性提取剂,使用微波消解仪对煤灰进行前处理,对样品量、微波消解时间、微波消解温度等微波消解条件进行了优化,通过共沉淀法分离消解液中的Cr(Ⅲ)与Cr(Ⅵ),应用电感耦合等离子体发射光谱法测定Cr(Ⅵ)含量。结果表明,当样品量为0.2 g,微波消解温度为90℃,消解时间为60 min时能够保证煤灰中Cr(Ⅵ)的完全提取及准确测定。方法检出限为0.00033μg/m L,测定下限为0.00134μg/m L,实际样品的加标回收率平均值为87.2%。传统的二苯卡巴肼-紫外分光光度法的检出限为0.001μg/m L。与传统方法相比,本方法检出限降低,提高了检测灵敏度。     

微波消解-电感耦合等离子体发射光谱仪测定土壤样品中的硼

本文采用微波消解-电感耦合等离子体发射光谱法(ICP-OES)对土壤样品中硼含量的测定进行了实验。对微波消解样品前处理条件和测定时的仪器参数进行了优化,最终确定了以HF-HNO_3-H_3PO_4体系,逐级升温的方式来消解土壤样品。该方法对硼元素的检出限为0.093μg/g。经标准物质验证,其准确度、精密度均达到行业标准的要求,适用于土壤样品中硼的测定。     

微波消解-电感耦合等离子体发射光谱法测定固体沥青中微量金属元素

原油、沥青中的微量元素信息已被应用于油气勘探和油气地球化学研究,然而沥青的分析方法较少,而且前处理过程繁琐.本文将微波消解法应用于沥青样品的消解,电感耦合等离子体发射光谱法测定固体沥青中Al、Ca、Fe、K、Mg、Mn、Na、Ti、Ba、Mo、Ni、Sr、V等13种微量金属元素.在高压密闭条件下,微波消解系统消解固体沥青样品的速度快,并确定了样品量和消解条件等影响因素.不同组合消解试剂优化实验研究表明,浓硝酸-氢氟酸作为消解试剂效果最好;通过实验验证在样品处理过程中没有发生损失和污染情况,精密度(RSD,n=8)小于5％,回收率在92.2％～101.0％之间,元素的方法检出限可达0.05 μg/g.本方法为沥青类样品中微量元素分析测定提供了新的参考方法.     

The terrestrial fauna of the Late Triassic Pant-y-ffynnon Quarry fissures,South Wales,UK and a new species of Clevosaurus (Lepidosauria: Rhynchocephalia)

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.     

Définition d'une limite multicritère ; stratigraphie du passage Campanien–Maastrichtien du site géologique de Tercis (Landes,SW France)Definition of a multi-criteria boundary; stratigraphy of the Campanian–Maastrichtian interval of the geological site at Tercis (Landes,SW France)

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.     

The effect of water on accessory phase solubility in subaluminous and peralkaline granitic melts

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.     

Late Wuchiapingian (Late Dzhulfian,early Late Permian) limestone olistolites within the Tertiary flysch of Glypia Unit (Mount Parnon,central–eastern Peloponnesus,Greece)

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.     

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.)     

GEOCHEMICAL EXPLORATION

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.)     

MICROPALAEONTOLOGY

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.)     

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.,     

ENVIRONMENTAL GEOLOGY

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     

PROSPECTING EXPLORATION

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