端视电感耦合等离子体发射光谱法测定土壤中有效钼

样品经草酸?草酸铵溶液(Tamm溶液)浸提,分取浸提液,蒸干灼烧破坏草酸盐,制备成硫酸介质溶液,采用端视电感耦合等离子体发射光谱法测定土壤中有效钼。方法检出限(3s)为0.013μg/g,精密度(RSD,n=12)为2.13%~6.70%。经国家一级标准物质验证,测定值与标准值吻合。     

盐酸提取-电感耦合等离子体原子发射光谱测定土壤中的有效钼

以草酸-草酸铵溶液(Tamm溶液)浸提土壤中的有效钼,过滤,滤液蒸干,马弗炉高温灰化,盐酸提取,采用电感耦合等离子体发射光谱仪测定土壤中的有效钼。方法检出限(3s)达0.012×10-6,精密度(RSD,n=12)为2.31%～4.78%,经国家土壤有效态一级标准物质的验证,结果满足分析要求。     

高压密闭消解技术在土壤有效态样品前处理中的应用

土壤样品经有机酸浸提后,浸提出的溶液中存在大量有机酸及有机质,如未进行破坏处理,进入电感耦合等离子体发射光谱仪(ICP-OES)进样系统后容易堵塞雾化器、中心管、矩管等,或有颗粒黏附于中心管壁和矩管壁上,造成测定结果精密度和准确度差、空白高等问题,进而影响土壤有效态的综合评价。本文将土壤样品用有机酸(DTPA、草酸-草酸铵、柠檬酸等)浸提后,过滤或离心,吸取上清液加入高压密闭消解罐中,经电热板上处理,再加2mL浓硝酸,于180℃烘箱中保温至少3h,采用ICP-OES测定有效态元素铜锌铁锰镉铅镍铬钼硅的含量。本方法采用高压密闭消解技术处理土壤样品,各元素测定结果的相对标准偏差(RSD)为2.5%～5.9%,相对误差为-2.1%～5.2%,回收率为90.1%～103.2%,方法检出限为0.32μg/kg～0.038mg/kg;而采用以往高温炉中灼烧法、硝酸-高氯酸(硫酸)敞开消解法等技术手段,回收率为89.2%～100.5%,方法检出限为0.50μg/kg～0.050mg/kg,两者相比,本方法的测定结果稳定、空白低,分析周期短,适合批量样品的连续分析。     

DTPA浸提-电感耦合等离子体质谱法测定石灰性土壤中的有效态钴和有效态铅

传统的原子吸收光谱和分光光度法测定土壤有效态钴和有效态铅,操作繁琐,且分析效率低,不适用于大量样品的测定;利用先进仪器测定虽然提高了分析效率,但由于浸提剂的浓度影响仪器灵敏度,测定结果不准确.本文用DTPA溶液浸提,电感耦合等离子体质谱法测定石灰性土壤中有效态钴和有效态铅的含量.稀释倍数实验表明,浸提液稀释2倍时,石灰性土壤国家标准物质的测定值与标准值基本一致;稀释5倍或10倍时,测定值较标准值偏高;不稀释时,由于浸提液的浓度较高,受到基体干扰,测定值偏低.本方法确定对浸提液稀释2倍进行实验,有效态钴的检出限为0.0130 μg/g,有效态铅的检出限为0.0142 μg/g,精密度(RSD,n=9)小于8％.用土壤国家标准物质进行验证,测定值与标准值的相对误差小于9％(n=9),满足了DD 2005 - 03对土壤样品中有效态钴和有效态铅的测定要求.     

催化极谱法同时测定化探样品中的钨、钼

样品经碱熔分解,热水浸取,干扰元素铁、锰、钴、镍等形成氢氧化物沉淀与钨、钼分离。分取清液,在硫酸-苦杏仁酸-氯酸钠-辛可宁底液中,钨和钼均能产生灵敏的极谱催化波,峰电位分别为-0.76V和-0.25V(对饱和甘汞电极而言),固定试液体积,混合底液用针管一次加入,节省了稀释、定容、混匀的步骤,在JP4000型示波极谱仪上一次扫描同时测定钨和钼的峰电流,以峰高为纵坐标、含量为横坐标绘制工作曲线,直接计算出样品中钨、钼的含量,方法检出限(以三倍标准偏差计算)钨0.21μg/g,钼0.17μg/g,测定体系中,钨、钼分别在0.02~10.0μg范围内成良好的线性关系。     

电感耦合等离子体原子发射光谱法测定土壤中有效硫

采用电感耦合等离子体发射光谱法测定土壤中有效硫,浸提剂分别为：Ca（H2PO2）2-2mol／LHAc（中酸性土壤有效硫）,5mol／LNaHCO3（碱性土壤有效硫）？研究了ICP-AES对有效硫测定谱线的选择以及浸提温度、静置时间等对浸提结果的影响,酸性土壤滤液直接经ICP—AES测定,碱性土壤滤液经酸化后再测定。方法检出限分别为0．32mg／kg,通过对国家土壤有效态一级标准物质测试,测定结果基本一致;GBW07415、GBW07413标准物质11次测定的相对标准偏差（RSD）分别为3．66％、2．59％。     

超声加热浸提-电感耦合等离子体质谱法测定土壤中的有效硼

通过试验建立了一种超声加热浸提技术结合电感耦合等离子体质谱法测定土壤样品中有效硼的分析方法。实验对浸提温度、浸提时间、试液过滤方式以及测定干扰进行了研究,确定了土壤有效硼的超声浸提最适宜温度为70℃,浸提时间为20min,采用离心加滤膜过滤方式得到待测溶液。在最佳仪器工作条件下,采用103 Rh作为内标元素,选择11B作为测定同位素消除了测定干扰。实验结果表明:本方法检出限为0.009μg/L,测定结果的相对标准偏差(RSD)在0.92%～3.10%之间,样品加标回收率为98%～101%。应用本方法对土壤有效态成分分析标准物质GBW07416a、GBW07417和GBW07460进行了分析,测定值与认定值相符。与传统的沸水浸提标准方法相比,操作更为简便快速,无污染,准确度和精密度高,并且具有更低的检出下限,可用于大批量农田区土壤、森林土壤、离子型稀土矿区土壤以及重金属矿区土壤样品中有效硼的测定。     

极谱催化波法测定化探样品中的钨钼

试样经高温焙烧、碱熔分解,铁、铜、锰、钴、镍、钛、铋、镁等元素呈氢氧化物沉淀与钨、钼分离。在硫酸—二苯乙醇酸—二苯胍—氯酸钾底液中,钼、钨分别于约-0.26V(相对饱和甘汞电极钼峰电位)、-0.76V(钨峰电位)产生灵敏的平行催化波,根据测定区间内极限扩散电流的大小(选定区间内峰谷间的垂直距离)同时测定这两种元素。方法适用于化探样品、水系沉积物、土壤及岩石等样品中ω(Mo或W)1.0¹00.0ng/mL的测定。     

极谱催化波法测定化探样品中的钨钼

试样经高温焙烧、碱熔分解,铁、铜、锰、钴、镍、钛、铋、镁等元素呈氢氧化物沉淀与钨、钼分离。在硫酸—二苯乙醇酸—二苯胍—氯酸钾底液中,钼、钨分别于约-0.26V(相对饱和甘汞电极钼峰电位)、-0.76V(钨峰电位)产生灵敏的平行催化波,根据测定区间内极限扩散电流的大小(选定区间内峰谷间的垂直距离)同时测定这两种元素。方法适用于化探样品、水系沉积物、土壤及岩石等样品中ω(Mo或W)1.0~100.0ng/mL的测定。     

微量钨、钼催化极谱的连续测定

在0.5mol/L的硫酸-0.3g/L的苯羟乙酸-3g/L的氯酸钾溶液中,钨、钼均产生单峰形极谱催化波,分别于-0.60V和-0.25V测量其峰高值,本法适用于试样中w(W)=0.5×10-6～200×10-6和w(Mo)=0.5×10-6～100×10-6的测定,标准偏差分别为0.02～0.08(W),0.02～0.04(Mo),已用于斑岩铜矿中微量钨、钼批量样品的连续测定,其结果稳定、可靠。     

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