自制Z-Ⅱ碘探针应用于快速测定食盐及海带中的无机碘和有机碘

目前食盐和海带产品中碘含量分析主要是总碘含量测定,而无机碘与有机碘形态分析主要依靠大型精密仪器联用技术。本文研制了一种基于硫化碘化银法研制的全固态、无内参液的晶体膜电极(Z-Ⅱ碘探针),采用聚四氟乙烯消化罐微波消解技术,建立了食用盐及海带中的无机碘及有机碘含量测定方法。实验结果表明:食盐中无机碘含量为20mg/kg,有机碘含量为2mg/kg,海带中有机碘含量为2.9×10~3mg/kg。无机碘及有机碘含量分别在10～100mg/kg范围内线性关系良好,加标回收率为97.1%～101.0%,检出限均为1mg/kg。本方法应用于食盐和海带实际样品中的碘含量测定,无机碘和有机碘测定结果的相对标准偏差(RSD)分别小于0.92%和2.49%,且测定结果与国家标准方法和紫外分光光度法的测定结果基本一致。该方法具有试剂耗量少、成本低的特点,操作方便,可应用于有机碘和无机碘含量的测定。     

高效阴离子交换色谱-紫外检测器联用测定海水中碘

建立了在碱性体系中采用高效阴离子交换色谱和紫外检测器联用测定海水中碘离子的分析方法。以63mmol／L NaOH为淋洗液，利用IonPac AS16型强亲水性阴离子交换分离柱．碘离子在8．3min洗脱，经抑制器后进入紫外检测器在波长226nm处检测。方法的检出限为0．05μg／L（进样量500μL，3倍信噪比），标准曲线的线性范围为1～2000μg／L（r=0．9995）。20μg／L碘离子标准溶液9次连续进样的相对标准偏差为1．85％。方法已成功地应用于海水中碘离子的测定，1μg／L碘离子的加标回收率为98％～105％。     

封闭酸溶-盐酸羟胺还原ICP-MS法测定土壤沉积物岩石中的痕量碘

碘是活跃元素,价态多,各价态间易相互转化,化学性质不稳定,使用ICP-MS测定土壤、沉积物和岩石样品中的痕量碘,样品前处理和测定结果的稳定性是主要问题。本文采用磷酸-高氯酸高压密闭消解处理样品,提高了样品分解效率,也避免了碘的挥发损失,通过加入0.5mL 20g/L盐酸羟胺溶液将碘还原为I~-,提高了碘的稳定性,再于100℃烘箱中保温至少20min,以稀氨水作介质,降低了ICP-MS测定过程中的记忆效应。方法相对标准偏差(RSD)为4.88%～9.19%,相对误差为-6.90%～8.33%,回收率为92.5%～109.6%,检出限(3s)为0.012μg/g。本方法的测定数据与半熔法一致,解决了当前方法存在的分析流程长、空白高、岩石样品提取不完全、提取装置繁多等问题,可以作为土壤、沉积物、岩石中痕量碘测定方法的一种补充,适合批量样品分析。     

电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗

在多目标的配套方法中,硼、碘、锡、锗四个元素的分析涉及三个配套方法,发射光谱法测定硼、锡,原子荧光光谱法测定锗,分光光度法或电感耦合等离子体质谱法(ICP-MS)测定碘,分析成本高、检测效率低。本文建立了一种ICP-MS同时测定地球化学样品中硼、碘、锡、锗的方法。样品用过氧化钠熔矿,使难熔元素锡分解完全,熔盐经水提取后加入铼内标,再用阳离子交换树脂分离大量钠盐及大部分阳离子,保证了盐分满足质谱测定的要求。方法检出限分别为硼0.92μg/g、碘0.10μg/g、锡0.29μg/g、锗0.09μg/g,满足多目标测试要求。用国家一级标准物质验证,测定值与认定值一致,相对标准偏差(RSD,n=12)≤5%,适用于批量地球化学样品中硼、碘、锡、锗的测定,样品处理过程简便,检测效率高。     

碘的分析现状

综述了碘(主要是痕量碘)的分析概况及进展,包括测定方法(分光光度法、容量法、离子色谱、电分析化学方法、中子活化分析法、原子吸收光谱、发射光谱、质谱、X荧光光谱及测温法)及分离富集方法,还介绍了流动注射分析技术在测碘中的应用。     

Carius管溶样-标准加入电感耦合等离子体质谱法测定土壤中碘

建立了利用Carius管提取与标准加入电感耦合等离子体质谱法测定土壤中碘的方法。样品用φ=10%的NH.H2O溶液于密封的Carius管中150℃提取4 h,溶液适当稀释后离心分离沉淀,取出5等份样品上清液,分别加入不同浓度的碘标准储备液,用电感耦合等离子体质谱法测定溶液中的碘,以126Te作为内标。应用该方法分析了土壤国家一级标准物质GBW07404、GBW 07406、GBW 07407中碘的含量分别为(9.58±0.02)μg/g、(19.83±0.01)μg/g和(18.88±0.03)μg/g。分析结果与标准值相符。碘的检出限为0.02μg/g。     

汞型活性碳纸富集—XRF法测定地质试样中痕量碘

本文用特制的汞型活性碳纸富集地质样品中痕量碘并用X-射线荧光光谱进行测定。方法操作简便,样品测定限为0.25ppm,测定含I~-量25μg薄试样片(n=10),其相对标准偏差为3％。经地质标准样品验证,结果与推荐值符合。     

碰撞反应电感耦合等离子体质谱法直接测定卤水中的溴碘

目前使用电感耦合等离子体质谱法(ICP-MS)测定环境水样中的溴和碘,方法较为成熟,但应用于高盐卤水中溴碘的检测研究很少见报道.本文针对柴达木盆地盐湖卤水矿化度高、钾含量高的特点,建立了ICP-MS直接测定卤水中溴和碘的方法.采用碰撞反应接口(CRI)模式,以H2为碰撞气体,降低了检测过程中的多原子离子质谱干扰(例如39K40 Ar+对79Br+的干扰);选用Rh作内标元素,校正高盐样品引起的基体效应、仪器漂移等非质谱干扰;通过延长快泵冲洗时间消除测定过程中的记忆效应.在优化的实验条件下,盐湖卤水样品稀释200倍后用ICP-MS测定,方法检出限溴为0.036μg/mL,碘为0.027 μg/mL;方法精密度(RSD,n=12)溴为2.77％,碘为2.19％;加标回收率溴为91.6％ ～ 106.1％,碘为94.4％ ～ 107.7％.本方法也可应用于钾含量高的岩盐样品中溴和碘的测定.     

催化比色法测定土壤中的全碘

油气田上方土壤中的碘,含不溶于水的腐殖土稳固滞留的碘。要测定其含量,首先需将不溶性碘转化为可溶性碘化物。本文将样品用K_2CO_3溶液润湿、烘干、灼烧,实现了不溶性碘的转化,较半熔法熔剂量少、引入杂质量少。浸取液用硫氰化铁-亚硝酸盐体系的催化比色法测定Ⅰ~-的含量,回收率高于88％。对含Ⅰ~-为2.75ppm的试样测定10次其RSD为3.55％。本法适用于样品数量多、分析周期短的石油地球化学勘探样品的测定。     

离子选择电极测定岩盐样品中的氯和碘

利用离子选择电极测定岩盐样品中的氯和碘离子的含量,测定氯离子时以KNO_3和柠檬酸三钠为离子强度调节剂,测定碘离子时以硝酸钾、柠檬酸和柠檬酸三钠为离子强度调节剂,Na_2SO_3为还原保护剂,再双盐桥饱和甘汞电极外盐桥填充均为0.1mo L/L的KNO_3溶液。结果表明碘和氯离子线性良好,氯离子检测下限为0.0116μg/g,有良好的样品回收率(98.1%～102.2%);碘离子检测下限为0.0030μg/g,有良好的样品回收率(97.6%～102.5%)。该方法操作过程简单、分析速度快,造价成本低,灵敏度高,同时改善了实验室用ICP-MS测定碘元素背景干扰严重和硝酸汞滴定法测定低含量氯元素难以准确检测的问题,在实际应用中得到有效的验证。     

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.     

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.     

Quaternary stresses revealed by calcite twinning inversion: insights from observations in the Savonnières underground quarry (eastern France)

Calcite samples were extracted both from the rock matrix and the superficial coating of a karstified fault plane of an underground quarry, located in the eastern border of the Paris basin. The karstification is dated as Quaternary. Analysis of mechanical calcite twinning reveals that only the calcite matrix has also undergone a compression trending WNW that can be attributed to the Mio-Pliocene alpine collision. Both coating and matrix have undergone a strike-slip regime with σ₁ roughly trending north–south, that could correspond to the regional present-day state of stress, a strike-slip compression rather trending NNW, modified by local phenomena. To cite this article: M. Rocher et al., C. R. Geoscience 335 (2003).     

HYDROGEOLOGY

正20141756 Chen Ruige(Mathematical College,China University of Geosciences,Beijing100083,China);Zhou Xun Numerical Simulation of Groundwater Level Fluctuation in a Coastal Confined Aquifer with Sloping Initial Groundwater Level Induced by the Tide(Geological Bulletin of China,ISSN1671-2552,CN11-4648/P,32(7),2013,p.1099-1104,6 illus.,16 refs.) Key words:confined water,groundwater level     

METAMORPHIC PETROLOGY

正20141408 Cai Jia(Institute of Geology,Chinese Academy of Geological Sciences,Beijing100037,China);Liu Fulai Petrogenesis and Metamorphic P-T Conditions of Garnet-Spinel-Biotitebearing Paragneiss in Danangou Area,Daqingshan-Wulashan Metamorphic Complex Belt(Acta Petrologica Sinica,ISSN1000-0569,CN11-1922/P,29(7),     

SERIALS

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GEOPHYSICAL EXPLORATION

正20142386An Guoying(China Aero Geophysical Survey and Remote Sensing Center for Land and Resources,Beijing 100083,China)Application of Satellite Remote Sensing in Regional Hydrogeological Investigation:Taking Cenozoic Strata in Wenquan Sheet(1∶250 000)of Karakoram Range as an Example(Geosci-     

QUATERNARY GEOLOGY & GEOMORPHOLOGY

正20141016An Chengbang(Key Laboratory of Western China’s Environmental Systems,Ministry of Education,Lanzhou University,Lanzhou 730000,China);Zhao Yongtao Lake Records during the Last Glacial Maximum from Xinjiang,NW China and Their Climatic Impli-     

PETROLEUM GEOLOGY

正20141538 Cao Qing(School of Earth Sciences and Engineering,Xi’an Petroleum University,Xi’an 710065,China);Zhao Jingzhou Characteristics and Significance of Fluid Inclusions from Majiagou Formation,Yichuan Huangling Area,Ordos Basin(Advances in Earth Science,ISSN1001-8166,CN62-1091/P,28(7),2013,p.819-828,7 illus.,3 tables,43 refs.)     

GEOCHEMISTRY

正20142002 Wei Hualing(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang065000,China);Zhou Guohua Element Content and Mineral Compositions in Different Sizes of Soil in Tongling Area,Anhui Province(Geological Bulletin of China,ISSN1671-2552,CN11-4648/P,32(11),2013,p.1861