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《矿物岩石地球化学通报》2016,(2)
为探究盐类矿床中Br和I元素的影响因素及其对钾盐矿床成因的指示意义,采集思茅盆地勐野井的石盐、钾盐样品,采用X射线衍射方法分析了其盐类矿物组成,用ICP-OES和离子色谱仪测试了阳离子(K~+、Ca~(2+)、Na~+、Mg~(2+))和阴离子(Cl~-、Br~-、I~-、SO_4~(2-))组成。结果显示,样品的Br含量为89.08×10~(-6)~555.45×10~(-6),高于海水含量,Br×10~3/Cl的质量比值为0.13~0.86,Br的主要影响因素是溶液的主要成分(SO_4~(2-),K~+,Ca~(2+)和Mg~(2+))和蒸发作用;I含量为0.07×10~(-6)~0.27×10~(-6),I×10~6/Cl的摩尔比值为0.03~0.11,略高于海水值,I含量随I×10~6/Cl摩尔比值的增加呈上升趋势,说明蒸发作用是影响卤水I含量的因素之一。但Br和I呈负相关,表明有机质的含量是I含量的主要影响因素,蒸发作用可能是次要影响因素,I和I×10~6/Cl摩尔比值可能是判断海陆相的潜在指标之一。 相似文献
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蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇 总被引：1，自引：1，他引：0
建立了蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇的分析方法。进行了蒸馏温度和时间、氧化剂、吸收液等条件的选择,消除了等离子体质谱法测定钌和锇的干扰。样品用过氧化钠熔融,酸化后以高锰酸钾-过硫酸钾-氯化钠作为同时蒸馏钌和锇的氧化剂,采用20 mL 50 g/L水合肼溶液同时吸收从混合物中分离出来的痕量钌和锇,用电感耦合等离子体质谱法测定。方法的检出限Ru为0.020 ng/g,Os为0.015 ng/g;方法加标回收率Ru为94.0%~102.7%,Os为96.0%~102.4%;精密度为4.72%~9.58%(n=12)。方法经国家一级标准物质验证,钌和锇的测定结果与标准值相符。 相似文献
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对石墨炉原子吸收光谱法测定地质样品中微量银进行了研究。样品经四酸溶解,在3mol/L的HCl介质中以EDTA-抗坏血酸溶液作为基体干扰改进剂,用石墨炉原子吸收光谱法测定地质样品中微量银。方法检出限为0.051ng/mL,精密度(RSD,N=11)5.91%~12.83%。能满足地质样品中w(Ag)/10-6=0.03~5范围内银测定的准确度和精密度的要求。 相似文献
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高纯硝酸银中痕量杂质元素的存在会影响其性能和质量,为提高现代测试技术分析痕量杂质元素的准确度,需要解决的首要问题是通过加入沉淀剂或还原剂将银除去,克服基体元素的基体效应。本文提出采用10 mL 10 g/L柠檬酸-5 g/L乙醇酸作络合保护剂,12 mL 100 g/L氯化铵作沉淀剂,建立了沉淀基体分离-电感耦合等离子体质谱同时测定高纯硝酸银中15种痕量杂质元素的分析方法。探讨了络合剂和沉淀剂浓度及用量、质谱干扰及同位素选择、非质谱干扰及内标选择、实验空白值等因素对测定结果的影响。在最佳的实验条件下,Cu、Pb、Ni、Mn、Au、Pd、Pt、Rh、Ru、Ir元素在0~100 ng/mL,Fe、Hg、Bi、Cr、Sn元素在0~250ng/mL浓度范围内呈良好的线性关系。方法检出限(3σ)为0.005~0.062 ng/g,方法精密度(RSD,n=11)为0.6%~2.6%,加标回收率为94.1%~103.1%。与现行的分析方法相比,本方法采用的络合剂和沉淀剂能将基体元素与杂质元素完全分离而不影响测定结果;实验流程简单快速,检出限低,准确度和精密度均满足了实际样品的分析要求。 相似文献
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电感耦合等离子体光谱／质谱法测定环境样品中的硼 总被引：7，自引：3，他引：7
采用HF-HNO3-H3PO4-HClO4密封溶样处理样品,电感耦合等离子体光谱/质谱法(ICP-AES/MS)测定农作物、膳食和粪便中的硼。所拟定的方法在测硼的同时,还可测定Cr、Cu、Li、V、Co、Zn、Sr、Cd、Ba、K、Na、Fe、Mn、Zn元素,可以为农作物和饮食中痕量元素研究提供参考。ICP-AES测定硼的方法检出限(3σ)为0.0063μg/mL,测定限(10σ,DF=100)为2.10μg/g;ICP-MS测定硼方法检出限(3σ)为0.0228ng/mL,测定限(10σ,DF=1000)为0.092μg/g。方法经植物国家一级标准物质GBW07602～07605验证,测定值与标准值接近,样品10次测定的RSD<10%。 相似文献
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野马山岩基位于中祁连地块西段,由早期岩体(花岗闪长岩、斑状二长花岗岩)和晚期岩体(二长花岗岩)组成,二者呈侵入接触。LA-ICPMS锆石U-Pb定年表明,早期岩体侵位时代为中奥陶世((469.0±1.3)Ma),晚期岩体侵位时代为晚奥陶世((450.0±1.0)Ma)。早期岩体Si O2=59.8%~64.2%,K2O/Na2O1,且A/NKC=0.8~1.0,为准铝质岩石;微量元素相对富集Rb、U、Th和亏损Ba、Nb、Ta、Sr、P、Ti;稀土总量为97.7×10-6~185×10-6,且(La/Yb)N=5.57~12.47,LREE/HREE=7.7~11.3,具轻重稀土分馏明显,轻稀土富集,弱Eu负异常(δEu=0.66~0.89)特征。晚期岩体Si O2=69.8%~76.5%、K2O/Na2O=1.2~1.7、A/NKC=1.0~1.1,属弱过铝质花岗岩;稀土总量为78.97×10-6~244.92×10-6,轻重稀土分馏不明显((La/Yb)N=1.90~5.72),强Eu负异常(δEu=0.11~0.24)。岩石地球化学特征表明,野马山岩基早期岩体为I型花岗岩,形成于俯冲环境,晚期岩体为高分异的I型花岗岩,形成于后碰撞环境。结合岩体产出的区域构造位置及区域地质演化,认为早古生代北祁连洋发生了双向俯冲,野马山岩基为其向南俯冲碰撞的产物。 相似文献
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土壤中25种有机氯农药和多氯联苯的气相色谱分析方法研究 总被引：6，自引：5，他引：1
研究了土壤中17种有机氯农药和8种多氯联苯组分的气相色谱分析方法。采用加速溶剂萃取技术提取,优化了萃取条件。提取液用固相萃取技术进行净化,采用20 mL含3%(体积分数)甲苯的正己烷-乙酸乙酯(体积比8∶2)进行淋洗,得到很好的净化效果。方法检出限在0.06~0.27μg/kg,线性范围在1.38~55.2 ng/mL,目标化合物的平均添加回收率在65%~97%,相对标准偏差(RSD,n=6)小于17.11%。方法快速、灵敏、准确,适合批量样品的分析。 相似文献
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在江西德兴斑岩铜矿的野外地质、地球化学研究工作的基础上,采用该矿床围岩——前震旦系九岭群九都组的变质岩作为实验试料,在250—400℃和200×10~5—500×10~5Pa的压力下,与不同酸度(pH=1.5—4.5)、不同浓度(0.1255M—1.00M)的钠、钾、氯和氟化物等水溶液持续120—480h的相互作用,其结果从变质岩中活化出铜29.01—1654.24mg/mL,最高达22685.00ng/mL;钼200.00—2720.00ng/mL,最高达9990.00ng/mL;铅34.90—106.20ng/mL,最高达271.90ng/mL;锌20.00—800.00ng/mL,最高达3200.00ng/mL,它们构成了成矿热液。实验证实了前震旦系九岭群九都组是德兴斑岩铜矿铜、钼、铅、锌的矿源层。 相似文献
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The concentrations of bromine and iodine in USGS reference material MAG-1 were determined by standard addition with secondary-source x-ray fluorescence spectrometric detection. Three determinations of bromine in the same sample yielded 311, 309 and 346 μg Br/g solid. The iodine content was found to be 380 μg I/g solid. The determination of bromine in a second bottle of MAG-1 (266 ± 9 μg Br/g) indicated that a large variation in halogen concentration may exist between samples of this reference material. 相似文献
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用硝基苯萃取[Cd（Phen）3]^2＋I2^-离子对,再用盐酸反萃取,利用氢化物发生-原子荧光光谱法测定镉的含量,从而间接测定碘。实验在pH=5．2的NaAc-HAc缓冲体系下进行,优化了还原剂KBH;中邻菲罗啉的浓度,镉溶液用量,萃取剂硝基苯的用量,反萃取盐酸的酸度,并制备碘的标准曲线,其线性相关系数R2≥0．9942,线性范围0～10ng／mL,精密度为8．5％,检出限0．80ng／mL,利用标准曲线测出水样中碘的浓度为17．78ng／mL,结果令人满意。实验表明,开发原子荧光光谱间接分析方法,使其能够准确测量更多种类的元素,有着十分积极的意义,同时也能够促进该方法得到更广范的应用。 相似文献
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A Rapid Acid Digestion Technique for the Simultaneous Determination of Bromine and Iodine in Fifty‐Three Chinese Soils and Sediments by ICP‐MS 
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下载免费PDF全文 Tao He Junyi Xie Zhaochu Hu Ting Liu Wen Zhang Haihong Chen Yongsheng Liu Keqing Zong Ming Li 《Geostandards and Geoanalytical Research》2018,42(3):309-318
Bromine and iodine are important tracers for geochemical and environmental studies. In this study, a rapid acid digestion (HNO3 + HF) with ammonia dilution for the simultaneous determination of bromine and iodine in soils and sediments using ICP‐MS was developed. The recoveries of Br and I were controlled by the synergic effect of temperature and time. It took only 15 min at 140 °C for the complete recovery of Br and I in sediment (GSD‐2) and soil (GSS‐24) reference materials, which is a process that needs 2–6 h at 90 °C. A serious loss of Br and I was found at a higher digestion temperature of 190 °C. A 5% v/v NH4OH dilution effectively eliminated the memory effects and stabilised the signals of Br and I. Moreover, ammonia dilution also avoided the corrosiveness of HF on the sample introduction system and torch of ICP‐MS. Tellurium is a more suitable internal standard element than In in the ammonia medium. To avoid the adsorption of residues of dissolution on Te, addition of Te should be carried out after centrifuging the solution. The developed method was successfully applied to determine Br and I in fifty‐three Chinese soil and sediment reference materials. This simple method shows great potential for the rapid determination of Br and I in large batches of geological and environmental samples commonly analysed for mineral exploration and environmental geochemistry studies. 相似文献
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采用微波消解-电感耦合等离子体原子发射光谱法(ICP-OES)测定了不同食品中总硼的含量。对微波消解样品前处理条件和仪器参数进行了选择和优化。方法对硼元素的检出限为0.10 mg/kg。方法的精密度(RSD,n=6)为1.6%~6.8%;回收率为96.5%~104.0%。方法用于分析国家一级标准参考物质GBW 07605(茶叶)、GBW 08501(桃叶)、面粉与鱿鱼粉中的硼,测定值与标准值或参考值吻合。 相似文献
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土壤样品中有机磷农药的加速溶剂萃取-气相色谱测定 总被引：7，自引：4，他引：3
建立加速溶剂萃取提取土壤样品中13种有机磷农药残留,经Carb柱净化、Rtx-OPP2大口径毛细管柱分离、气相色谱-火焰光度检测器检测。方法仪器检出限在0.67～1.50ng/mL,线性范围在0.67～600ng/mL,相关系数在0.9994～0.9999。模拟土壤样品和实际土壤样品基体加标回收率分别在54.3%～106%和60.7%～133%,方法精密度(RSD,n=5)在2.2%～9.9%。方法简便、灵敏,适用于土壤样品中有机磷农药残留的分析。 相似文献
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硼具有两种稳定同位素10B和11B,其在自然界的丰度分别是19.90%和80.10%。自然界硼同位素组成变化很大, δ11B变化可达90‰以上(－30‰～＋60‰)。硼同位素的分析精度优于0.2‰,因此被广泛应用于多种地质过程的示踪研究。近年来,硼元素的提取、分离纯化和仪器测定技术均取得了可喜的进展,分析精度不断提高,为硼同位素地球化学研究奠定了良好的基础。本文从样品分解、化学分离和仪器测定等方面对硼同位素分析测试方法进行了归纳总结。 相似文献
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原子荧光光谱法测定铟中锡 总被引：4，自引：0，他引：4
试验了采用原子荧光光谱法测定铟产品中锡时,以EDTA为络合剂掩蔽铟,利用EDTA与铟和锡形成络合物的稳定常数不同,克服基体铟对锡的正向干扰;优化了仪器测定条件,测定范围w(Sn)为0.001%~1.00%,标准加入回收率为99%~105%。所拟方法用于铟产品中锡的测定,结果与苯基荧光酮比色法和碘量法相符。8次独立分析的精密度(RSD)为2.4%~10%。 相似文献
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The vertical distribution of iodine, bromine and organic carbon has been examined in sediment cores from a range of environments on the Namibian shelf. The relationship between Br and C org. is linear, and that between I and C org. is variable, for all surface sediments; I/C org. ratios show a decrease of about one order of magnitude between the outer shelf oxidising sediments () and the organic-rich inner shelf sediments (). The contrasting behaviour of the halogens in surface sediments is explained by differences in the amount of halogen absorbed by living organisms within the euphotic zone and on seston on the seabed. It is suggested that sorption by seston occurs only in oxidising sediment where free O2 is available. Hence, iodine is sorbed by seston in the outer shelf environment, but is not sorbed by the reducing sediments of the inner shelf. Here the iodine in the sediment represents only that taken up by plankton. On the outer shelf, 50–80% of the total iodine in the organic matter is sorbed by seston. The principal site of Br uptake is not known.The distribution of C org. in subsurface sediments broadly reflects that found at the surface, although there is a slight decrease with depth in the outer shelf cores due to dilution by terrigenous materials. In the inner shelf cores, there is no change in the relationship of iodine and bromine to organic carbon at depth. Those from the mid shelf, and especially the outer shelf, on the other hand, show decreases in both I/C org. and Br/C org. ratios, reaching values at about 70 cm depth that are similar to those in surface reduced sediments from the inner shelf. Over this depth interval I/C org. ratios decrease by a factor of five while Br/C org. ratios show a two fold decrease. These changes in the ratios at depth imply that diagenesis within the reducing cores is negligible compared with that of oxidised sediments. The implications of diagenesis with regard to halogen recycling in sediments are briefly discussed. 相似文献
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Hélène Balcone‐Boissard Agnès Michel Benoît Villemant 《Geostandards and Geoanalytical Research》2009,33(4):477-485
Concentrations of halogens (fluorine, chlorine, bromine and iodine) were determined in six geochemical reference materials (BHVO‐2, GS‐N, JG‐1, JR‐1, JB‐1b, JB‐2). Halogens were first extracted from powdered samples using a pyrohydrolysis technique, then hydrolysis solutions were analysed by ion chromatography for F and Cl and inductively coupled plasma‐mass spectrometry for Br and I. The detection limits in solutions were 100 μg l?1 for both F and Cl and 10 ng l?1 for Br and I. Considering the extraction procedure, performed on a maximum of 500 mg of sample and producing 100 ml of pyrohydrolysis solution, detection limits in rock samples were 20 mg kg?1 for F and Cl and 2 μg kg?1 for Br and I. The mean analytical errors on the studied composition ranges were estimated at 10 mg kg?1 for F and Cl, 100 μg kg?1 for Br and 25 μg kg?1 for I. The concentration values, based on repeated (generally > 10) sample analysis, were in good agreement generally with published values and narrowed the mean dispersion around mean values. Large dispersions are discussed in terms of samples heterogeneity and contaminations during sample preparation. Basaltic RMs were found to be more suitable for studies of halogen compositions than differentiated rock material, especially granites – the powders of which were heterogeneous in halogens at the 500 mg level. 相似文献