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电感耦合等离子体质谱法同时测定地质样品中痕量碘溴硒砷的研究：Ⅱ.土壤及沉积物标准物质分析 总被引：11，自引：8，他引：11
样品用碳酸钠和氧化锌混合熔剂半熔，热水提取，然后用强酸性阳离子交换树脂将阴离子形式存在的分析元素与溶液中大量钠、锌等阳离子分离，采用电感耦合等离子体质谱法直接同时测定溶液中的碘、溴、硒、砷。用0.07mol/L的氨水溶液清洗进样系统，有效减少了碘等元素的记忆效应和清洗时间。方法检出限（10σ，DF=100）溴、碘分别为0.15和0.028μg/g，砷、硒分别为0.04和0.004μg/g。用土壤和沉积物等地质标准物质分析验证了方法的准确度和精密度，绝大多数分析结果在标准值的允许误差范围之内。样品10次测定的RSD为0.8%～2.8%。 相似文献
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原子荧光法测定地质样品中的硒、砷已被广泛应用。但用于测定动物组织中痕量硒、砷却报道不多，本文着重研究了动物组织的消化条件及测试条件。经对国家标准物质ＧＢ０８５５１猪肝标样进行分析，结果令人满意。 相似文献
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现有的国家标准及行业标准方法测定水中溴及碘均较繁琐、效率低，且结果是某一形态溴或碘含量，不同方法得到的结果存在差异，建立一个简单快速测定地下水中溴量及碘量的方法非常重要。在优化仪器参数下，建立了电感耦合等离子体质谱同时测定地下水样品中溴含量及碘含量的方法，研究了测定中钾对溴的干扰因素，并对比讨论了不同实验条件下的结果，以及pH对样品测定的影响。最终确定水介质的Re元素作内标，定量限均为1.01μg/L,精度为2.80%,用国家标准物质验证了该方法的准确度，测定实际地下水样品加标回收率均为85%～110%,可用于无有机污染的地下水等环境水质检测。 相似文献
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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 总被引：2，自引：2，他引：0
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. 相似文献
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对氢化物发生-原子荧光法同时测定水中砷、硒含量的条件进行探讨,并通过实例进行验证。通过对不同仪器测试条件和试剂用量的分析,选择最优测试条件进行测试,测定线性关系0.999,砷、硒检出限低,分别为0.052和0.073μg/L,满足检测应用要求;并且通过国家标准样品测试和地下水样品加标实验进行验证,标准样品测试结果与加标回收率均合格,方法的准确度及精密度结果满意。该实验方法操作简单、快速,适用于地下水中砷、硒的同时测定。 相似文献
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水系沉积物和土壤中硒含量极低,一般为0.xppm,用通常方法测定有一定困难。ICP测定硒检出限约为50μg/ml,即使采用分离富集手段也难以测定。 Thompson等首先报导将氢化物发生法用于ICP—AES测定砷、锑、铋、硒和碲等元素,大大地改善了它们的检出限, 相似文献
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为了探讨中国西南地区二叠系乐平统(上二叠统)龙潭组中下部煤系不同煤组分中砷、硒的含量和演化及古环境意义,对近10年来采集于中国西南扬子地台的二叠系乐平统龙潭组主采煤层的原煤、亮煤、煤矸石、黄铁矿结核等样品中砷、硒元素含量进行了测定和分析,并与中国华北地台一些煤矿的上石炭统-下二叠统太原组、山西组的原煤、镜煤、亮煤、煤矸石、黄铁矿结核等样品中砷、硒含量进行对比分析。结果表明：西南地区乐平统龙潭组煤的砷、硒含量变化较大,但总体高于华北晚石炭世和早二叠世煤的砷、硒含量;西南二叠系乐平统龙潭组大多数的亮煤中砷、硒含量高于原煤全煤样(刻槽样)中的砷、硒含量,也远远高于同煤层煤矸石的含量,龙潭组部分亮煤的砷含量尤其高,为55～338 mg/kg,还发现砷含量为89 mg/kg的亮煤。但华北上石炭统-下二叠统的镜煤中的砷、硒含量与之相反,低于原煤全煤样的砷、硒含量,其中砷含量非常低,为063～129 mg/kg。说明西南地区上二叠统煤中的砷和硒与煤的有机质密切相关,可能主要来源于成煤古植物。在西南乐平世早、中期第Ⅰ幕陆生生物集群灭绝事件期间,陆生动物的食物--植物中有毒有害元素砷、硒含量明显增加,陆生环境或泥炭沼泽中可溶性砷、硒含量增加。 相似文献
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建立了电感耦合等离子体质谱法同时测定地下水中B、Br、I的方法。选定φ=2%(体积分数)的稀NH3.H2O介质消除碘的记忆效应。采用干扰较少的10B和79Br同位素。B、Br、I在0~10 000 ng/mL呈良好的线性关系。方法的检出限为10B 0.176 ng/mL,79Br 0.876ng/mL,127I 0.132 ng/mL;精密度(RSD,n=12)为10B 2.86%,79Br 3.36%,127I 2.69%;10B的阶梯加标回收率为94.6%~101.5%,79Br为98.3%~104.9%,127I为96.5%~102.0%。 相似文献
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耦合等离子体质谱技术在地质调查中的应用研究 总被引：6，自引：1，他引：6
本文简要介绍近年来开展的ICP—MS在地质调查中的应用研究工作进展。新方法包括镍锍试金-ICPMS测定铂族元素；封闭酸溶-ICPMS测定地质样品中稀土等47个元素；封闭酸溶乙醇增强ICP—MS测定碲；半熔或稀氨水封闭溶样ICP—MS测定碘溴等非金属元素。 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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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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样品经硝酸、氢氟酸、高氯酸分解，制成硝酸溶液，经巯基棉层析柱过滤富集Ag，并用2mol／LHBr溶液洗脱，用火焰原子吸收法测定洗脱液中的Ag和滤液中的Cu，Pb，Zn。用该法测定化探样品中银和铜铅锌，检出限低，结果准确度和精密度均令人满意。 相似文献
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Determination of Halogens (F, Cl, Br, I), Sulfur and Water in Seventeen Geological Reference Materials 总被引：5，自引：0，他引：5
Fluorine, chlorine, bromine, iodine and sulfur were determined in seventeen geological reference materials after extraction by pyrohydrolysis. Fluorine, Cl and S (as sulfate ions) were determined in the extraction solution by ion chromatography with detection limits of around 0.2 mg l−1 . Bromine and I were measured by ICP-MS with detection limits of 1 μg l−1 for Br and 0.1 μg l−1 for I. For rock samples, using normal extraction conditions (500 mg of sample and 100 ml of final solution) detection limits were 40 mg kg−1 for F and Cl, 15 mg kg−1 for S, 0.2 mg kg−1 for Br and 0.02 mg kg−1 for I. These detection limits may be improved by increasing the amount of sample and hence the concentration of the final solution. Water was also determined using an extraction technique based on H2 O degassing, reduction on zinc at 1000 °C and H2 manometry. Our results for fluorine, chlorine, sulfur and water are in good agreement with literature data. Very few reference materials have recommended values for bromine and especially for iodine. Among the analysed samples, three are new reference materials: BHVO-2, BCR-2 and AGV-2. 相似文献
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Li Bing Ma Xinrong Han Lirong Yang Hongxia 《Geostandards and Geoanalytical Research》2004,28(2):317-323
A simple sample treatment method for the accurate and precise determination of iodine in soil, sediment and biological samples by inductively coupled plasma-mass spectrometry (ICP-MS) is described. Iodine in samples was extracted in screw top PTFE-lined stainless steel bombs using a 10% v/v ammonia solution at 185 C for 18 hours (overnight), after which the extract was introduced into the ICP-MS for direct measurement. 126 Te was employed as the internal standard to compensate for matrix effects and instrument drift. The limit of detection (LOD, three times the standard deviation of the procedural blank solution, expressed as the concentration in the sample solution) was 0.003 ng ml--1 . The limit of quantitation (LOQ, ten times the standard deviation of the procedural blank solution, expressed as the concentration in the solid samples, dilution factor DF = 100) was 0.01 μg g--1 (dry mass). The accuracy and precision of the method were demonstrated by analysing different Chinese geological certified reference materials (soils, stream sediments and a hair sample). The measured concentrations were in a good agreement with the certified values indicating that bias in the method was not significant. The precision (n = 10) for different concentrations ranged from 1.82% to 4.32% RSD. Comparison of the ammonia extraction procedure with a "sintering" method indicated that there was no significant difference in results obtained with the two methods for geological soil and stream sediment samples. However, for biological samples, such as hair, kelp, tea etc., the results obtained by the sintering method were far below those of the ammonia extraction method. The ammonia extraction has advantages, as it is simpler than the "sintering" method, and has a lower procedural blank, better detection limits and reproducibility. Due to the simplicity of the method, a high rate of sample throughput is possible. 相似文献
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建立了利用GasBenchⅡ联用同位素比值质谱仪（GasBench Ⅱ-IRMS）用于测定地下水中溴稳定同位素的方法。基于溴比氯更容易被重铬酸钾氧化的性质,将Br-氧化成Br2,而氯残留在原溶液中,从而把溴与氯分离开;再利用AgNO3将溴以AgBr的形式沉淀下来,然后将AgBr转化成CH。Br进行溴稳定同位素质谱测定。反应中,CHsI用量为20μL,AgBr用量为0．5mg。本测试流程需溴4～10mg,质谱测试时问由1．5h缩短为800s,测试精度优于±0．1‰（2σ）。该方法可以用于地下水中溴同位素测定,在水文地质研究中具有广阔的应用前景。 相似文献
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Marcel LANGENAUER Urs KRÄHENBÜHL Verena FURRER Armin WYTTENBACH 《Geostandards and Geoanalytical Research》1992,16(1):41-44
The concentrations of fluorine, chlorine, bromine and iodine of seven geochemical reference samples have been determined. Analytical techniques were neutron activation analysis for chlorine, bromine and iodine and ion-selective potentiometry for fluorine. After irradiation of the samples, these halogens were separated from the matrix elements by pyrohydrolysis in presence of vanadium (V) oxide. This extraction allows to measure the four halogens in the same sample. 相似文献