Evaluation of Pb-Pb and U-Pb Laser Ablation ICP-MSZircon Dating using Matrix-Matched Calibration Sampleswith a Frequency Quadrupled (266 nm)Nd-YAG Laser     

Olivier Bruguier  Philippe Télouk  Alain Cocherie  Anne-Marie Fouillac  Francis Albarède 《Geostandards and Geoanalytical Research》2001,25(2-3):361-373

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改进的卡洛斯管溶样等离子体质谱法测定地质样品中低含量铂族元素及铼的含量   总被引：7，自引：1，他引：7  

漆亮  周美夫  严再飞  皮道会  胡静 《地球化学》2006,35(6):667-674

报道了一个改进的卡洛斯管溶样等离子体质谱法测定地质样品中铂族元素及Re含量的新方法。将封闭的卡洛斯管置于高压釜中,然后在高压釜中加水,密封在高压釜中的水在高温下产生的外压将会抵消卡洛斯管中由酸产生的内压,这样就可以避免传统的卡洛斯管在高温高压下可能发生爆炸的危险。由此可以加大取样量,降低铂族元素测定过程中的块金效应及检出限,使超低含量铂族元素的测定成为可能。12g样品在75mL卡洛斯管中用35mL王水于320℃溶解15h,基本上可以使各种地质样品中的铂族元素矿物完全溶解。一次溶样可以测定全部铂族元素及Re,全流程空白值极低,国际标样测定结果稳定可靠。  相似文献   

贵州荔波地区2000年来石笋高分辨率的气候记录   总被引：9，自引：1，他引：9  

张美良  程海  林玉石  覃嘉铭  朱晓燕  冉景丞  杨琰  陈会明  Edwards R L 《沉积学报》2006,24(3):339-348

通过对荔波董哥洞石笋进行高精度的ICP MS或TIMS U系测年和碳、氧同位素分析，建立了荔波地区2 300a B.P.来高分辨率的古气候变化的时间序列。研究结果表明，贵州荔波地区2 300a B.P.以来石笋记录的季风气候变化，大致可分为8个气候(亚)期:① 2 300～1 800a B.P.为降温期，显示东亚夏季风减弱，东亚冬季风增强，气候干旱寒冷；② 1 800～1 080a B.P.气温有所回升，显示东亚冬季风缓慢减弱，东亚夏季风有所回升，表现为半湿润的温凉气候期；③ 1 080～680a B.P. 为降温期，气温再次下降，显示东亚冬季风再次增强，但降水相对增大，表现为寒冷湿润的气候期，是气候变化的关键转折时期；④ 680～550a B.P.温暖期，显示东亚夏季风再次增强，气温升高，降水增大，表现为温暖湿润的气候期。⑤ 550～400a B.P.寒冷期，显示东亚冬季风快速增强，气温下降，表现为寒冷湿润的气候环境，是近1 000年以来最冷的时期；⑥ 400～364a B.P.温凉期，显示东亚夏季风有所增强，气温有所回升，表现为温凉湿润气候环境；⑦ 364～324a B.P.冷凉期，显示东亚夏季风有所减弱，气温有所下降，表现为冷凉湿润气候环境；⑧ 324a B.P.至今，气候相对波动期，同位素记录曲线呈锯齿状波动，在其内包括若干个冷凉半湿润、冷湿的气候变化亚阶段。根据荔波董哥洞石笋的高分辨率的古气候变化的连续记录，揭示了荔波地区2 300a B.P.以来的一些百年尺度的重大气候事件——干旱寒冷期、隋唐温暖期(或小温暖期)、小寒冷期以及一些十年尺度的降水、温度变化。石笋记录的这种百年、十年尺度的突发性气候变化事件，与冰芯记录极为相似，反映低纬度地区石笋记录的季风气候与高纬度及北极地区的气候具有极好的相关性，这对于认识现代气候系统变化以及对未来十年—百年尺度的气候预测和演化的驱动机制，具有重要的科学意义。  相似文献   

ICP-MS测定生物样品中的微量金属元素     

王佳丽  李东雷  段英楠 《吉林地质》2007,26(4):69-72

采用SP-60型恒压消解罐消解生物样品,用ICP-MS测定8种金属元素(Mn、Zn、Pb、La、Ce、Mo、Cr和Fe)的质量分数。依据分析结果,比较了消解程序的效果。结果表明,由10.0 mLHNO3对生物样品具有很好的消解能力,各元素的测定值与推荐值相符。  相似文献   

ICP-MS测定地质样品中37个元素的准确度和长期稳定性分析   总被引：8，自引：10，他引：8  

刘晔柳小明  胡兆初第五春荣  袁洪林高山 《岩石学报》2007,23(5):1203-1210

对Elan6100DRC型ICP-MS近五年来所测得的国际地质标样BHVO-1(玄武岩)和AGV-1(安山岩)中的37个元素的测定值以及仪器灵敏度的长期漂移情况进行了统计分析(共计146次)。结果表明,几年来ICP-MS所测数据的长期稳定性和准确度都较好,除个别元素Li(BHVO-1)、Be(BHVO-1))、Cr(AGV-1)、Cs(BHVO-1)和Pb(BHVO-1)的相对误差(与参考值比较)接近或略大于10%外,绝大多数元素的相对误差和相对标准偏差(RSD,测定值之间,n=146)都在5%以内;仪器灵敏度并不是随着时间一直往下漂,有的是往上漂的,也有上下漂的,即使是在同一时间内,有的元素灵敏度往上漂,而有的往下漂。常用的内标法无法较好校正这种漂移,而需要采用内外标相结合的校正方法。不同批次,210个各种地质样品中Rb、Sr、Zr和Nb的XRF和ICP-MS分析结果对比情况表明,绝大多数样品中Rb、Sr、Zr和Nb的ICP-MS和XRF的测定值的相对误差小于10%。以上的分析结果表明,我们实验室所建立的以密闭高温高压消解技术为样品前处理方法,以模拟地壳样品中元素天然丰度比的基体匹配校正标准溶液为外标和以Rh为内标结合外标校正的ICP-MS多元素分析方法具有非常好的准确度和长期稳定性。  相似文献   

Evaluation of Simultaneous Analyte Leaching/Vapour Phase Introduction for Direct Osmium Isotope Ratio Measurements in Solid Samples by Double-Focusing Sector Field ICP-MS     

Ilia Rodushkin  Emma Engström  Douglas C. Baxter 《Geostandards and Geoanalytical Research》2007,31(1):27-38

The analytical performance of a method for Os isotope ratio measurement by double‐focusing, sector field ICP‐MS (ICP‐SFMS) was evaluated. The method is based on several optimised, concurrent processes: Os extraction from samples in hot concentrated nitric acid; separation of Os from the digest solution by the formation of volatile osmium tetroxide accelerated by continuous hydrogen peroxide addition; transport of analyte vapour by an oxygen flow into the ICP; and isotopic determination by ICP‐SFMS. Due to the very efficient utilisation of analyte (approaching 0.5‰), Os isotope ratio measurement could be performed at low pg levels. Combined with an ability to process sample sizes up to 2 g (up to 50 g if the organic matrix of biological or botanical samples is eliminated by ashing), materials with Os concentrations in the low, or even sub pg g^?1 range could be determined by this method. Given that two complete digestion/distillation systems were available for interchangeable use, throughputs of up to fifteen samples per 8 hour shift could be achieved. The method precision, evaluated as the long‐term reproducibility of ¹⁸⁷ Os/¹⁸⁸Os ratio measurements in a commercial Os reference sample containing 0.5 ng Os, was 0.16% relative standard deviation (RSD, 1s). The method has been applied to perform replicate ¹⁸⁷ Os/¹⁸⁸ Os ratio measurements on a suite of fifty reference materials of various origins and matrix compositions, with Os concentrations varying from < 0.1 pg g^?1 to > 100 ng g^?1, yielding an average precision of 3% RSD. Though none of the materials tested are certified for Os content or Os isotope composition, comparison of the obtained data with published Os isotope information for similar sample types revealed close agreement between the two. The method can also be used for the simultaneous, semi‐quantitative determination of Os concentrations.  相似文献   

Determination of Bromine and Iodine in Twenty-three Geochemical Reference Materials by ICP-MS   总被引：1，自引：0，他引：1  

Jian Y. Chai  Yasuyuki Muramatsu 《Geostandards and Geoanalytical Research》2007,31(2):143-150

Trace amounts (from nanogram to microgram levels) of bromine and iodine were determined by inductively coupled plasma-mass spectrometry (ICP-MS) in twenty-three geochemical reference materials issued by the GSJ, USGS, IAEA etc. The pyrohydrolysis technique was used to separate bromine and iodine from samples analysed in the form of powder. The accuracy and precision of the experimental values were assessed by the comparative analysis of well established reference materials such as USGS AGV-1, BCR-1 and IGGE GBW07312. The measured values agreed well with reported values within a 10% error range. We also report reliable new data for these elements in these geochemical reference materials.  相似文献   

Determination of the Platinum-Group Elements and Gold in Twenty Rock Reference Materials by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) after Pre-Concentration by Nickel Sulfide Fire Assay     

Hans-Gerrit Plessen  Jörg Erzinger 《Geostandards and Geoanalytical Research》1998,22(2):187-194

The platinum-group elements (PGE) and gold have been determined in twenty international rock reference materials by inductively coupled plasma-mass spectrometry (ICP-MS) after pre-concentration by a nickel sulfide fire assay. It was possible to achieve determination limits for a 50 g sample that ranged from 1 pg g^-1 (Rh) to 23 pg g^-1 (Au). Compared to published certified and recommended values for rock reference materials, the trueness of the method was found to be good. However, in some cases we observed large deviations for all elements in the sub 10 ng g^-1 range within individual reference sample splits. Our results show that the PGE and Au are inhomogeneously distributed in the reference materials analysed here, where they are present in low concentrations, using 50 g test portions.  相似文献   

High resolution micromill sampling for analysis of fish otoliths by ICP-MS: effects of sampling and specimen preparation on trace element fingerprints     

Arslan Z  Secor DH 《Marine environmental research》2008,66(3):364-371

Otoliths are calcified structures in the head of fish that record environmental information about fish's life history. Gathering the elemental information from the core of an otolith corresponding to the juvenile period of fish's life is critical to discriminate the adult fish to their natal habitats reliably. A high resolution micromill has been used to isolate the otolith core from a whole otolith for elemental analysis. The effects of micromilling procedures (e.g., sectioning, embedding and drilling) on contamination to otolith trace element levels were examined using paired blackfin tuna (Thunnus atlanticus) otoliths. Otoliths were decontaminated by dilute hydrogen peroxide and nitric acid throughout to remove surface contamination. A preconcentration procedure was used to determine the trace elements from the small core material by ICP-MS. It was found that micromilling procedures introduce significant contamination to otoliths, especially for Al, Cu, Pb and Zn. The sectioning procedure caused significant contamination for Co and Cu, while the embedding procedure resulted in contamination for nearly all trace elements (Al, Cd, Co, Cu, Ga, Mn, Ni, Pb, V and Zn). The combined sectioning, embedding and drilling procedure also resulted in contamination for most trace elements. Despite the contamination across all procedural steps, the decontamination procedure effectively removed the surface contamination with the exception of Pb and Zn. Bias (e.g., residual contamination) on Pb was small in comparison to overall concentration of Pb expected to occur in fish otoliths, therefore, its effect may be minor in discriminating individuals. Bias on Zn was larger that could limit its application in discriminating individuals.  相似文献   

贵州织金地区稀土磷块岩矿床中稀土元素赋存状态   总被引：10，自引：1，他引：9  

张彦斌  龚美菱  李华 《地球科学与环境学报》2007,29(4):362-368

以稀土磷块岩矿床为研究对象,采用电感耦合等离子体光谱法和质谱法研究了3个代表性样品的基本化学组成,分析了40多个元素的含量,确定了矿物质量分数和赋存状态,研究了稀土元素在其中的分布特征。结果表明,97%以上的稀土元素呈类质同象状态部分置换磷灰石晶格中的Ca2 存在,只有小于3%的稀土元素呈被粘土质等吸附状态或离子交换(吸附)状态存在。  相似文献