共查询到20条相似文献，搜索用时 93 毫秒
1.
Re-Os法能够直接厘定内生金属矿床成矿时代,但是封闭Carius管法化学流程复杂,且有一定的危险性。本文建立了一种简便快速测定辉钼矿Re-Os年龄及其Re含量的方法。用3 mL浓硝酸在10 mL比色管中溶解5~15 mg辉钼矿样品,将溶液中的钼酸沉淀分离后稀释定容,直接采用质谱测量187和185质量数比值(M187/M185)。利用辉钼矿Re-Os年龄标准物质JDC和HLP的M187/M185值与其年龄的正相关线性关系计算未知辉钼矿样品的Re-Os年龄,并通过185Re计数利用相对法计算Re含量。本方法应用于测量13.26~2130 Ma的辉钼矿,Re-Os年龄的测定值与推荐值的相对偏差多数在0.36%~7.42%之间,由于放射性积累较多,长年龄样品测量的准确度较高。与传统Carius管法相比,该方法不需要加入稀释剂,省去了封闭和打开Carius管环节以及Re-Os分离纯化流程,适合于辉钼矿Re-Os年龄的初步分析。 相似文献
2.
Re-Os同位素定年中,丙酮萃取法分离Re比传统的阴离子交换法流程简单快速.用本实验室原有丙酮萃取流程纯化的Re溶液可用电感耦合等离子体质谱(ICP-MS)测定,但由于盐量较高(＞1 mg/mL)不能直接用于负离子热表面电离质谱(N-TIMS)测定.本文对Re-Os同位素定年方法中原有丙酮萃取分离Re的流程进行改进,将丙酮萃取和碱洗时的氢氧化钠浓度由5 mol/L提高到10 mol/L,有效降低了萃取后的Re溶液中的盐量,由此分离纯化的Re溶液经硝酸和过氧化氢处理,可直接点带用于N-TIMS测定.与阴离子交换分离Re方法相比,改进的丙酮萃取方法操作简单,缩减实验时间,同时有效降低全流程空白至3 ～7 pg,并且1 ng的Re测量信号可达到100 mV以上.经国家一级标准物质(GBW 04436)和实验室铜镍硫化物监控样品(JCBY)验证,利用改进的方法纯化,Re的测定值分别为(17.17±0.50)μg/g和(38.34±0.44) ng/g,与推荐值(17.39±0.32) μg/g和(38.61 ±0.86) ng/g在不确定度范围内完全吻合.目前改进的丙酮萃取方法已经应用于实际样品分析,并取得了长期稳定的良好效果. 相似文献
3.
含辉钼矿全岩样品Re-Os同位素定年研究:在北京大庄科钼矿床中的应用 总被引：1，自引：1，他引：0
采用硝酸在比色管中对辉钼矿样品中Re含量进行初测的方法,测得辉钼矿标准样品JDC Re含量与推荐值在误差范围内基本一致,与传统的Carius管法相比,该方法具有简便快速的特点。传统的辉钼矿Re-Os同位素定年分析对象为辉钼矿单矿物,根据所测得的187Re/187Os值获得辉钼矿的Re-Os年龄,Re、Os在辉钼矿中大量富集,而在硅酸盐矿物中几乎没有,探索性地对含有辉钼矿的全岩样品进行Re-Os同位素定年,虽然所得Re、Os含量偏低,但187Re/187Os值不会变。该方法省去了选样过程花费的大量时间,避免了选样过程中可能造成的交叉污染。采用同位素稀释Carius管逆王水法探索性地对北京大庄科钼矿床中含辉钼矿全岩样品进行Re-Os同位素年龄测定,获得了(137.6±3.7)Ma精确的等时线年龄,与挑选出辉钼矿单矿物样品的Re-Os同位素等时线年龄(136.8±2.6)Ma吻合较好,直接厘定了大庄科钼矿的成矿时代。该年龄与矿区汉家川石英二长岩锆石U-Pb年龄一致,表明大庄科钼矿的形成与汉家川石英二长岩关系较为密切,为中国东部第二期大规模成矿作用的产物,形成于中国东部岩石圈伸展环境。 相似文献
4.
镁铁-超镁铁岩铼-锇同位素体系分析方法 总被引：11，自引：5，他引：11
通过试验建立了镁铁-超镁铁岩Re-Os同位素体系分析方法，包括Re-Os的化学分离纯化流程，Re同位素比值的电感耦合等离子体质谱测量方法和Os同位素比值的负离子热电离质谱测量方法。化学流程包括Carius管溶样，小型蒸馏分离Os，微蒸馏纯化Os，阴离子交换法分离、纯化Re。用该流程测定了汉诺坝幔源橄榄岩、辉石岩捕虏体和大别山饶拔寨超镁铁岩样品的Re、Os含量和Os同位素比值。 相似文献
5.
6.
云南马关县都龙锡矿万龙山矿区深部辉钼矿尚属首次发现,对此辉钼矿样品应用Re-Os同位素定年方法进行了测定,获得Re-Os同位素等时线年龄为88.9±3.5 Ma,模式年龄为89.2±1.5~91.8±1.3Ma。该Re-Os同位素等时线年龄与文山老君山花岗岩体中白云母花岗岩的形成年龄(87.6±1.4)Ma~(91.7±1.8)Ma、花岗斑岩的结晶年龄为(87.3±2.1)Ma、二云母花岗岩的成岩年龄(84.3±2.2)Ma~(85.0±1.3)Ma相吻合,表明滇东南地区的晚白垩世时期,存在大规模花岗岩成岩及锡成矿活动,两者关系密切。 相似文献
7.
《大地构造与成矿学》2020,(3)
仁里铌钽矿床是我国东部近年来新发现的超大型高品位花岗伟晶岩型铌钽矿,已探明的Ta2O5资源量10791t,Nb2O5资源量14057 t, Ta2O5平均品位0.036%, Nb2O5平均品位0.047%,矿床仍具有较大的找矿潜力。为了厘定铌钽等稀有金属矿的成矿年龄,研究其成矿物质来源,为下一步勘查及成矿预测指明方向,本次对5号主矿脉钻孔ZK1616中的4件辉钼矿样品进行了Re-Os同位素年龄测试,获得的4件辉钼矿Re-Os平均模式年龄为130.5±1.1 Ma(MSWD=0.17), 4件辉钼矿中Re含量为76.59～106.33μg/g,平均值为96.81μg/g。综合研究表明稀有金属成矿作用发生在中生代早白垩世,成矿年龄为130.5 Ma左右,成矿物质来源于壳幔混合源,以及岩浆演化晚期富F、Cl热液流体对冷家溪群地层稀有金属元素的释出、迁移和叠加。 相似文献
8.
Pt-Os、Re-Os和Hf-W同位素体系的母体和子体Pt、Os、Re、Hf和W以及其它铂族元素(PGE)化学性质上都是难熔的,我们将这些元素和相关同位素称为难熔元素和难熔元素放射性同位素体系。难熔元素及其放射性同位素体系不仅可以直接测定金属矿床、油气藏和沉积岩系的年龄,而且还可以有效示踪地球深部的核幔反应等过程,这是其它地球化学工具不可替代的。本文评述了当前Pt-Os、Re-Os和Hf-W同位素体系和PGE元素分析技术的研究进展,指出：(1)目前Re-Os同位素定年误差仍较大,迫切需要优化改进分析技术,大幅提高Re-Os同位素定年的准确度和成功率;(2)Pt-Re-Os和W同位素的分析技术需要简化繁琐的化学分离流程和提高仪器分析的效率,同时探索建立新的化学分离和仪器分析方法,进一步提高分析精度,实现对更低Pt、Re、Os和W含量样品的准确分析,才能更有效地示踪地球深部物质循环过程;(3)PGE的元素分析技术尚需改进,分析精度仍需要进一步提升。我们预期随着进一步提升难熔元素和代表性放射性同位素的分析精度,显著降低同位素定年误差,其将在核-幔、幔-幔和壳-幔物质循环过程示踪、金属矿床精细... 相似文献
9.
Re-Os同位素定年技术在富有机质沉积岩、低变质沉积岩、湖相沉积物、煤、油气藏样品等富碳质地质样品的尝试和成功应用,使其成为直接厘定地层沉积时代、重大地质事件发生时限和机制、古环境重建、油气藏直接定年、油气演化过程推演等研究的关键技术手段。然而,受到富碳质地质样品中极低的Re和Os丰度、采样方式以及地质作用等因素的影响,很多样品的Re-Os等时线年龄和初始Os同位素比值精度超过10%,不能有效地评价海水Os的真实来源和地质作用程度,影响了对不同沉积体系及油气演化过程中Re和Os的化学行为和Re-Os等时线年龄地质意义的理解。由此,本文从富碳质地质样品的Re-Os化学行为和地质应用进展出发,对富碳质地质样品Re-Os同位素分析过程中的采样和取样方式、溶样方法、分离富集方式和标准物质选择四方面进行了总结和完善。指出以沉积速率为采样间距参考,通过预处理方式提高样品的均匀性,使用流程空白更低、对同位素分馏影响更小的溶样方法和分离富集方式进行Re-Os同位素分析,以基质匹配的地质标样进行数据监控可进一步提高样品Re-Os同位素分析质量,有助于不同类型富碳质地质样品Re和Os赋存机制研究、Re-O... 相似文献
10.
辉钼矿的铼-锇同位素地质年龄测定方法研究 总被引：234，自引：27，他引：234
本研究在国内首次将同位素稀释等离子体质谱法应用于铼-锇同位素系统地质年龄测定。建立的化学分离方法包括碱熔分解样品、丙酮萃取分离铼、 蒸馏法分离锇。全流程化学回收率在90％以上。铼和~(187)Os的空白值分别为0.07ng和0.01ng。用本法测定了我国4个钼矿床的辉钼矿矿化年龄,其年龄测定精度(2σ)在3％以内。测定结果与地质背景的符合情况令人满意。直接测定金属矿床年龄的铼-锇法较之间接测定围岩时代来推断矿化年龄的其它定年方法更能反映真实年龄。鉴于许多热液硫化物矿床常含有辉钼矿,该法有较广泛的应用前景。 相似文献
11.
12.
Yoshio Takahashi Tomoya Uruga Hajime Tanida Keiko H. Hattori 《Geochimica et cosmochimica acta》2007,71(21):5180-5190
Local atomic structures of Re and radiogenic Os in molybdenite from the Onganja mine, Namibia, were examined using X-ray absorption fine structure (XAFS). Rhenium LIII-edge X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) show that the oxidation state of Re, the interatomic distances between Re and the neighboring atoms, and the coordination number of Re to S are very similar to those of Mo in molybdenite. The results confirm that Re is present as Re(IV) in the Mo site in molybdenite.Measurement of LIII-edge XANES and EXAFS of a minor concentration (8.55 ppm) of radiogenic Os was accomplished in fluorescence mode by removing the interfering X-rays from Re and other elements using a crystal analyzer system. The data indicate that the oxidation state of radiogenic Os is Os(III) and Os(IV) and clearly different from Os(II) in natural sulfide minerals, such as OsS2 (erlichmanite). XANES data also suggest that radiogenic Os does not form a secondary Os phase, such as OsS2 or Os metal, in molybdenite.EXAFS of radiogenic Os was successfully simulated assuming that Os is present in the Mo site in molybdenite. The data are consistent with the XANES data; Os does not form Os phases in molybdenite. The EXAFS simulation showed that the interatomic distance between Os and S is 2.27 Å, which is 0.12 Å smaller than the distances of Re-S and Mo-S (2.39 Å) in molybdenite. Similar valences and ionic sizes of Re and Mo in molybdenite support the fact that large amounts of Re can be incorporated into the Mo site as has been observed in previous studies, whereas the different properties of Os compared to Mo and Re suggested here support much lower abundance of common Os in molybdenite. This makes molybdenite an ideal mineral for the Re-Os geochronometer as shown in many studies. However, the shorter distance between radiogenic Os and S compared to those of Re-S and Mo-S in molybdenite suggests that the radiogenic Os has a smaller ionic size than Re(IV) and Mo(IV). Furthermore, Os may be partly present as Os(III). Smaller and lower charge Os can diffuse faster than larger and higher charge Re in molybdenite at a given set of conditions. Hence, our study provides an atomic-level explanation for the high mobility of Os compared to Re, which has been suggested by earlier workers using laser ablation ICP-MS. 相似文献
13.
Digestion with aqua regia in a Carius tube and separation of Re with anion exchange resin is commonly employed for Re–Os dating of molybdenite and pyrite. However, the recovery of Re is extremely low when this routine anion exchange method is applied to galena, causing difficulty in Re–Os dating of galena. In this study, we investigated the mechanism of Re loss during sample preparation and tested a revised procedure for Re–Os dating of galena and sphalerite. 相似文献
14.
Jie Li Xiao‐Ying Jiang Ji‐Feng Xu Li‐Feng Zhong Xuan‐Ce Wang Gui‐Qin Wang Pei‐Pei Zhao 《Geostandards and Geoanalytical Research》2014,38(1):37-50
We report an improved procedure for the determination of the platinum‐group elements (PGE) and Re, and Os isotopes from a single sample aliquot by isotope dilution (ID) using inductively coupled plasma‐mass spectrometry (ICP‐MS) and negative thermal ionisation mass spectrometry (N‐TIMS), respectively. A two‐stage column method was used to purify PGE‐Re from their sample matrix and interfering elements (e.g., Mo, Zr and Hf) after Os had been separated by CCl4 solvent extraction. The first column separation step used cation exchange resin (AG50W‐X8) to concentrate PGE‐Re and some potential interfering elements (e.g., Mo, Zr and Hf). In the second step, N‐benzoyl‐N‐phenylhydroxylamine (BPHA) extraction resin was used to separate PGE‐Re from the remaining interfering elements, which all remained strongly absorbed to the resin. The method was used to determine the PGE and rhenium, and Os isotope ratios in a range of geochemical reference materials (TDB‐1, WGB‐1, BHVO‐2 and UB‐N). The obtained results agree well with those previously published. This new method enables PGE‐Re abundances and Os isotopic ratios to be determined on the same sample digestion, and circumvents the problems created by sample heterogeneity when comparing PGE and Re‐Os isotope data. 相似文献
15.
We present a detailed study of Re-Os age determinations for eight natural molybdenite samples of like polytype (2H), spanning a range of age, natural grain size and deposit type. The focus of the study is to critically evaluate the effects of sampling, sample preparation and aliquant size on the accuracy and reproducibility of Re-Os ages for these molybdenite samples. We find that for some molybdenite samples, analysis of small sample aliquants (<20 mg) may not yield accurate or reproducible Re-Os ages, whereas analysis of larger aliquants from the same mineral separate do yield reproducible Re-Os dates. Such an observation is best explained if Re and 187Os are internally decoupled within molybdenite grains. This finding is supported from spot analyses by laser ablation MC-ICP-MS analyses presented here and is consistent with previously published observations.The degree of decoupling between Re and 187Os appears to increase both as a function of increasing grain size, and increasing age of molybdenite. From detailed dating of individual molybdenite mineral separates, we provide approximate minimum aliquant amounts required for reproducible Re-Os age dating, as a function of molybdenite age and grain size. Geologically younger, naturally fine-grained molybdenite samples appear to show little Re and 187Os decoupling, and reproducible ages can be determined from some samples with as little as 1 mg of aliquant. Geologically old, and coarse-grained molybdenite samples may require as much as 40 mg of aliquant from a much larger mineral separate to overcome Re and 187Os decoupling. The mechanism(s) of Re and 187Os decoupling within molybdenite is not constrained by this results of this study, but the observation that the degree of decoupling increases with grain size (distance) and age (time/geologic history) may suggest primary diffusive control. Assuming that Re and 187Os decoupling in molybdenite results primarily from diffusion of 187Os, apparent diffusion coefficients are calculated (D = x2/t). Estimates of D for Os made in this way range from 2.8 × 10−26 to 2.1 × 10−21 m2/s, which are broadly similar to experimentally derived diffusion coefficients for Os in Fe-sulfide minerals and for Re in molybdenite at temperatures <500°C. 相似文献
16.
The Re–Os (rhenium–osmium) chronometer applied to molybdenite (MoS2) is now demonstrated to be remarkably robust, surviving intense deformation and high‐grade thermal metamorphism. Successful dating of molybdenite is dependent on proper preparation of the mineral separate and analysis of a critical quantity of molybdenite, unique to each sample, such that recognized spatial decoupling of 187Re parent and 187Os daughter within individual molybdenite crystals is overcome. Highly precise, accurate and reproducible age results are derived through isotope dilution and negative thermal ion mass spectrometry (ID‐NTIMS). Spatial decoupling of parent–daughter precludes use of the laser ablation ICP‐MS microanalytical technique for Re–Os dating of molybdenite. The use of a reference or control sample is necessary to establish laboratory credibility and for interlaboratory comparisons. The Rb–Sr, K–Ar and 40Ar/39Ar chronometers are susceptible to chemical and thermal disturbance, particularly in terranes that have experienced subsequent episodes of hydrothermal/magmatic activity, and therefore should not be used as a basis for establishing accuracy in Re–Os dating of molybdenite, as has been done in the past. Re–Os ages for molybdenite are almost always in agreement with observed geological relationships and, when available, with zircon and titanite U–Pb ages. For terranes experiencing multiple episodes of metamorphism and deformation, molybdenite is not complicated by overgrowths as is common for some minerals used in U–Pb dating (e.g. zircon, monazite, xenotime), nor are Re and Os mobilized beyond the margins of individual crystals during solid‐state recrystallization. Moreover, inheritance of older molybdenite cores, incorporation of common Os, and radiogenic Os loss are exceedingly rare, whereas inheritance, common Pb and Pb loss are common complications in U–Pb dating techniques. Therefore, molybdenite ages may serve as point‐in‐time markers for age comparisons. 相似文献
17.
辉钼矿Re-Os同位素定年方法的改进与应用 总被引：13，自引：9，他引：4
公认的Re-Os同位素定年代表物辉钼矿,目前已在金属硫化物矿床年代学研究领域获得了广泛的应用。本研究采用浓HNO3分解辉钼矿样品,大大地简化了Re和Os的化学制备过程,并根据辉钼矿中正常Os含量水平相对放射成因187Os可以忽略的特点,以正常Os标准为稀释剂,实现了仪器测量过程中Os同位素质量分馏的在线校正,改善了分析数据的质量。该方法经辉钼矿国家标准物质进行验证,获得了满意的Re、Os含量及Re-Os年龄数据,并且在南岭地区与连阳复式岩体相关的姓坪夕卡岩型钼矿床成矿年龄研究中获得了成功应用。在实际应用中,为了获得有意义的能反映真实地质事件的年龄数据,辉钼矿样品不仅要有足够的取样量,而且还要保证粒度细、混合均匀。 相似文献
18.
铼-锇同位素分析样品预处理研究进展 总被引：1，自引：0，他引：1
文章评述并归纳了近年来地质样品中Re-Os同位素分析的化学前处理方法研究进展。总结了锍镍火试金法、碱熔法、Carius管溶样法以及HPA-S高温高压釜溶样法等常用的Re-Os同位素样品消解方法。归纳了离子交换、溶剂萃取富集Re以及蒸馏、萃取等分离富集Os的方法。由于地质样品的复杂性,Re、Os含量的不均一性及测试方法的多样性,要求在具体分析过程中不同的样品使用不同的消解方法和分离富集方法。当前国内应用较成熟的Re、Os分离方法是Carius管逆王水分解样品,原位蒸馏或CCl4萃取方法分离Os,阴离子交换法或丙酮萃取分离Re。 相似文献
19.
Reproducibility of Re-Os molybdenite ages depends on sample size and homogeneity, suggesting that Re and Os are decoupled within individual molybdenite crystals and do not remain spatially linked over time. In order to investigate the Re-Os systematics of molybdenite at the subgrain (micron) scale, we report LA-ICP-MS Re-Os ages for an Archean molybdenite crystal from Aittojärvi, Finland, analyzed in situ in a white aplite matrix. A related Aittojärvi molybdenite (A996D), in the form of a very fine-grained mineral separate, is used as one of our in-house NTIMS standards, and thus its age of 2760 ± 9 Ma is well established. Measurements of (187Re + 187Os)/185Re on micron scale spots along 200 μm traverses across the crystal yield a wide range of ages demonstrating that, in this case, microsampling of molybdenite does not produce geologically meaningful ages. Experimentation with mineral separations and sample size over a 7-yr period predicted that this would be the outcome. We suggest that 187Os is more likely to be the mobile species, based on its charge and ionic radius, and that 187Os becomes decoupled from parent 187Re with time on the micron and larger scale. Incompatible charge and ionic radius for Os ions formed during reduction of molybdenite-forming fluids may explain the widely observed absence of common (initial) Os in molybdenite. Geologically accurate ages for molybdenite can only be obtained for fully homogenized crystals (or crystal aggregates) so that any post-crystallization 187Re-187Os decoupling is overcome.A growing number of geologically accurate ID-NTIMS 187Re-187Os ages for homogenized molybdenite suggest that postcrystallization mobility of radiogenic 187Os must be limited to within the molybdenite mineral phase. We suggest that radiogenic 187Os may be stored in micron scale dislocations, kink bands, and delamination cracks produced by deformation, and that the unusual structure and deformation response of molybdenite results in an increased chemical stability in this mineral. Migration of 187Os into adjacent silicate phases is highly unlikely, but other contacting sulfides may take in Os. In an example from a Proterozoic skarn deposit at Pitkäranta (western Russia), we demonstrate minor loss of radiogenic 187Os from molybdenite and a corresponding gain in adjacent chalcopyrite such that the molybdenite age is not perceptibly disturbed, whereas the resulting chalcopyrite ages are impossibly old. Therefore, it is unadvisable to perform Re-Os analytical work on any sulfide in contact or intimate association with molybdenite. In addition to large errors in the age, if the isochron method is employed, initial 187Os/188Os ratios could be erroneously high, leading to seriously errant genetic interpretations. 相似文献