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1.
元素分析仪-同位素比值质谱仪测定海洋沉积物有机碳稳定同位素方法初探 总被引：9，自引：6，他引：3
初步建立了利用元素分析仪-同位素比值质谱仪(EA-IRMS)联用技术测定海洋沉积物中有机碳稳定同位素的方法。标定了标准工作参考气CO2(δ13CvsPDB为-32.053‰);验证了仪器的稳定性,标准偏差为0.009‰;当离子流强度范围为0.4～8.7 V时,总体线性为0.0337‰/V,小于仪器线性指标0.06‰/V的要求;同时测定了国家标准物质GBW 04408、国际标准物质Urea和海洋沉积物样品M01的精密度和准确度,标准偏差在0.04‰～0.13‰范围内;并在三家实验室进行了测量比对实验,标准偏差小于0.20‰,满足地质样品再现性0.5‰的要求。所选样品区域δ13Corg范围为-25.29‰～-22.30‰,表明该海域总有机碳是陆源和海源两种来源的混合物。 相似文献
2.
渤海东海海洋沉积物中碳氮稳定同位素标准物质研制 总被引：2，自引：2，他引：0
海洋沉积物中碳氮稳定同位素因其能够确定有机质的来源,有助于了解碳循环、气候变化、有机质迁移转化而备受关注,但其分析测试过程中尚缺乏海洋沉积物碳氮稳定同位素标准物质进行质量监控。本文依据ISO导则35和国家《一级标准物质技术规范》(JJG1006—1994),研制了三个海洋沉积物碳氮稳定同位素标准物质(MSCNI-1、MSCNI-2和MSCNI-3),候选物样品分别采自我国渤海锦州湾湿地、东海闽浙近岸和东海冲绳海槽,定值组分为总碳氮同位素(δ~(13)C-TC、δ~(15)N-TN)和有机碳氮同位素(δ~(13)C-C~(org)、δ~(15)N-N~(org)),定值方法采用元素分析-同位素比值质谱法(EA-IRMS)多家实验室协同定值。经检验,三个标准物质候选物均匀性良好,一年内定值组分均无显著变化,具有良好的稳定性;δ~(13)C和δ~(15)N的标准不确定度分别小于0.15%和0.24%,标准值和标准不确定度合理。该套标准物质是我国以海底沉积物为介质的基体型碳氮稳定同位素标准物质,定值方法准确可靠,可供海洋、地质及环境等相关领域实验室用于仪器校准、方法评价和质量监控等。 相似文献
3.
实验室和研究人员所使用的碳、氮同位素标准物质一般由国际原子能机构(IAEA)获得,然而近年来,随着碳氮同位素在实验室质量监控、方法评价、仪器校准等方面的广泛应用,市场需求量不断增加, IAEA研制的碳、氮同位素标准物质的种类与数量逐渐不能满足科学研究快速发展的需求。我国急需研制适应当今分析技术水平的有机质碳氮同位素国家标准物质用以进行质量监控、方法评价、仪器校准。为保证量值传递精度,本文研制了4个有机化学物质的碳氮稳定同位素标准物质,其中3个为尿素样品,1个为L-谷氨酸。经检验4种标准物质的均匀性通过F值检验,标准物质的δ~(13)C和δ~(15)N值经过一年的稳定性检验,特征量值变化在测量方法允许的不确定度范围内,由此判定δ~(13)C和δ~(15)N值稳定性良好。由包括研制单位实验室在内的12家实验室协同定值,采用高温燃烧-气体同位素质谱法测定了δ~(13)C和δ~(15)N值,系列标准物质δ~(13)C和δ~(15)N认定值区间呈梯度分布,δ~(13)C值为-40‰～0‰,δ~(15)N值为-10‰～30‰,涵盖了我国天然样品中有机质碳氮稳定同位素组成范围;研制的系列标准物质δ~(13)C的定值扩展不确定度不大于0.08‰,δ~(15)N的定值扩展不确定度不大于0.09‰,定值水平与国际标准物质相当。该系列标准物质已被国家质检总局批准为国家一级标准物质,批准号为GBW04494～GBW04497。可被用于地质、生态、环境等多种样品δ~(13)C和δ~(15)N比值测定时的分析监控、仪器校准、方法评价、质量保证和质量监控。 相似文献
4.
激光同位素光谱法测量水中氢氧同位素组成的实验室间比对研究 总被引：3，自引：3，他引：0
激光同位素光谱分析方法是近些年使用较广泛的一种便捷、快速的测试稳定同位素组成的技术,能同时分析出水中δD、δ~(18)O同位素组成,因其操作简单,检测效率高,体积小,野外现场测试携带方便,迅速在环境、地质、生态和能源等领域得到广泛应用,但是该测试分析方法尚没有相应的国家标准,测试结果得不到有效的溯源,在使用过程中缺乏规范和统一。为此,本文通过在全国范围内12家实验室选取8个比对水样(δD值在-189.1‰~-0.4‰内,δ~(18)O值在-24.52‰~0.32‰内),利用激光同位素光谱法测试比对D/H和18O/16O值,探讨激光同位素光谱仪分析水中δD、δ~(18)O值的准确度和精密度。测试结果表明:各个协作实验室数据准确、稳定,方法的重复性和再现性良好;激光光谱法测定的δD精密度为0.4‰(1σ),δ~(18)O精密度为0.05‰(1σ),与传统稳定同位素质谱的精度几乎一致,因此适用于常规水样中δD、δ~(18)O测定,可以开展野外在线实时检测水中氢氧同位素组成。本研究为开展制定激光同位素光谱法测定环境液态水中δD、δ~(18)O同位素组成标准方法的工作推广和应用提供了参考。 相似文献
5.
测定矿物或水中硫酸根的氧同位素组成(δ18O)能够识别物质来源及转化过程,常用的方法是将硫酸根转化为硫酸钡再用离线或在线法测试其δ18O值。目前普遍采用1420℃在线测试硫酸钡的氧同位素组成,该方法极易缩短反应炉的寿命,通过添加还原剂碳可以降低反应温度,但是已有报道对于添加还原剂后的反应温度讨论较少。本文选择镀镍碳(Ni-C)作为还原剂,将样品经Ni-C高温处理后进行一系列条件实验,确认了采用元素分析仪-稳定同位素质谱仪(EA-IRMS)测定硫酸钡中氧同位素组成的分析方法的关键技术参数:硫酸钡在线反应温度为1350℃; Ni-C与硫酸钡样品量的质量比范围选择0. 73～2. 15;为了获得更加精确的数据,硫酸钡与Ni-C用量都控制在700±100μg。在以上实验条件下,EA/HT-IRMS测定硫酸钡δ18O值的精密度为±0. 12‰～±0. 26‰,优于在线法已报道的精密度±0. 20‰～±0. 50‰。本方法在满足测试精密度的前提下,通过添加Ni-C降低了硫酸钡在线反应温度,延长了反应炉使用寿命。 相似文献
6.
元素分析仪-同位素比值质谱测量碳氮同位素比值最佳反应温度和进样量的确定 总被引：2，自引：2，他引：0
沉积有机质的碳氮稳定同位素值是进行古气候、古环境及生态系统研究不可或缺的主要研究手段,目前碳氮同位素主要利用元素分析仪-同位素比值质谱(EA-IRMS)系统来测定。EA-IRMS测定过程中的反应温度及样品进样量直接影响反应物在测试中的燃烧程度,从而影响测试数据的精度。本文利用EA-IRMS技术,以标准样品为参考,在不同转化温度下测试碳氮同位素值,研究保证测试精度的最佳反应温度条件;同时,通过分析不同含氮量样品的检测限,明确了样品含氮量与最低检测限之间的关系,确定了精确测定氮同位素值的最低进样量。结果表明:反应温度对测试精度有显著影响,在碳同位素测定时,将反应温度设定为900℃或以上时测试精度均能达到±0.2‰;氮同位素测定时,反应温度须设定为950℃时测试精度才能达到±0.3‰。实验得出样品含氮量与检测限之间的线性相关性为R2=0.873,开展氮同位素测定时可根据此关系来判断和控制进样量。 相似文献
7.
三种方法测试岩溶水样氢氧同位素的对比研究 总被引：1，自引：0，他引：1
通过高温热转换元素-同位素比值质谱法（TC/EA-IRMS）、多用途气体制备仪-同位素比值质谱法（GasbenchⅡ-IRMS）以及激光光谱法对岩溶水样进行对比检测,其结果显示:对于氢同位素,TC/EA-IRMS的精密度达到0.3 ‰,激光光谱法的精密度达到0.1 ‰,均优于GasbenchⅡ-IRMS的精密度1.4 ‰;对于氧同位素,GasbenchⅡ-IRMS的精密度达到0.02 ‰,激光光谱法的精密度达到0.04 ‰,优于TC/EA-IRMS的精密度0.16 ‰。使用激光光谱法测定岩溶水样的氢氧同位素,所需要的样品量少,精密度高,能够满足岩溶区样品的高精度测试要求。 相似文献
8.
地下水硝酸盐15N和18O同位素在线测试技术研究 总被引：1，自引：1，他引：0
测定水和土壤的氮氧同位素组成能够识别硝酸盐来源和研究氮素的迁移转化过程,用在线高温热解法测试硝酸盐的15N和18O同位素是目前应用最广泛、最流行的高新技术.但是由于离子源内NO的干扰,使该方法测定的δ㈨O值不准确,而采用He稀释法则可有效减少该项干扰 本文选取4个国际标准样品(IAEA-No-3、USGS32、USGS34和USGS35)和一个实验室标准样品(CUGL-No-1),使用元素分析仪耦合MAT 253稳定同位素比值质谱仪(EA-IRMS),在8个月时间内对100多个地下水样品进行238次测试,对在线高温热解测试硝酸盐15N和18O技术进行了检验,验证其实用性.得到三点新认识:①用KNO3作为靶样品形式成本低,且便于和国际标准对比;②在线高温热解法测定标准和样品中硝酸盐的15N和18O同位素组成需样量仅为500μg的KNO3,一次选样可同时测定NO3的δ15N和δ 18O,消耗时间仅720 s,δ15N和δ 18O的测试精度分别为0.25‰、0.6‰,达到了国外相应水平,速度快,效率高;③He稀释法可减少离子源内NO对δ 18O测试的干扰,不必改变EA-IRMS系统的任何硬件. 相似文献
9.
海洋沉积物有机碳和稳定氮同位素分析的前处理影响 总被引：2，自引：0，他引：2
海洋沉积物中的有机碳和稳定氮同位素为海洋古环境和碳氮循环提供了大量信息,然而不同的前处理方法对有机碳和稳定氮同位素测定结果的准确性产生不同程度的影响.笔者通过大量条件实验,分析了前处理过程中影响结果准确性的可能因素.①器皿材质:使用聚丙烯和玻璃离心管进行酸处理所得样品的δ13C和δ15N基本无差别.②干燥方式:样品经热烘干燥会导致样品中轻碳组分和易挥发组分的逸散,引起样品中δ13C的分馏.鲜样和酸处理后样均采用热烘干燥会引起样品中δ15N发生明显分馏.③驱酸方式和洗酸程度:水洗造成溶解性有机碳和氮的损失,致使δ13C和δ15N值较真实值偏正,但酸蒸法不能保证氯离子的有效驱除.洗至中性后的洗酸次数对δ13C影响甚小,但会导致δ15N继续偏正.全程采用冷冻干燥,选用PP离心管作为主要酸处理水洗和干燥的器皿,具有很好的重复性,可获得较理想、准确的δ13C和δ15N测试数值. 相似文献
10.
样品质量对EA-IRMS法测量硫同位素组成的影响 总被引：2，自引：0，他引：2
研究不同样品质量对EA-IRMS法测量硫同位素组成的影响,通过对质量为47~1124μg国家标准物质硫化银GBW04414质量数66、65、64的SO2+和质量数50、49、48的SO+测试,结果表明该方法精密度受到样品质量的影响较大。当δ~(34)S的精密度要求标准偏差±0.2‰时,控制硫化银的样品质量应为(420±50)μg,即样品的硫含量应为(54±6)μg为佳。国家标准物质GBW04414的质量在380~420μg之间,δ~(34)S和δ~(33)S的精密度较高,标准偏差分别为±0.14‰、±0.09‰,精密度满足国家标准测量精度±0.2‰的实验要求。 相似文献
11.
镁同位素地球化学研究新进展及其应用 总被引：7，自引：3，他引：4
作为一种新兴的地质示踪剂,Mg同位素正受到国际地学界日益广泛的关注。Mg同位素地球化学研究已取得了巨大的进展,近期研究工作主要包括两个方面。首先,调查了地球各主要储库和陨石的Mg同位素组成特征,结果表明陨石和地球地幔具有均一并且相似的Mg同位素组成,平均δ26Mg值分别为-0.28±0.06‰和-0.25±0.07‰;相反,上地壳和水圈的Mg同位素组成很不均一,δ26Mg值变化范围分别为-4.84‰~+0.92‰和-2.93‰~+1.13‰。其次,对一些地质和物理化学过程中Mg同位素的分馏行为进行研究,结果表明:(1)地表风化作用可以造成大的Mg同位素分馏,导致重Mg同位素残留在风化产物中而轻Mg同位素进入水圈;(2)岩浆分异过程中Mg同位素平衡分馏很小;(3)高温化学扩散和热扩散过程中Mg同位素会发生显著的动力学分馏。基于这些研究成果,Mg同位素体系已经被初步应用于示踪早期地球形成和壳内物质再循环等过程,并有望在不久的将来应用于示踪大陆地壳的化学演化和地质温度计等研究领域。 相似文献
12.
13.
Analyses of environmental isotopes (18O, 2H, and 87Sr/86Sr) are applied to groundwater studies with emphasis on saline groundwater in aquifers in the Keta Basin, Ghana. The 87Sr/86Sr ratios of groundwater and surface water of the Keta Basin primarily reflect the geology and the mineralogical composition
of the formations in the catchments and recharge areas. The isotopic compositions of 18O and 2H of deep groundwater have small variations and plot close to the global meteoric water line. Shallow groundwater and surface
water have considerably larger variations in isotopic compositions, which reflect evaporation and preservation of seasonal
fluctuations. A significant excess of chloride in shallow groundwater in comparison to the calculated evaporation loss is
the result of a combination of evaporation and marine sources. Groundwaters from deep wells and dug wells in near-coastal
aquifers are characterized by relatively high chloride contents, and the significance of marine influence is evidenced by
well-defined mixing lines for strontium isotopes, and hydrogen and oxygen stable isotopes, with isotopic compositions of seawater
as one end member. The results derived from environmental isotopes in this study demonstrate that a multi-isotope approach
is a useful tool to identify the origin and sources of saline groundwater.
Electronic Publication 相似文献
14.
锑被广泛用于生产各种阻燃剂、玻璃、橡胶、颜料、陶瓷、半导体原件等。锑在火成岩中属于分散元素,但可以富集在沉积岩中（如深海黏土、页岩及碎屑岩）。锑常出现在与辉长质深成岩有关的岩浆硫化物矿床、与花岗岩有关的硫化物矿床、碎屑岩-碳酸岩赋矿的钨-锑-汞层控矿床及热液铅锌矿床中。目前高精度锑同位素的分析测试方法已基本成熟,即酸溶、阳离子树脂交换柱结合硫醇棉纤维法或阴阳离子交换柱法分离富集锑、氢化物发生器MC-ICP-MS测定锑同位素。仪器的质量歧视校正通常采用标样-样品匹配法、In内标法和Sn内标法。不同地质储库端元的锑同位素组成变化较大（达18‱）,海水为～3.7‱,硅酸岩为0.9‱～2.9‱,硫化物（辉锑矿、闪锌矿、黄铁矿、白铁矿）为-1.9‱～16.9‱。且来自不同国家的辉锑矿具有不同的锑同位素组成,不同产地玻璃的锑同位素组成也不同。锑同位素在氧化还原过程（或硫化物沉淀）和无机吸附过程会发生明显分馏,分别达～9‱和～4‱。因此,锑同位素有可能作为一种灵敏的地球化学示踪剂,对示踪成矿物质来源、刻画与氧化还原等过程有关的成矿过程和探讨矿床形成机理、矿区重金属锑污染的治理以及考古等方面具有重要指示作用。 相似文献
15.
Steven J. Skotnicki Andrew C. Hill Malcolm Walter Richard Jenkins 《Precambrian Research》2008,165(3-4):243-259
Detailed mapping and C and O stable isotopic data from sedimentary carbonate in units both above and below the paleo-erosion surface on the Bitter Springs Formation (BSF) in the northeastern Amadeus Basin, Australia, have clarified the stratigraphy of the area. Isotopic data indicate that the top of the Loves Creek Member of the Bitter Springs Formation is preserved near Corroboree Rock, and is overlain by fenestrate-carbonate-clast breccia, and dolomitic quartz sandstone and chert-pebble conglomerate of the Pioneer Sandstone. The isotopic data, as well as lithologic data, indicate the presence of a 1–2 m-thick cap carbonate preserved between Corroboree Rock and areas 10 km to the northeast. In many places the cap carbonate layer is mostly a syn-sedimentary dolomite-clast breccia, consistent with deposition and disturbance in shallow water. C and O isotopic data also indicate that thin-bedded sandstone and dolomite above the Bitter Springs Formation at Ellery Creek, and a newly discovered massive chert-bearing dolomite at Ross River could both belong to the glaciogenic Olympic Formation. Detailed mapping also provides a more detailed context for the famous black chert microfossil locality in the Bitter Springs Formation at Ross River. 相似文献
16.
Prosenjit Ghosh S. K. Bhattacharya Ashok Sahni R. K. Kar D. M. Mohabey K. Ambwani 《Cretaceous Research》2003,24(6):743-750
A single locality of the Late Cretaceous (Maastrichtian) Lameta Formation at Pisdura in Central India has yielded a large number of coprolites attributed to titanosaurian dinosaurs. Internally the coprolites are dark grey and contain abundant plant tissues and other organic materials. The plant tissues are mostly of gymnospermous origin. In addition, remains of bacterial colonies, fungal spores and algae are seen in the macerated fraction under scanning electron microscope. The dark grey appearance is probably attributable to fine-grained organic matter within voids in tracheids or xylem. The average 13C/12C ratio of the organic matter in the coprolites is -24‰ (relative to PDB) suggesting that plants of C3type were the main diet of their producers. A comparison of δ15N value (about 4‰ w.r.t. air) of the coprolites with that of faecal matter of modern herbivores and carnivores suggests that gut fermentation may not have been an active mechanism in the digestion process of titanosaurs. 相似文献
17.
Cadmium (Cd) is a scarce, but not an extremely rare element in the Earth’s crust (crustal average: 0.2 ppm Cd). Geochemically, Cd exhibits thiophile, lithophile, and volatile behavior in different geologic processes. Biologically, it is a nutrient-like element that is closely related to P and Zn and is toxic element to organisms. Presently, Cd isotopes have been successfully utilized to trace Cd sources and nutrient cycling in marine systems in addition to unearthing other geochemical processes. Using published studies and our recent work, this survey summarizes the chemical preparation and mass spectrometry of Cd isotopes. It also reviews Cd isotopic compositions and fractionation mechanisms in nature as well as experiments. 相似文献
18.
The role of volatiles in the stabilization of the lower (granulite facies) crust is contentious. Opposing models invoke infiltration of CO2-rich fluids or generally vapour-absent conditions during granulite facies metamorphism. Stable isotope and petrological studies of granulite facies metacarbonates can provide constraints on these models. In this study data are presented from metre-scale forsteritic marble boudins within Archaean intermediate to felsic orthogneisses from the Rauer Group, East Antarctica. Forsteritic marble layers and associated calcsilicates preserve a range of 13C- and 18O-depleted calcite isotope values (δ13C= -9.9 to -3.0% PDB, δ18O = 4.0 to 12.1% SMOW). A coupled trend of 13C and 18O depletion (～2%, ～5%, respectively) from core to rim across one marble layer is inconsistent with pervasive CO2 infiltration during granulite facies metamorphism, but does indicate localized fluid-rock interaction. At another locality, more pervasive fluid infiltration has resulted in calcite having uniformly low, carbonatite-like δ18O and δ13C values. A favoured mechanism for the low δ18O and δ13C values of the marbles is infiltration by fluids that were derived from, or equilibrated with, a magmatic source. It is likely that this fluid-rock interaction occurred prior to high-grade metamorphism; other fluid-rock histories are not, however, ruled out by the available data. Coupled trends of 13C and 18O depletion are modified to even lower values by the superposed development of small-scale metasomatic reaction zones between marbles and internally folded mafic (?) interlayers. The timing of development of these layers is uncertain, but may be related to Archaean high-temperature (>1000d?C) granulite facies metamorphism. 相似文献
19.
Three types of groundwater occur in the area of the Ranger mine. Type A groundwater occurs in the loose sands and gravels occupying the present day stream channels, Type B in the weathering profile and Type C occurs in relatively fresh fractured bedrock occupying open fractures and other cavities. The three types of groundwater can be distinguished both chemically and isotopically. Light stable isotope data suggest that most early rains are lost by evapotranspiration and have no imprint on the groundwater. Later in the wet season, the ground is saturated and groundwater recharge occurs on a regional scale. This younger groundwater sits on the older waters. Mixing is probably minimal as before any large scale mixing could occur, most younger waters are lost by evapotranspiration. Stable isotope data suggest that Type B groundwater in certain areas has some connection with evaporated surface water bodies. Stable isotope measurements for the pollution monitoring bores around the tailings dam do not indicate any connection with the polluted pond waters at the time of sample collection. 相似文献