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1.
激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)作为一项实用的技术被广泛应用于原位微区分析。在学者们更为关注的元素空间分布问题上,LA-ICP-MS线扫描较单点剥蚀具有更大的优势。线扫描过程中元素的空间分辨率是影响分析结果准确程度的因素之一。每个脉冲间的信号如果严重叠加会导致较低的空间分辨率。文章通过LA-ICP-MS的单脉冲剥蚀实验,研究了合成硅酸盐玻璃标准样品CGSG中不同元素的信号时间结构,及其对线扫描的空间分辨率的影响。结果表明,当激光束斑40 μm时,应用LA-ICP-MS进行线扫描测量空间分辨率能够满足线扫描技术分析的需求。 相似文献
2.
This paper illustrates that sample size cannot be reduced below a theoretical limit and still achieve the highest precision obtainable on modern mass spectrometers. Reproducibility at the few ppm level is achievable and is related essentially to ion counting statistics. The number of atoms necessary to carry out such measurements is related directly to the sensitivity of the instrumentation. As most of the elements of interest are not major constituents of natural silicates, a lower limit to the size of the starting sample is assessed. Even for a number of elements for which very high ion per atom yields are attained by TIMS, minimum sample mass is an important limiting factor for precious or rare samples and may reduce the scientific output of experiments or place a major constraint on the sampling strategy itself. For rare meteorites or individual Martian samples expected to be returned in amounts at the gramme scale for rocks or at the microgramme scale for dust, the high sensitivity of TIMS is a requirement. Nevertheless, a compromise has to be found between sample consumption and the minimal desirable precision for a useful isotopic measurement. 相似文献
3.
加速器质谱(AMS)是一门发展非常迅速的核分析技术,诞生于20世纪70年代末,是基于加速器和离子探测器的一种高能质谱,它克服了传统质谱存在的分子本底和同量异位素本底干扰的限制,对同位素丰度灵敏度的测量可以达到10-16。经过的30多年发展,AMS以其多方的优势,日益受到人们的重视与青睐。在地学领域,通过测26Al、10Be等核素,可以实现地表暴露年龄、侵蚀速率测定和地貌演变研究;在海洋学领域,通过测量129I、10Be等核素,可以研究海洋沉积物、锰结核、锰结壳等生长速率和沉积速率;在考古学领域,通过测量14C、10Be等核素,可以实现珍贵样品的年代测定和第四纪人类进化的年代学研究;在环境科学领域,通过测量129I、14C等核素,可以对核污染、城市环境污染、全球气候变化进行监测与研究。目前,AMS从技术和应用研究两个方面都在迅速发展。文章对AMS的工作原理、设备和技术发展,以及在地学、海洋科学、考古学、环境科学等领域的应用进行详细阐述。 相似文献
4.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) has recently emerged as a powerful in situ microanalytical technique for major to trace elements in heterogeneous samples such as fluid and melt inclusions. Here, a rigorous comparison of melt inclusion (MI) data acquired by electron microprobe (EMP), ion microprobe (the secondary ion mass spectrometry, SIMS) and LA-ICPMS is used to evaluate the applicability and advantages/drawbacks of these approaches. We are specifically interested in determining if LA-ICPMS data on entire, unexposed, crystallized MI that cannot be homogenized in the lab are accurate and of a useful precision. Quantification of LA-ICPMS MI signals requires the use of an internal standard, i.e., the concentration of one element, or an element ratio, at the time of MI entrapment must be known independently, in order to derive the pure MI composition from the MI plus host mixed signal. Analysis of plagioclase-hosted glassy MI of a mid-ocean ridge basalt (MORB) sample from the East Pacific Rise illustrates that melt inclusion chemistry can be accurately quantified by LA-ICPMS, including the correction for postentrapment sidewall crystallisation of the host mineral without prior reheating in the lab. The LA-ICPMS data obtained on crystallized MI demonstrate agreement with the EMP and SIMS data on exposed glassy MI at the 1 standard deviation uncertainty level except for a few elements close to their limits of detection. LA-ICPMS data reduction schemes include the quantification of analytical uncertainty on each element of single MI. Therefore, weighted average element concentrations can be obtained for MI assemblages, at precisions that compare well with those of average element concentrations obtained by EMP and SIMS. Simple sample preparation minimizing inclusion loss through polishing combined with the analytical efficiency of 50 inclusions plus neighbouring host mineral at up to 40 elements per day enable the collection of statistically relevant datasets by LA-ICPMS. These allow to recognize nonrepresentative MI (e.g., heterogeneous entrapment). Application to individual clinopyroxene crystals from the AD79 pumice horizon of Mt. Somma-Vesuvius reveals chemical variability that exceeds the analytical precision on single melt inclusions. This variability was not obvious from the limited data set obtained by SIMS and EMP. The largest source of nonquantifiable error for EMP and SIMS data stems from the requirement of reheating the melt inclusions in the lab in order to reverse postentrapment crystallisation onto inclusion walls or growth of crystallites. For LA-ICPMS analysis of unexposed MI, the reliability with which the internal standard (IS) element concentration is known determines the quality of the data. LA-ICPMS, however, cannot analyse H2O, F, S and Cl reliably, has higher limits of detection (LODs) than SIMS for some elements for MI below 25 μm, has lower spatial resolution than both EMP and SIMS and consumes much more sample per analysis. Therefore, EMP, SIMS and LA-ICPMS are complementary in MI research, and the type of application will determine the analytical method or methods of choice. 相似文献
5.
采用双带测量方式,法拉第杯和离子计数器同时接收与跳峰接收相结合,建立了超微量钐同位素的热表面电离质谱的测量方法。优化了制样程序和质谱测量程序,研究了蒸发带电流对离子流强度的影响,考察了从纳克至微克不同样品用量的测量效果及其中Nd、Eu干扰核素的情况。对4 ng~2μg的天然丰度钐样品进行了同位素比值分析,相对标准偏差均小于1.1%。 相似文献
6.
13C solid-phase NMR and pyrolysis-chemical ionization mass spectrometry were used to characterize adsorbed organic material isolated on an XAD-2 macroreticular resin. Pyrolysis-chemical ionization mass spectrometry was used directly to fingerprint the organics sorbed to a titanium foil exposed in the same marine environment. The XAD-2 isolate was shown to be fractionated relative to the native material and contaminated with the isolation resin. 相似文献
7.
用甲醇-水-乙酸(体积比49∶49∶2)混合溶液作为喷雾溶剂,在优化实验条件下,将电喷雾解吸电离质谱(DESI-MS)用于各种质地纺织品中24种致癌性芳香胺的非破坏性快速检测,均获得满意结果。分析实际样品时,由于该方法无需样品预处理,单个样品单一指标的检测不到30 s,大大节省了分析时间,提高了分析效率。同时借助串联质谱的特异性,能够有效地避免实验结果的假阳性。方法对大部分芳香胺具有较高的灵敏度,二级质谱中特征离子的检出限一般为10-9g/kg。建立的方法能灵敏、快速、无损检测纺织品中的致癌芳香胺,精密度较好,对同一样品10次测量结果的相对标准偏差为5%~10%。 相似文献
8.
建立电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中铌、钽、锆、铪四种元素的分析方法。将样品与氢氧化钠、过氧化钠混合物放入高温炉中,熔融分解完全,用热水提取,过滤后弃去滤液,将滤纸及沉淀用酒石酸-盐酸溶液溶解,稀释至刻度测定。方法检出限(3s)为:LD(Nb)=0.08μg/g,LD(Ta)=0.04μg/g,LD(Zr)=0.5μg/g,LD(Hf)=0.04μg/g,精密度(RSD%,n=6)为:0.84%~4.21%。该测定方法具有灵敏度高、精密度好、分析速度快、线性范围宽、操作性强等优势。采用该方法对国家一级标准物质进行测定表明,其结果与标准值吻合。此方法已在实际地质调查样品分析中得到应用。 相似文献
9.
采用超声波清洗及离子交换分离等技术，对新疆青铜时代古人类骨骼中样品进行预处理及分离，该方法制备的同位素锶样品，保证了样品在前处理过程中不受处外界物质的污染，并提取纯度高的锶用于质谱测试。 相似文献
10.
The Cr isotope ratios of terrestrial and extra-terrestrial materials are emerging as one of the most important tracers in geosciences. Previous studies on Cr isotopic measurements using TIMS have found that there is residual Cr isotopic fractionation between the mass-fractionation-corrected 53Cr/ 52Cr and 54Cr/ 52Cr ratios, which may cause an offset of obtained ratios from the reference values. The residual fractionation was thought to be caused by the evaporation of Cr-oxide species during thermal ionisation, but the mechanism by which this residual fractionation could be reduced remained unclear. Here we revisit the issue of residual fractionation and propose that this problem can be alleviated by utilising W filaments instead of conventionally used Re filaments for Cr ionisation. Using W filaments, the formation of CrO + was suppressed during heating as the filament temperature was ~ 100 °C lower than when Re filaments were used. In repeated measurement of a carbonaceous chondrite, the intermediate precisions of 53Cr/ 52Cr and 54Cr/ 52Cr ratios in the W filament runs were two to three times better than those of the Re filament runs. Therefore, the new finding of this study will be of key importance for future studies of Cr isotopes for terrestrial and extra-terrestrial materials. 相似文献
11.
将掺钕的钇铝榴石（Ｎｄ：ＹＡＧ）激光器与高精密ＭＭ１２００质谱计、电子倍增器联网，应用连续激光质谱对单颗粒矿物、光片样品进行微区４０Ａｒ／３９Ａｒ测年、坪年龄和等时线年龄研究。在光片上测定南极乔治王岛北海岸玄武岩等时线年龄（５２．３８±１．０５）Ｍａ和贵州绿豆岩年龄（２３９．１６±１４．１３）Ｍａ，两者与实际地质背景吻合。对两个中生代和太古代单颗粒黑云母进行连续激光质谱阶段升温４０Ａｒ／３９Ａｒ坪年龄谱测定，获得与常规法相一致的坪年龄谱 相似文献
12.
对某地下工程围岩进行声波测试,利用FFT方法进行信号的频谱分析,得到围岩声波的频谱特性。结果表明,声波传播过程中携带了反映岩体固有特性的信息,声波的频谱在一定程度上反映了岩体的结构、构造、完整性等特征;完整岩石的声波频谱以高频为主,裂隙岩体的声波频谱以低频为主;比较岩石与岩体声波测试的频谱差异,可对岩体质量的好坏进行判断。 相似文献
13.
本文采用电感耦合等离子体质谱法,对地质样品中的碲的测定进行了研究,建立了一种快速、准确、简便的测定土壤样品中碲的方法。该方法克服了常规方法的局限性。此方法对6个国家标准物质进行了方法验证,12次测定精密度、准确度均符合标准要求。 相似文献
14.
反射光谱法是一种古老的实验方法，具有快速简便、无损伤等特点。但是，这种实验技术至今还未得到充分的开发应用。本文介绍矿物的红外反射光谱的实验方法、光谱特征及应用前景。 相似文献
15.
为了提高激光解吸飞行时间质谱仪的分辨率,在自行研制的激光解吸飞行时间质谱仪上进行了离子延时引出新技术的探讨与实验,比较了不同的脉冲引出方式,在线性方式下得到了分辨率超过１０００的质谱图。 相似文献
16.
本文以敞开式四酸溶样,电感耦合等离子体质谱测定了新疆、青海区调样品中的Co、Mo、W、Pb等元素,并把ICP-MS、ICP-AES和XRF三个大型仪器对新疆卡克-色帕巴衣地区样品的测定结果进行了比较,确定了区调样品元素分析方法的配套方案,并对溶样过程进行了一系列的优化,其方法检出限和精密度均符合DZ0130.4-2006及补充说明中1﹕5万化探样品标准要求。经国家标准物质验证,结果与标准值相符。优化的分析方法快速灵敏度高,能用于地球化学填图计划中分析测试任务, 同时也用于日常大规模多元素分析。 相似文献
17.
An analytical system and operating protocol are described for high resolution, stepped-combustion mass spectrometry, designed for the extraction, purification, quantification and isotopic analysis of light elements (e.g. C and N) in fine-grained reduced components (e.g. diamond) which have been chemically extracted from natural samples (e.g. meteorites). Specifically, a simple model has been developed for the extraction of diamond from meteorite and its analysis by high resolution stepped heating under an atmosphere of oxygen. Changes in the pressure of oxygen within the range 1.3 to 12kPa (10 to 90 torr) were not found to have any detectable effect on the combustion. Results obtained by this procedure were compared with those predicted by a model and excellent agreement was found, taking into account the limitations of this approach. Results of a preliminary attempt to find fine-grained diamond in a lamproite are outlined. 相似文献
18.
铅笔芯内所含石墨和黏土的混合比例如果不符合国家标准,将不利于计算机读卡设备正确识读和非专业人士鉴定.本文采用常压质谱法对不同黑度(石墨含量)、硬度的铅笔芯进行分析,为实现铅笔品质的快速鉴别提供了一种有效的技术手段.该方法直接将铅笔芯作为电离装置,在高电压作用下以空气(相对湿度40％)为介质,铅笔芯产生电晕放电,其放电行为能够对质谱信号产生直接影响.实验优化了工作条件,分析了6种型号铅笔芯(4B、3B、2B、HB、H和2H)中石墨含量与其质谱信号之间的关系,并结合主成分分析(PCA)对不同型号铅笔芯进行区分.结果表明,不同型号铅笔芯的放电行为对质谱信号产生较大影响,质谱信号随铅笔芯中石墨含量的增多而增强;6种型号铅笔芯区分正确率高达99％以上.此方法操作简单且可重复性强,可用于市场上不同品质铅笔芯的快速鉴定. 相似文献
19.
The GENESIS space mission recovered ions emitted by the Sun during a 27 month period. In order to extract, purify and determine the very low quantities of solar nitrogen implanted in the GENESIS targets, a new installation was developed and constructed at the CRPG (Nancy, France). It permitted the simultaneous determination of nitrogen and noble gases extracted from the target by laser ablation. The extraction procedure used a 193 nm excimer laser that allowed for surface contamination in the outer 5 nm to be removed, followed by a step that removed 50 nm of the target material, extracting the solar nitrogen and noble gases implanted in the target. Following purification using Ti and Zr getters for noble gases and a Cu-CuO oxidation cycle for N 2, the extracted gases were analysed by static mode (pumps closed) mass spectrometry using electron multiplier and Faraday cup detectors. The nitrogen blanks from the purification section and the static line (30 minutes) were only 0.46 picomole and 0.47 picomole, respectively. 相似文献
20.
随着农业集约化和城市化的推进,世界上大量水环境中农药残留量已超过规定的限值,水环境中农药污染问题受到社会各界的广泛关注。作为世界上最大的农药生产国和使用国,中国水环境中农药残留量远高于其他发达国家,已有研究表明在我国七个典型流域(长江、太湖、黄河、松花江、黑龙江、大运河和东江)中检测到19种农药,平均浓度范围为0.02～332.75ng/L。农药及其转化产物对生态环境和人体健康具有潜在威胁,水环境中农药残留的研究是水质评估中必不可少的组成部分,而靶向筛查难以检测未知农药及其转化产物。因此,环境中农药残留及其转化产物的非靶向筛查亟需完善。本文依据农药组分非靶向筛查的分析流程,对近五年水质样品中农药残留靶向及非靶向筛查方法进行综述,梳理了近年来国内外食品与水环境中农药残留限量的相关法律法规,对水环境中农药残留分析方法的研究进展进行概述;总结了液液萃取(LLE)、固相萃取(SPE)、固相微萃取(SPME)等样品前处理方法的特点,在这些方法中,固相萃取是农药非靶向筛查的主要前处理方法,具有良好应用前景。本文还探讨了分析仪器从色谱检测到色谱-质谱联用的发展趋势,多种高分辨率质谱的产生为农药非靶向筛查提供了多层次的分析需求;同时通过总结近年来农药筛查确证相关的指导标准、质谱数据库与多种鉴定方法,指出水环境中农药污染分析技术的发展趋势。 相似文献
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