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1.
主要针对宝石材料进行了激光诱导离解光谱技术定量分析方法的总结以及对比研究。选择外标法、自由定标法和归一化的外标法三种较为适用于宝石材料分析的方法进行了介绍。选取陨石玻璃、绿辉石、紫色翡翠以及硅酸盐玻璃等成分较为均匀的样品作为分析对象,使用中国地质大学(武汉)珠宝学院自制的激光诱导离解光谱设备,分别运用三种方法对其进行了定量分析的计算。定量分析结果显示,外标法易受成分变化及结构差异而造成的基体效应的影响,分析的准确度不高;自由定标法在分析成分复杂的样品时,其影响因素十分复杂,会产生较大的误差;归一化的外标法可有效校正基体效应的影响,其定量分析结果要优于前两者,虽然在微量元素分析准确度上尚需改进,但不失为一种较好的快速定量分析宝石材料的定量分析方法。  相似文献   

2.
利用激光诱导离解光谱检测铍铝元素区分透闪石白玉产地   总被引:2,自引:1,他引:1  
涂彩  袁心强  周钊 《岩矿测试》2012,31(2):301-305
利用自行搭建的激光诱导离解光谱仪分析54块新疆、青海、俄罗斯产地的透闪石白玉样品,提出通过检测Be、Al元素来区分白玉产地的方法。使用波长1064 nm的激光器激发样品,4CCD光谱仪采集光谱,为避免外界条件干扰,以透闪石白玉中含量比较固定的Si元素作为内标元素测量原子谱线强度比值IBe/ISi、IAl/ISi,分别代表Be、Al元素的含量变化,重复测量10次的相对标准偏差(RSD)<3%。结果表明,新疆白玉的IBe/ISi为0.3~0.6,IAl/ISi为0.1~0.4;青海白玉IBe/ISi<0.1,IAl/ISi<0.2,显示出低Be低Al的明显特征;俄罗斯白玉的IBe/ISi分为高值和低值两个区域,部分样品的IBe/ISi>0.7,指示Be的含量较高,另一部分样品的IBe/ISi为0.1~0.5,略低于新疆白玉。研究显示Be、Al元素特别是Be元素具有较好的产地指示意义,激光诱导离解光谱技术用于鉴别白玉产地有着较好的推广前景。  相似文献   

3.
吉林蛇纹石玉特征初步研究   总被引:1,自引:0,他引:1  
对产自吉林省白山市抚松县沿江乡的蛇纹石玉样品分别从地质背景、激光诱导离解光谱、X射线粉末衍射和红外吸收光谱等方面进行了研究,并与辽宁岫玉样品进行了对比。结果表明,吉林蛇纹石玉样品的主要颜色为深浅不一的绿色,主要含Si,Al,Cr,Fe,Mn,Mg,Ca,Sr和Na等元素,其中Ca与Mg的谱线较强,Al,Mn与Sr的质量分数少;X射线粉末衍射结果显示,样品的主要矿物组成为纤蛇纹石,红外光谱结果也显示了其具有纤蛇纹石峰值的特征。  相似文献   

4.
实验在德国耶拿分析仪器股份公司的Contr AA连续光源原子吸收光谱仪上进行,仪器配有SFS 6分段流动注射和AS 52 s自动进样器,测定饮用水中的钠、钾、锂。为了在检出限和检测限附近低浓度范围进行校准,样品需用自动进样器进行自动稀释,并在测定时加入0.1%(质量分数)的CsC l/LaC l3和1.5%(体积分数)的HC l。待分析样品可以直接进行测定。1仪器工作条件设定Contr AA原子吸收光谱仪的工作条件见表1,元素测量条件见表2。表1仪器工作条件元素波长λ/nm火焰类型燃气流量(L/h)燃气/助燃气比燃烧头宽度(mm)燃烧头角度θ/(°)燃烧头高度(mm)Na 588.995 C2  相似文献   

5.
利用常规宝石学测试、X射线荧光光谱仪(XRF)、激光诱导离解光谱仪(LIBS)、电子探针(EPMA)对近来在珠宝市场上的铅玻璃充填碧玺样品进行测试与分析,旨在探讨其鉴定特征。结果表明,该铅玻璃充填样品的充填特征不明显,与传统的有机物充填处理方法不同;X射线荧光光谱和激光诱导离解光谱的测试结果显示,该铅玻璃充填碧玺样品具有明显的Pb峰。铅玻璃充填碧玺样品中充填物的电子探针二次电子像及背散射电子像特征,可作为碧玺样品是否经过了铅玻璃充填的诊断性依据,其充填物的化学成分主要为Si和Pb,呈不规则斑块状分布于裂隙中。  相似文献   

6.
连续光源原子吸收光谱法测定土壤水溶性盐中钙镁   总被引:2,自引:1,他引:1  
使用连续光源原子吸收光谱仪在不更换元素灯情况下,一次进样测定土壤水溶盐组成中钙、镁离子含量,测定值与标准值的相对偏差小于5%,测定速度显著提高。连续光源原子吸收光谱法可选择元素任一谱线测定,对比30个土壤样品Mg次灵敏线202 nm与主灵敏线285 nm两条谱线测定结果,两者基本一致。高浓度时Mg次灵敏线202 nm的标准曲线相关性好于主灵敏线285 nm。与传统线光源原子吸收光谱仪相比,连续光源原子吸收光谱仪测试灵敏度显著提高。  相似文献   

7.
单个流体包裹体LA-ICPMS定量分析技术及其应用(英文)   总被引:7,自引:0,他引:7  
ThomasULRICH 《地学前缘》2003,10(2):379-393
对于不同类型的地球化学勘查样品 ,运用恰当的分析方法处理 ,是成功地发现矿床的关键。激光熔融电感耦合等离子质谱分析 ,即LA ICPMS ,是功能最强的多元素分析技术之一。该方法获得数据快捷 ,样品制备简单 ,其高灵敏度为很多主元素和微量元素 (包括铂族元素、稀土元素、高场强元素和多种成矿示踪元素 )提供了低检测限 ,正在并将要持续为地球化学应用提供新的信息。仪器由ICPMS(四极 ,多接受或磁扇域 )附加激光器 (紫外或红外波长 )而构成。应用于地球科学研究的标准仪器的激光器为具有 2 6 6nm四倍频率的Nd :YAG激光器 ,或者是具有 193nm波长的ArF激态原子激光器。激光器熔融样品 ,并通过运载气体将熔融的样品物质传送到IP ,而不是将样品溶解后 ,通过雾化器和雾化室将样品传输给ICP。这就使我们能够进行微区分析 ,如矿物环带 ,或者矿物中的微小矿物、融体和流体包裹体等。运用外标校对元素比值 ,并结合内标使用 ,可以获得定量测试结果。对于固体熔融物的分析精度一般为 2 %~ 5 %RSD(相对标准误差 ) ,对于流体包裹体则为 10 %~ 30 %RSD。LA ICPMS的一些复杂系统可能引起成分分馏和质量干扰。对于分馏效应 ,可以通过运用产生小粒子的短波长激光器和运用He作为运载气体来减小 ;对于质量干扰 ,则可以通过?  相似文献   

8.
HyMap-C机载高光谱仪能够在400~2 500 nm波长范围内获取144个精细光谱通道,对于地球表面地物特征有极强的探测能力。为保证高光谱遥感数据的可靠性与定量化分析的精度,作者分别采用单色准直光法、漫反射板定标法和内部参考标准法对HyMap-C机载高光谱仪进行了实验室光谱定标、绝对辐射定标以及飞行过程中航线上相对辐射定标。通过航空飞行测量与地面实际测量的光谱反射率数据进行对比验证,结果表明两者整体谱型与局部吸收特征非常一致,定标结果可靠,数据可信。文中阐述的定标原理与方法为我国自主研制机载高光谱仪的定标提供了依据与思路,定标后获取到的高光谱分辨率数据可广泛应用于地质调查领域特别是矿物填图中。  相似文献   

9.
本文以K2S2O7、NaF、Al2O3、NH4I和C粉做为缓冲剂,Ge元素做内标,试样与缓冲剂1∶1混合均匀后用杯状带颈碳电极直接双份装样。利用原子发射光谱法,采用交流电弧激发火焰光源对试样燃烧以摄取锡元素多条光谱线。使用新型全自动CCD测光系统,以Ge 270.963 nm为内标线,选择了波长分别为283.993 nm,285.079 nm和281.358 nm的三条不同灵敏度的Sn元素谱线,对矿石中中、低及微量锡元素进行了测试,解决了传统原子发射光谱法只能进行微量元素分析无法对中低含量准确测试的缺陷,也克服了化学仪器法流程复杂、干扰严重的不足。本法不需要对试样进行稀释,就能对未知含量范围的试样直接测试,有效拓宽了锡元素的测试范围:0.001×10-2~15.00×10-2,分析数据与参考值和原子荧光测试值相吻合。方法操作简便、快速,用于样品测试取得了满意的效果。  相似文献   

10.
锆石变生程度与放射性元素含量间的定量研究   总被引:1,自引:0,他引:1  
为获得锆石变生程度与放射性元素质量分数之间的相互关系,对来自山东蒙阴金伯利岩中的锆石进行了阴极发光、激光拉曼光谱、离子探针测试和研究.研究表明,锆石样品的年龄近于一致;按照拉曼光谱特征峰1000cm-1左右的强度/半高宽比值和放射元素质量分数(wB)可以将锆石分为全晶质锆石、弱变生锆石、变生锆石、强变生锆石4类.放射元素总质量分数(wB)与拉曼光谱特征峰1000cm-1左右的强度/半高宽比值(H/W,设为r)之间符合经验关系方程:(1/r)1/2=1.3×10-2·(wB/10-6)1/2—0.11,可以借助锆石在1000cm-1左右的拉曼光谱特征峰值强度/半高宽比值并采用这一经验关系方程来大致计算出拉曼测试位置的放射性元素的质量分数.  相似文献   

11.
For the trace element analysis of gold by laser ablation ICP-MS, external calibration samples of differing matrix composition have been used in previous studies. Data presented here suggest that even for calibration samples and unknowns with closely-matched matrices, discrepancies arise due to variations in the coupling behaviour of the laser with the sample at different power deliveries, and can lead to erroneous trace element determinations. Internal standardisation for gold is complicated because Au and Ag, the most common major elements, do not have minor isotopes that can be used as internal standards. This problem was overcome for natural gold samples by using an external calibration sample only for the major elements Au and Ag, then defocussing the ion path and using 107Ag in each sample as an internal standard against which μg g-1 levels of Te, Sb, Hg, Bi, and Cu were determined. The results suggest that trace elements can occupy lattice sites in gold rather than occurring only as micro-inclusions of other phases. The analytical approach taken here may be used in trace element analysis where adequate external calibration samples are not readily available.  相似文献   

12.
A new reference material, STDGL3, for the calibration of in situ analyses of sulfide minerals by LA-ICP-MS has been developed and characterised. It represents a lithium-borate-based glass containing a mixture of Zn- and Fe-sulfide concentrates doped with several chalcophile elements as well as Zr, Gd, Hf and Ta required for assessing common interferences on Ag, Au and Pt. STDGL3 has a wider range of elements and a better homogeneity compared with existing reference materials for LA-ICP-MS analysis of sulfides. Compositional variations for most elements are below 3% RSD, below 5% RSD for Ag, Au and Pt, and below 7% RSD for Se, when performing spot analyses with a 50 μm beam size. Its preparation recipe is reproducible allowing for multiple batches to be made. Use of STDGL3 significantly improves accuracy of sulfide mineral analysis by LA-ICP-MS when compared with use of other available reference materials. Performance of STDGL3 was evaluated using several different laser systems. No significant change was observed between 193 nm ArF excimer lasers with 5 and 20 ns pulse widths, but use of 213 and 248 nm lasers displays more systematic differences, especially when analysing galena. Correction coefficients are needed for some elements (Zn and Cd in particular) when analysing sulfide minerals using STDGL3 as a calibration reference material.  相似文献   

13.
等离子体质谱法直接测定地球化学样品中金铂钯   总被引:19,自引:0,他引:19  
建立了王水分解地球化学样品报直接用等离子体质谱法测定Au、Pd和Pt的分析方法。方法测定下限为Au4,0ng/g,Pd3.6ng/g,Pt2.4ng/g,方法精密度(RSD,n=12)为Au14.2%,Pd3.6%-5.2%,Pt6.6%-10.8%,三个元素的线性范围都为0.02-300μg/L。采用文中制定的分析方法直接测定了国家一级地球化学标准物质中的Au、Pd、Pt,在测定下限以上的测定结果与标准值吻合。  相似文献   

14.
石墨炉原子吸收法测定化探样品中的痕量金   总被引:2,自引:0,他引:2  
试样经灼烧、王水(1 1)分解后,置于10%±的王水介质中经泡塑富集,高温灰化,小体积王水浸取后,以N i作为A u的稳定改进剂,用石墨炉原子吸收法测定A u。本方法检出限为0.18ng/mL,相对标准偏差为3.98%~6.12%。适用于地质、化探样品中痕量金的测定。  相似文献   

15.
李勇 《岩矿测试》2008,27(4):305-309
用φ=50%的王水分解样品,聚氨酯泡沫塑料吸附富集金,10g/L硫脲为解脱剂,偏振塞曼石墨炉原子吸收分光光度计测定痕量金。对干燥、灰化、原子化、净化温度和时间,以及载气流量和灯电流强度进行了讨论;对影响金吸附效果的泡塑载体和王水浓度等因素进行了研究。通过实验得到了Z-2000偏振塞曼原子吸收分光光度计最佳石墨炉分析测试条件。方法检出限为0.3ng/g,回收率为95.0%~101.0%,精密度(RSD,n=12)低于8.0%,经国家一级标准物质(GBW07243~GBW07245)分析验证,结果与标准值相符。  相似文献   

16.
The Ahar area is located in NW Iran. The main part of the area is covered by Eocene andesitic and andesi‐basaltic rocks within which several granitoid intrusives of Oligocene age are emplaced. This caused vast hydrothermal alterations and Cu and Au mineralization. In this regard, this contribution aims to explore the distribution of gold across the region based on systematic sampling of stream sediments and using the secondary geochemical halos, as well as the bulk leach extractable gold (BLEG) method. Meanwhile, the results obtained from these two methods will be compared in order to find out if the anomalous zones match with each other. For this, 620 stream sediment samples of ?80 mesh grain size and 422 BLEG samples were collected and analyzed by Fire Assay and atomic absorption spectroscopy (AAS) methods, respectively. For BLEG samples, gold was first dissolved using KCN before being analyzed by the AAS method. Furthermore, 84 rock samples were also collected during the field control surveys and were analyzed by Fire Assay and ICP‐OES methods for gold and other elements, respectively. After determining the distribution characteristics and statistical parameters of gold in each group of samples, anomaly maps of gold for each method were prepared, revealing almost similar anomalous zones across the region. Based on these maps, most of the discovered anomalies correlate well with granitoid intrusives of Oligocene age and the related hydrothermal alterations, which have occurred within the intrusives and the host andesitic‐basaltic rocks of Eocene age, especially at the NE and central parts of the area and east of Ahar. Some silicic veins and veinlets have been observed during field surveys in these parts, within which high concentrations of Au and sometimes Cu are determined. Another anomalous zone is located over the hydrothermal alterations within trachy‐andesitic and andesitic volcanics of Pliocene age at the SE part of the quadrangle, where vast alterations caused by volcanic fumaroles and epithermal mineralization of gold and Pb–Zn is discovered. In this regard, the SE and NE parts of the area and the east Ahar area are proposed, in order of importance, for further detailed investigations.  相似文献   

17.
动力变形条件下Au迁移、富集的构造地球化学实验研究   总被引:2,自引:0,他引:2  
对海南二甲金矿和广东河台金矿形成的动力学条件进行了一系列的构造地球化学模拟实验。结果表明,动力变形中发生了明显的力学—化学耦合作用。云母矿物变形强烈,塑性变形,定向拉长显著。黑云母发生了褪色作用,从褐色变成浅褐色甚至无色;白云母干涉色从鲜艳的蓝色变为黄色,甚至无色。随试验温度、压力条件的升高,岩石、矿物从脆性变形向塑性变形演变。动力变形还使岩石和矿物中的元素呈现化学迁移和富集作用:云母矿物中的杂质容量降低,导致铁质释放;硫化物矿物的反射率增高,成矿元素特别是Au在其不同部位发生一定的变化。自然金颗粒在析出过程中,与Si、Fe分离而纯化。动力变形中成矿元素(特别是Au)的迁移、富集等效应是通过压溶作用实现。  相似文献   

18.
New glass reference materials GSA-1G, GSC-1G, GSD-1G and GSE-1G have been characterised using a prototype solid state laser ablation system capable of producing wavelengths of 193 nm, 213 nm and 266 nm. This system allowed comparison of the effects of different laser wavelengths under nearly identical ablation and ICP operating conditions. The wavelengths 213 nm and 266 nm were also used at higher energy densities to evaluate the influence of energy density on quantitative analysis. In addition, the glass reference materials were analysed using commercially available 266 nm Nd:YAG and 193 nm ArF excimer lasers. Laser ablation analysis was carried out using both single spot and scanning mode ablation. Using laser ablation ICP-MS, concentrations of fifty-eight elements were determined with external calibration to the NIST SRM 610 glass reference material. Instead of applying the more common internal standardisation procedure, the total concentration of all element oxide concentrations was normalised to 100%. Major element concentrations were compared with those determined by electron microprobe. In addition to NIST SRM 610 for external calibration, USGS BCR-2G was used as a more closely matrix-matched reference material in order to compare the effect of matrix-matched and non matrix-matched calibration on quantitative analysis. The results show that the various laser wavelengths and energy densities applied produced similar results, with the exception of scanning mode ablation at 266 nm without matrix-matched calibration where deviations up to 60% from the average were found. However, results acquired using a scanning mode with a matrix-matched calibration agreed with results obtained by spot analysis. The increased abundance of large particles produced when using a scanning ablation mode with NIST SRM 610, is responsible for elemental fractionation effects caused by incomplete vaporisation of large particles in the ICP.  相似文献   

19.
Data are reported for rare earth elements (REE) in three geological glass reference materials (BIR-1G, BHVO-2G and BCR-2G) using a UV (266 nm) laser ablation ICP-MS system and the classical (HF-HClO4) acid decomposition method, followed by conventional nebulisation ICP-MS. External calibration of laser ablation analyses was performed using NIST SRM reference materials with internal standardisation using 29Si and 44Ca. Replicate analyses of reference basaltic glasses yielded an analytical precision of 1-5% (RSD) for all the elements by solution ICP-MS and 1-8% (RSD) by laser ablation ICP-MS. The relative differences between the REE concentrations measured by solution and laser ablation ICP-MS compared with the reference values were generally less than 11 % for most elements. The largest deviations occurred for La determined by solution ICP-MS in BIR-1G. The results of both solution and laser ablation ICP-MS agreed well, generally better than 7%, with the exception of La, Pr and Sm in BIR-1G. The measured REE laser ablation data for BIR-1G, BHVO-2G and BCR-2G agreed with the previously published data on these basaltic reference glasses, within a range of 0-10% for most elements. No significant influences were observed for the predicted spectral interferences on some REE isotopes in the analysis of basaltic glasses.  相似文献   

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