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1.
Standard reference material and different geological samples were dissolved by system A （the mixture of nitric and perchloric acids） and system B （mixture of nitric, perchloric and hydrofluoric acids）, and total Se in all samples was measured by hydride-generation atomic fluorescence spectrometry （HG-AFS） after concentration with thiol cotton fiber （TCF）. The analytical results obtained by the two digestion method are in good agreement （within the limit of errors） for most of the samples, particularly for those having recommended values. The Se concentrations determined by the two methods are of no difference, and the correlation coefficient is 0.9986; the relative standard deviation （RSD） for the determination of 0.04 μg/g Se is 10.2%. The recovery rates of systems A and B by the standard-addition method were 96%-106% and 99%-104%, respectively.  相似文献   

2.
Lithium separation technique for three reference materials has been established together with precise determination of lithium isotope using a Neptune multi collector-inductively coupled plasma mass spectrometry (MC-ICP-MS). The solutions of lithium element standard reference materials, potassium, calcium, sodium, magnesium and iron single element, were used to evaluate analytical methods applied. Three separate stages of ion-exchange chromatography were carried out using organic cation-exchange resin (AG 50W-X8). Lithium was enriched for the three stages using different eluants, which are 2.8 M HCl, 0.15 M HCl and 0.5 M HCl in 30% ethanol, respectively. The columns for the first and second stages are made of polypropylene, and those for the third stage are made of quartz. Total reagent volume for the entire chemical process was 35 mL for three reference materials. The recovery yielded for the three stages is 98.9–101.2% with an average of 100.0%, 97.6–101.9% with an average of 99.9%, and 99.8–103.3% with an average of 100.6%, respectively. The precision of this technique is conservatively estimated to be ±0.72–1.04‰ (2σ population), which is similar to the precision obtained by different authors in different laboratories with MC-ICP-MS. The δ7Li values (7Li/6Li relative to the IRMM-016 standard) determined for andesite (AGV-2) and basalt (BHVO-2) are 5.68‰ (n=18), 4.33‰ (n=18), respectively. The δ7Li value (7Li/6Li relative to the L-SVEC standard) determined for IRMM-016 is –0.01‰ (n=15). All these analytical results are in good agreement with those previously reported. In addition, the results for the same kinds of samples analyzed at the MLR Key Laboratory of Metallogeny and Mineral Assessment, Institute of Mineral Resources, Chinese Academy of Geological Sciences, are consistent with those obtained at the Plasma Laboratory, University of Maryland, within analytical uncertainty. According to these experiment results, it is concluded that this proposed procedure is a suitable method for determining the lithium isotopic composition of natural samples.  相似文献   

3.
In the Triassic marine sediments, an obvious enrichment of lithium has been found. The source and enrichment mechanism of lithium is unknown. Here, we report trace and rare earth element and isotope analyses for Triassic sedimentary samples from core ZK601, recovered from the Huangjinkou anticline in the Xuanhan basin. Lithium concentrations from the Leikoupo and Jialingjiang formations are much higher than the average concentrations in the crust of eastern China and in other marine sediments. Lithium concentrations are highest at depths of 3300–3360 m (in argillaceous marine sediments), and Li is positively correlated with Rb, Ga, Zr, Nb and other trace elements. The range of δ7Li values in our samples is consistent with that in other Triassic marine carbonate rocks. Lithium concentrations and isotope ratios are negatively correlated in the argillaceous dolomite samples at depths of 3300–3360 m. We compared the results in this study with trace and rare earth elements in the clay from Sichuan and Chongqing, and propose that the clay in the argillaceous marine evaporites from Huangjinkou formed via the hydrolysis of volcanic ash during Early–Middle Triassic volcanic eruptions into brine basins, during which clay adsorbed Li from the brine and formed Li-rich argillaceous dolomites. The addition and hydrolysis of volcanic ash in the evaporative brine is also related to the formation of a new type of polyhalite.  相似文献   

4.
In this study, the δ^13C and δ^18O values were systematically measured on NBS-18, NBS-19 and IAEA-CO-1 with different sample sizes, with the objective to examine the stability and reproducibility of previously developed linearity correction strategy especially for small-sized samples （e.g. 〈50 μg）. Firstly, the δ^13C and δ^18O values of NBS-19 standards （6-10 samples per run） with sample sizes scattered below -100 μg were determined in three different runs. The logarithmic regressions were performed on the plots of δ-values vs. peak area （sample size） for each run and the correction was applied using peak area of the first peak. Results show that two of the three data sets have almost the same regressive equations for both δ^13C and δ^18O values. The maximum difference in δ^13C values calculated by three equations when sample size varies between -10 and -100 μg is better than 0.15‰, compared with the maximum 0.82‰ for δ^18O values. Since alteration of phosphoric acids could not influence carbon isotope, the 〈0.15‰ difference in calculated δ^13C values should reflect the stability of mass spectrometer conditions. In contrast, the large difference in regressive equations for δ^18O values may be attributed to changed oxygen isotope in phosphoric acids due to exchange with atmosphere through time. It means that standards with sample sizes properly distributed should be arranged in every run for subsequent linearity correction of δ^18O values of small-sized samples （e.g. marine ostracode）.  相似文献   

5.
Total 138 coal samples and 14 parting samples were taken from the No. 6 Seam of the Jungar Coalfield, Inner Mongolia. These samples were analysed by optical microscopy, sequential chemical extraction procedure (SCEP), inductively coupled plasma mass spectrometry (ICP-MS), X-ray powder diffraction (XRD), and scanning electron microscope in conjunction with an energy-dispersive X-ray spectrometer (SEM-EDX) analysis. The results indicate that the Li contents have reached the industrial grade of the coal associated Li deposit, and the total Li reserves have reached 2406600 tons, that is, 5157000 tons Li2O in the No. 6 seam in the Jungar Coalfield. The sequential chemical extraction procedure results suggest that the Li concentration is mainly related to inorganic matter. The minerals in the coals consist of kaolinite, boehmite, chlorite-group mineral, quartz, calcite, pyrite, siderite and amorphous clay material. Some Li could be absorbed by clay minerals in the Li-bearing coal seam. The chlorite phase?could be?most likely the host for a part of Li. The Yinshan Oldland should be the most possible source of Li of the coal.  相似文献   

6.
The rare-earth elements （REEs） are a series of elements including lanthanides with atomic numbers from 57 to 71, as well as Y with an atomic number of 39. The REEs are commonly used as geochemical tracers in the study of many geologic processes because of their unique and chemically coherent behavior. The main purpose of this research is to understand the effect of water-particle interaction on trace metal transport, the distribution and chemical species of the REEs in water through case studies on geochemical behavior of the REEs in the Chaohu and Longgan lakes, eastern China. Concentrations of the dissolved REEs were detected by ICP-MS （Inductively Coupled Plasma-Mass Spectrometry）. Before ICP-MS measurement, REEs were concentrated from water samples by using solvent extraction and back extraction with a mixture 65% HDEHP （2-etheylhexyl hydrogen phosphate） and 35% H2MEHP （2-ehtylhexyl dihydrogen phosphate）. The results showed that the average concentrations of dissolved REEs in summer are higher than in winter for Chaohu Lake： they were 162.6 ng/kg and 86.5 ng/kg, respectively. On the country, the REE contents of winter samples were higher than those of summer water samples for Longganhu Lake： they were 111.1 ng/kg and 44.0 ng/kg, respectively. The contents of suspended particulate matter and pH are the two important factors controlling the concentrations of dissolved REE in the lakes. The contents of the REEs decrease with increasing pH in the Longgan and Chaohu lakes. The suspended particulate matter shows different sorption/desorption toward the dissolved REEs in the two water bodies. Most lake water samples have a fiat NASC-normalized REE pattern, and the others have heavy REE-enrichment patterns relative to NASC, which may imply that the dissolved REEs were mainly present in the form of fine colloids in the Chaohu and Longgan lakes.  相似文献   

7.
A new aproach to isotopic analysis of carbon,oxygen,sulfur and nitrogen in microsamples has been established.Samples were conventionally prepared by mixing microsamples to be analyzed with reference samples with known δ values in a proper proportion,and then analyzed for their stable isotopes as those at ordinary levels.According to the equilibrium relationships before and after mixing,the δvalues of unknown microsamples were calculated.The δ^15N of the atmosphere was estimated at zero by this approach,which is concordant with the internationally recommended value.  相似文献   

8.
Based on the systematic analysis of the coal gangue in Weibei Coalfield, such as petrologic characteristics, chemical composition, nutrient elements, deleterious elements, and the transformation, and compared with the soil element content background values of Loess Plateau and national harmful materials controlling standards, we conclude that the coal gangue in the Weibei Coalfield has huge potential to be used as clay fertilizer.  相似文献   

9.
Since 1976 high arsenic coal in Xingren County, Guizhou Province, has attracted more and more attention because of coal-burning-type arsenic poisoning, There are many studies on enrichment of arsenic in high-arsenic coal and they come from difference materials： organic matter, authigenic pyrite, epigenetic pyrite, authigenic clay mineral and epigenetic clay mineral. In this paper, fourteen samples were examined by proximate analysis. Inductively coupled plasma mass spectrometry （ICP-MS） was used to determine the trace element contents of thirty-six samples in high-arsenic coal, As was determined by instrumental neutron activation analysis （INAA） and atomic fluorescence spectrometry （AFS）. SEM-EDX was used to analyze the contents of As, Sb, Tl and Se in sample XR-8 from Xingren, Guizhou, and we analyzed the petrographic compositions of the same sample.  相似文献   

10.
Eolian dust deposition is intimately related to atmospheric circulation and environmental setting of the source region, and therefore is an invaluable tool for studying the evolutionary history of atmospheric circulation patterns and paleoclimatic change. Identifying the provenance of any eolian deposit is crucial not only for reconstructing the paleoenvironmental history of the dust source region, but also for understanding the paleoclimatic significance of various indices. Loess and paleosol samples from the Garze region on the eastern margin of the Tibetan Plateau(TP) were analyzed for their elemental(major and trace elements) and isotopic(Sm-Nd) geochemistry and compared with those of Northern Chinese(NC) loess formed at the same age. The results show that the geochemical compositions of the Garze loess and paleosol samples are similar to those eolian deposits on the Chinese Loess Plateau(CLP), and also resemble the average UCC. This indicates that the eolian deposits on the eastern margin of the TP were derived from well-mixed sedimentary protoliths that had undergone numerous upper crustal recycling processes, just as with the CLP loess deposits. However, compared with NC loess, the Garze samples have higher ∑REE, Li, Rb, Zr, Cs, Hf and Bi concentrations, higher TiO2/Al2O3, Hf/Nb, La/Nb, Th/Nb and lower K2O/TiO2, Zr/Hf, Ba/Rb ratios. From the Sm-Nd isotopic geochemistry, εNd(0) and 147Sm/144Nd values of Garze loess and paleosol samples are clearly lower than the NC loess. The higher Bi, Zr and Hf concentrations are relevant to the widely distributed acid-magmatic rocks in this region, whereas the higher contents of Li, Cs, Rb are attributed to the high background values of the TP. The geochemical characteristics of the Garze loess and paleosol samples further prove that the local glacial and other Quaternary detrital sediments are predominantly the contributors for the eolian deposits on the eastern margin of the TP. Stable element concentrations and their ratios in the Garze loess and paleosol samples formed at different times have relatively greater variation ranges in comparison with the NC loess, indicating that the source regions for eolian deposits have been unstable since the late Early Pleistocene. We attribute the instability of dust sources to variable earth surface conditions and the changeable TP winter monsoon in direction and intensity, which are in turn related to the uplift of the TP.  相似文献   

11.
标准物质参考值的准确性在测试仪器校准、分析数据质量监控以及方法评价等方面具有非常重要的作用.为了检验国家地质标准物质参考值的准确性,本文应用高温高压密闭溶样-电感耦合等离子体质谱法分析了国家地质标准物质的18种岩石(GBW 07103 ～ GBW 07125)、19种沉积物(GBW 07301 ～ GBW 07318)和19种土壤(GBW 07401 ～ GBW 07430)中36种痕量与稀土元素.结果表明,除个别标准样品中的几个元素(Ni、Cr、Pb、Co、Cu、Sc、Yb、Lu)外,其余国家标准物质中36种元素测定结果的相对标准偏差均小于10％;绝大部分元素测定值的相对误差小于10％,测定值与参考值能较好地吻合.将误差较大元素的测定值与其他实验室的测定值以及文献报道值进行了比较,指出已有的参考值需要修正;针对部分沉积物和土壤中的元素未提供参考值,如GBW 07306的Ni、GBW 07313的Be、Hf、Ta,GBW 07314的Li、Be,GBW 07409、GBW 07410和GBW0741 1的Hf、Ta,GBW 07426的Gd、Ta,本文给出了相应的参考值.  相似文献   

12.
采用HNO3-HClO4-HF常压消解、HNO3-H2O2-HF高压密闭消解、HNO3-H2O2微波消解,干法灰化后残渣用HNO3-HF-HClO4溶解等四种方法对植物样品进行前处理,使用电感耦合等离子体质谱(ICP-MS)对植物样品中的27种元素进行定量分析,探讨了不同前处理方法对ICP-MS测定植物样品中微量元素的影响。分析结果表明: HNO3-HClO4-HF常压消解使用大量试剂,污染环境,造成空白值高;在常压体系中HClO4的加入能提高样品的消解效率,但赶酸不完全,会造成复合离子对钒和砷的干扰;干法灰化过程中某些元素(硼、汞等)会损失;常压消解和高压密闭消解中加入HF能有效地提高铍、稀土、钇、钛、锑、铀等元素的回收率,但在蒸干赶HF的过程中,会造成硼和汞的损失,并且钢套的生锈会造成铬、镍空白值高。尽管没有一种方法能适用于所有元素的分析,但相比较而言,HNO3-H2O2微波消解体系操作简单,大部分元素(除铍、钛、锑、铋、稀土)能得到满意的结果,精密度(RSD)均小于10%(n=10),相对误差(RE)为-4.6%~13.6%。  相似文献   

13.
The United States Geological Survey granitic and granodioritic reference materials G‐2 and GSP‐2 were decomposed in high‐pressure bombs using both HF‐HNO3 and HF‐HNO3‐HClO4 in order to evaluate the feasibility of characterising the entire suite of geologically relevant trace elements through direct analysis with a high‐resolution inductively coupled plasma‐mass spectrometer (HR‐ICP‐MS). The digested samples were diluted to the appropriate levels and analysed at low, medium and high resolution depending on the required sensitivity and potential interferences for each element. Memory effects during analysis of the high field strength elements (HFSE) were negligible when analysed using an all‐Teflon, uncooled sample introduction system and combined with adequate wash times with 4% v/v aqua regia + 0.5% v/v HF between samples. The concentration of the remaining lithophile elements was determined with a conventional, cooled, Scott‐type spray chamber using a wash solution of 1% v/v HNO3. Total procedural blanks contributed between 0.01 to 0.5% to final sample concentrations and blank subtractions were typically unnecessary. Abundances for Li, Hf, Ba, Zr, Ga, Rb, Sr, La, Ce, Th and U were systematically higher, while those for the heavy rare earth elements (HREEs), Cu and Y were systematically lower in this study compared to USGS values for G‐2 and GSP‐2. This is likely to be related to, respectively, higher recoveries from more efficient digestion of refractory phases (i.e., zircon, tourmaline), and better resolution of interferences when using a HR‐ICP‐MS. Sample digestion experiments also showed that perchloric acid digestion in high pressure bombs resulted in superior recoveries and better precision for the bulk of the trace elements analysed. The concentration of the remaining elements overlapped within uncertainty with recommended reference values and with values determined in other studies using isotope‐dilution TIMS, ICP‐MS and XRF. Concentrations for the elements Cd, Sn, Sb, Ta, Bi, Tb, Ni and Mo are also reported for G‐2 and GSP‐2 reference materials. Our study shows therefore that it is feasible to determine thirty‐nine geologically relevant trace elements accurately and directly in granitoid sample digests when using a HR‐ICP‐MS, thereby negating the need for ion exchange or isotopic spiking.  相似文献   

14.
In this contribution, we report Hf isotopic data and Lu and Hf mass fractions for thirteen Chinese rock reference materials (GBW07 103–105, 109–113 and 121–125, that is GSR 1–3, 7–11 and 14–18, respectively) that span a broad compositional range. Powdered samples were spiked with a 176Lu‐180Hf enriched tracer and completely digested using conventional HF, HNO3 and HClO4 acid dissolution protocols. Fluoride salts were dissolved during a final H3BO3 digestion, and chemical purification was performed using a single Ln resin. All measurements were carried out on a MC‐ICP‐MS. This work provides the first comprehensive report of the Lu‐Hf isotopic composition of Chinese geochemical rock reference materials, and results indicate that they are of comparable quality to the well‐characterised and widely used USGS and GSJ rock reference materials.  相似文献   

15.
采用HNO3-H2O2体系对植物样品进行风冷回流消解,电感耦合等离子体质谱法(ICP-MS)同时测定植物样品中46个元素的含量。将称有样品的磨口锥形瓶加装风冷管后直接放在普通平板铝块电热板上,一次可对45个锥形瓶回流装置同时进行加热,不需要严格地规定消解时间,保证回流加热微沸消解至消解完全即可。植物标准物质(GBW 10012、GBW 10014和GBW 10019)的分析结果与标准值相一致,方法精密度(RSD,n=6)为0.44%～5.59%。与干法灰化消解和微波消解等样品处理方法相比较,操作简单快捷,试剂用量少,空白值较低,溶液盐度较小,有利于植物样品中多元素ICP-MS同时测定。采用调试液调节ICP-MS仪器测定的最佳化,确定了ICP-MS测定的最佳条件,同时探讨了元素之间的干扰关系,采用数学校正法有效地消除了测定的干扰。  相似文献   

16.
应用电感耦合等离子体质谱法(ICP-MS)分析碳酸盐岩样品中的痕量元素,其中高钙基体的存在会对元素的分析信号产生明显的抑制或增强作用,从而引起显著的基体干扰。本文研究了硝酸-盐酸-高氯酸-氢氟酸四酸敞开溶样体系下ICP-MS同时测定碳酸盐岩中30种痕量元素的方法。重点分析了质谱干扰包括样品基体本身所带来的谱线干扰、同量异位素干扰和多原子离子干扰,并对钙含量高的碳酸盐岩样品中Ca对Ni的干扰进行了试验,分别采用数学公式或干扰系数等方法对干扰因素进行校正,使分析结果得到了明显改善。标准物质的测定值与标准值基本一致,方法精密度(RSD)除个别元素为10%~15%,大多数元素均小于10%,符合地质样品分析规范要求。  相似文献   

17.
Complete dissolution is essential to obtain accurate analytical results for geological samples. Felsic rocks are known to be very difficult to dissolve because of the presence of refractory minerals such as zircon. In this study, we undertook a systematic evaluation of the effect of the HF/HNO3 ratio, digestion time, digestion temperature, digested test portion mass and the presence of insoluble fluorides on analytical results for the felsic rock GSP‐2 using high‐pressure HF and HF/HNO3 digestion. Digestion in mixtures of HF and HNO3 acids is a commonly used method of dissolution for geological samples. However, our results clearly indicate that adding HNO3 inhibited the digestion capabilities of HF for refractory minerals such as zircon. It took 8–12 hr for Zr to be completely recovered in GSP‐2 at 190 °C, whereas it needed about 36 and 72 hr at 160 and 140 °C, respectively. White precipitates were observed in the final solution for test portion mass > 100 mg, irrespective of which of the five different digestion solutions was used (1 ml HF, 2 ml HF, 1 ml HF + 0.5 ml HNO3, 1 ml HF + 1 ml HNO3 and 1.5 ml HF + 1.5 ml HNO3). Environmental scanning electron microscopy showed that these precipitates were mainly composed of AlF3. Instead of further HCl, HNO3 or HClO4 attack, we propose that using ultra‐fine samples and a small sample size is a good way to avoid the formation of insoluble residues (e.g., fluorides). To further investigate the precision and accuracy of the proposed method (using HF alone as the digestion solution during the first acid attack step), a suite of silicate rock reference materials was analysed. Most of the results were found to be in reasonable agreement with the reference values, with a relative error of < 10%.  相似文献   

18.
利用电感耦合等离子体质谱法(ICP-MS)测定植物样品中微量元素的关键技术是消除植物样品的有机基体效应,本文通过预处理方法中的酸消解体系、称样量和消解方式消除其影响。以国家标准物质灌木枝叶组合样(GBW07603)为材料进行研究,对比分析了硝酸-过氧化氢、硝酸-氢氟酸、硝酸-氢氟酸-过氧化氢3种酸溶体系的消解效果,以确定最佳酸溶体系,进而定量研究2种称样量(50 mg和100 mg)和3种消解方式(密封高压二次消解、密封高压一次消解、微波消解)的消解效果,并以In作为内标采用ICP-MS测定微量元素含量。结果表明:硝酸-氢氟酸-过氧化氢酸溶体系的消解效果最好;50 mg的测定值更接近于参考值;微波消解法的测定值明显偏低,而密封高压二次消解法是灌木枝叶样品预处理的有效方法。  相似文献   

19.
Eleven synthetic silicate and phosphate glasses were prepared to serve as reference materials for in situ microanalysis of clinopyroxenes, apatite and titanite, and other phosphate and titanite phases. Analytical results using different micro-analytical techniques showed that the glass fragments were homogeneous in major and trace elements down to the micrometre scale. Trace element determinations using inductively coupled plasma-mass spectrometry (ICP-MS), multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS), laser-ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) and secondary ionisation mass spectrometry (SIMS) showed good agreement for most elements (Li, Be, B, Cs, Rb, Ba, Sr, Ga, Pb, U, Th, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Er, Tm, Yb, Lu, Zr, Hf, Ta, Nb) studied and provide provisional recommended values.  相似文献   

20.
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   

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