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1.
A method for the selective separation of Ag, Cd, Cr, Cu, Ni, Pb and Zn in traces from solutions of calcite (CaCO3), dolomite (CaMg(CO3)2) and gypsum (CaSO4.2H2O) before their determination by inductively coupled plasma-atomic emission spectrometry (ICP-AES) is presented. The expected interferences of Ca and Mg on intensities of trace analytes were removed by collecting the elements of interest with cobalt(III) hexamethylenedithiocar-bamate, Co(HMDTC)3. The flotation of aqueous solutions (1 l) of calcite, dolomite and gypsum was performed at pH 6.0, by 1.5 mg l−1 Co and 0.6 mmol l−1 HMDTC−. To minimise the effect of the reaction between Ca/Mg, which restrains the function of the surfactant, careful selection of the most suitable foaming reagent was necessary. The accuracy of the method was established by analysing natural alkaline-earth minerals by the standard addition method as well as using the dolomite reference materials GBW 07114 and GSJ JDo-1. The ICP-AES limits of detection following flotation on different minerals were found to be 0.080 μg g−1 for Cd, 0.105 μg g−1 for Ag, 0.142 μg g−1 for Cu, 0.195 μg g−1 for Cr, 0.212 μg g−1 for Ni, 0.235 μg g−1 for Zn and 0.450 μg g−1 for Pb.  相似文献   

2.
Fluorine, chlorine, bromine, iodine and sulfur were determined in seventeen geological reference materials after extraction by pyrohydrolysis. Fluorine, Cl and S (as sulfate ions) were determined in the extraction solution by ion chromatography with detection limits of around 0.2 mg l−1. Bromine and I were measured by ICP-MS with detection limits of 1 μg l−1 for Br and 0.1 μg l−1 for I. For rock samples, using normal extraction conditions (500 mg of sample and 100 ml of final solution) detection limits were 40 mg kg−1 for F and Cl, 15 mg kg−1 for S, 0.2 mg kg−1 for Br and 0.02 mg kg−1 for I. These detection limits may be improved by increasing the amount of sample and hence the concentration of the final solution. Water was also determined using an extraction technique based on H2O degassing, reduction on zinc at 1000 °C and H2 manometry. Our results for fluorine, chlorine, sulfur and water are in good agreement with literature data. Very few reference materials have recommended values for bromine and especially for iodine. Among the analysed samples, three are new reference materials: BHVO-2, BCR-2 and AGV-2.  相似文献   

3.
Trace elements in the Geological Survey of Japan carbonate reference materials Coral JCp-1 and Giant Clam JCt-1 were determined by inductively coupled plasma-mass spectrometry after digestion with 2% v/v HNO3. A standard addition method was adopted in this determination in order to neutralise the Ca matrix effect. In addition, Sc, Y, In and Bi were used as internal standards to control the matrix effect and correct instrumental drift. Of the eighteen elements measured in JCp-1, precisions for fourteen elements, including Cu, Cd and Ba, were better than 10% RSD and concentrations ranged from 0.002 μg g-1 (Cs) to 8.02 μg g-1 (Ba). The concentrations of measured trace elements in JCt-1, except for Cu, were lower than those in JCp-1. Precisions for all elements with concentrations higher than 0.04 μg g-1 in JCt-1 were also better than 10% RSD and concentrations were found to be between 0.001 μg g-1 (Cs) and 4.84 μg g-1 (Ba). The concentrations of more than fifteen trace elements in the aragonite reference materials are reported here for the first time. Both reference materials are suitable for use in geochemical studies of environmental reconstruction based upon biogenic carbonate materials.  相似文献   

4.
The high sensitivity, minimal oxide formation and single internal standard capability of high resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS) is demonstrated in the direct determination of Sc, Y and REE in the international reference materials: basalts (BCR-1, BHVO-1, BIR-1, DNC-1), andesite (AGV-1) andultramafics (UB-N, PCC-1 and DTS-1). Time consuming ion exchange separation or preconcentration were found to be unnecessary. Smooth chondrite normalized plots of the REE in PCC-1 and DTS-1 were obtained in the range 0.8-50 ng g-1 (0.01-0.1x chondrite). Method precision was found to be digestion dependent with an average external repeatability of 2-4% for the basalts, AGV-1 and UB-N, and 10% for PCC-1 and DTS-1. The mass peak due to 45Sc was completely resolved from 29Si16O and 28Si16O1H spectral interferences using medium resolution, which casts doubt on the accuracy of Sc determinations using quadrupole ICP-MS. Literature values for Y in rock reference materials were found to be approximately 9% high after HR-ICP-MS and XRF analysis.  相似文献   

5.
Six low abundance rock reference materials (basalt BIR-1, dunite DTS-1, dolerite DNC-1, peridotite PCC-1, serpentine UB-N and basalt TAFAHI) have been analysed for high field strength elements (Zr, Nb, Hf, Ta, Th and U), Rb, Sr, Mo, Sb, Cs, Tl and Bi at ng g−1 levels (in rock) by magnetic sector inductively coupled plasma-mass spectrometry after HF/HClO4 high pressure decomposition. The adopted method uses only indium as an internal standard. Detection limits were found to be in the range of 0.08 to 16.2 pg ml−1 in solution (equivalent to 0.08 to 16.2 ng g−1 in rock). Our data for high field strength elements, Rb, Sr, Mo, Sb, Cs, Tl and Bi for the six selected low abundance geological reference materials show general agreement with previously published data. Our Ta values in DTS-1 and PCC-1 (1.3 and 0.5 ng g−1) are lower than in previously published studies, providing smooth primitive mantle distribution patterns. Lower values were also found for Tl in BIR-1, DTS-1 and PCC-1 (2, 0.4 and 0.8 ng g−1). Compared with quadrupole ICP-MS studies, the proposed magnetic sector ICP-MS method can generally provide better detection limits, so that the measurement of high field strength elements, Rb, Sr, Mo, Sb, Cs, Tl and Bi at ng g−1 levels can be achieved without pre-concentration, ion exchange separation or other specialised techniques.  相似文献   

6.
江苏基础地质工作程度概述   总被引：1，自引：0，他引：1  
江苏基础地质工作开展较早，研究程度较高，从区域地质调查，地球物理勘探，地球化学勘探三方面对江苏的基础地质工作情况进行了概述。  相似文献   

7.
Cordierite samples from pegmatites and metamorphic rocks have been analysed for major [electron microprobe analysis (EMPA)] and trace elements [inductively coupled plasma mass spectrometry (ICP-MS), secondary ion mass spectrometry analyses (SIMS)] as well as for H2O and CO2 (coulometric titration), and the results evaluated in conjunction with published data in order to determine which exchange mechanisms are significant. Apart from the homovalent substitutions FeMg−1 and MnMg−1 on the octahedral site, some minor KNa−1 on the Ch0 channel site, and Fe3+Al−1 on the T11 tetrahedral site, the three most important substitution mechanisms are those for the incorporation of Li on the octahedral sites (NaLi□−1Mg−1), and of Be and other divalent cations on the tetrahedral T11 site (NaBe□−1Al−1 and Na(Mg,Fe2+)□−1Al−1). The dominant role of the last vector is clearly demonstrated. We propose a new generalized formula for cordierite: Ch(Na,K)0–1 VI(Mg,Fe2+,Mn,Li)2 IVSi5 IVAl3 IV(Al, Be, Mg, Fe2+, Fe3+)O18 *xCh(H2O, CO2…). Our results show that the population of (Mg, Fe2+) on the T11-site is limited to about 0.08 a.p.f.u. Other exchange mechanisms that were encountered in experiments operate only under P–T conditions or in bulk compositions that are rarely realized in nature. Routine analyses by electron microprobe in which Li and Be are not determined can be plotted as (Mg+Fe+Mn) versus (Si+Al) to assess whether significant amounts of Li and Be could be present. These amounts can be calculated as Li (a.p.f.u.)=Al+Na–4 and Be (a.p.f.u.)=10–2Al–M2+–Na.  相似文献   

8.
New concentrations for Au, Ir and Ag obtained by instrumental neutron activation analysis are presented for seventy geochemical reference materials. Results in agreement with literature values for Au and Ir down to concentrations of a few ng g−1 were obtained. For Au and Ir concentrations above 10 ng g−1, the repeatability of replicate analyses of reference materials was mostly better than 10%. For concentrations between 1 and 10 ng g−1 the RSD for Ir was 10–30%, whereas for Au it was higher and more variable (20–50%). In addition, concentrations for Cd and Hg are presented for some of the same reference materials. The high RSD at relatively high concentrations seen in gold for some RMs (e.g., WMG-1, WMS-1) did not exist for Ir and suggests homogeneity for this platinum-group element at the sub-sample size used in this study. For the following eight RMs, mostly ultramafic rocks (CHR-Pt+, OREAS-13P, OREAS-14P, PCC-1, UMT-1, WMG-1, WMS-1, WPR-1), Ir measurements agreed within ± 10% of mostly certified or recommended concentrations, which ranged from 2 ng g−1 to 6 μg g−1. For the reference material UB-N, iridium concentration compared favourably to published results obtained by isotope dilution ICP-MS methods and a previously unrecognised heterogeneity is inferred for Au, Hg and Sb, but not for the other measured elements.  相似文献   

9.
利用细颗粒热释光技术对渭南剖面重要地层界线处的 7个样品进行了年龄测定 ,并在此基础上 ,结合已发表数据利用多项式回归方法建立了渭南剖面高分辨率的古气候时间标尺 ,其中S0 /L1- 1,L1- 1/L1- 2 ,L1- 4/L1- 5 ,L1- 5 /S1,S1/L2的界线年龄分别为 1.1,2 .5 ,5 .1,7.6 ,12 .8ka ,除了L1- 4/L1- 5的界线年龄与氧同位素 3阶段的起始年龄差距较大之外 ,它们与SPECMAP深海氧同位素 5以上各阶段的界线年龄可进行较好的对比 ,而L1- 4/L1- 5的界线年龄与北太平洋风尘记录的氧同位素年龄却有很好的一致性 .  相似文献   

10.
使用珠海市1984—2015年R1h-R6h、R1h-R12h、R1h-R24h3个历时暴雨组合推算排水排涝两级标准衔接的设计暴雨水平。应用阿基米德极值Copula与Kendall分布函数构建不同历时暴雨组合的联合概率分布模式。分析各历时暴雨组合的遭遇概率、"或"重现期、"且"重现期和二次重现期,以出现最大可能概率的方法推算各组合的设计暴雨值。结果表明:二次重现期所对应的累积频率更准确地代表了特定设计频率情况下不同历时暴雨组合的风险率;重现期分别为2年、3年、5年、10年、20年、50年、100年推算的二次重现期设计值介于"或"重现期和"且"重现期设计值之间,小于相应的边缘分布重现期设计值,R1h-R6 h组合推算的设计值相对误差为3.1%~7.1%;R1h-R12h组合推算的设计值相对误差为3.3%~9.3%;R1 h-R24 h组合推算的设计值相对误差为3.9%~12.0%。二次重现期推算的不同历时暴雨组合的设计暴雨分位值为内涝工程的风险管理和管渠尺寸提供了优选标准和设计参考。  相似文献   

11.
We found that the suppression of signals for 88Sr, 140Ce and 238U in rock solution caused by rock matrix in ICP-MS (matrix effects) was reduced at high power operation (1.7 kW) of the ICP. To make the signal suppression by the matrix negligible, minimum dilution factors (DF) of the rock solution for Sr, Ce and U were 600, 400 and 113 at 1.1, 1.4 and 1.7 kW, respectively. Based on these findings, a rapid and precise determination method for Rb, Sr, Y, Cs, Ba, REE, Pb, Th and U using FI (flow injection)-ICP-MS was developed. The amount of the sample solution required for FI-ICP-MS was 0.2 ml, so that 1.8 mg sample was sufficient for analysis with a detection limit of several ng g-1. Using this method, we determined the trace element concentrations in the USGS rock reference materials, DTS-1, PCC-1, BCR-1 and AGV-1, and the GSJ rock reference materials, JP-1, JB-1, -2, -3, JA-1, -2 and -3. The reproducibilities (RSD %) in replicate analyses (n=5) of BCR-1, AGV-1, JB-1, -2, -3, JA-1, -2, and -3 were < 6 %, and typically 2.5%. The difference between the average concentrations of this study for BCR-1 and those of the reference values were < 2%. Therefore, it was concluded that the method can give reliable data for trace elements in silicate rocks.  相似文献   

12.
Fifty-two trace elements in NIST SRM 614, 616 and MPI-DING BM90/21-G glass reference materials as well as in NIST SRM 612, USGS BCR2-G and other MPI-DING reference glasses (KL2-G, GOR132-G, GOR128-G, ATHO-G, Tl-G, StHs6/80-G and ML3B-G) were determined by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Accurate ultra-low trace element abundances in the NIST SRM 614, 616 and BM90/21-G reference glasses down to lower ng g−1 levels were determined with relative standard deviations (RSD) of less than 10%. Limits of detection using He as carrier gas were up to two times lower than with Ar and were 0.004 to 0.12 μg g−1 for elements of lower mass numbers (amu < 85) and 0.002 to 0.06 μg g−1 for elements having amu < 85. The measured concentrations generally agree within 15% with previous studies except for B in NIST SRM 614 and 616, which appears to be heterogeneously distributed, and Co, Zn, Ga and Ag in NIST SRM 616 for which the existing data set is too small to evaluate the discrepancies. New values for As (0.593 μg g−1), Ag (0.361 μg g−1) and Cd (0.566 μg g−1) in NIST SRM 614 and new values for Na (94864 μg g−1) and As (0.276 μg g−1) in NIST SRM 616 are reported.  相似文献   

13.
TheWeinanloesssectionislocatedatNanjiangVillage(34"21'N,lO9"3l'E),YangguoTown,Weinan,ShaanxiProvince,whichisoneofthecontinuousloesssequencedis-coveredofthelasto.l5MaB.P.,whichhassoforbeenthebestdatedbyboththeAMSl4CandTL(Liuetal.,l994),andisusedasastratigraphicstandard.Basedontheorbitaltuningmethod(Dingetal.,l99l)lapreliminaryhighresolu-tiontimescaleofthissectionhasbeenestab1ished(Liuetal.,l995).Howeverlinrecentyears,increasingeffortshavebeenmadetodocumentsub-orbitalscaleclimaticvariat…  相似文献   

14.
Twenty-eight samples of groundwater from bedrock boreholes in three distinct Norwegian geological provinces have been taken and analyzed for content of Rn, U, and Th, together with a wide variety of minor and major species. Median values of 290 Bq/1, 7.6 g/1, and 0.02 g/1 were obtained for Rn, U, and Th respectively, while maximum values were 8500 Bq/1, 170 g/1, and 2.2 g/1. Commonly suggested drinking water limits range from 8 to 1000 Bq/1 for radon and 14 to 160 g/1 for uranium. Radioelement content was closely related to lithology, the lowest concentrations being derived from the largely Caledonian rocks of the Trøndelag area, and the highest from the Precambrian Iddefjord Granite of southeast Norway (11 boreholes) where median values of 2500 Bq/1, 15 g/1 and 0.38 g/1, respectively, were obtained. The Iddefjord Granite is not believed to be unique in Norway in yielding high dissolved radionuclide contents in groundwaters, and several other granitic aquifers warrant further investigation in this respect.  相似文献   

15.
为了研究南堡凹陷南堡1号馆三段火山岩盖层上下油气分布规律,在馆三段火山岩盖层及其内油气渗漏断裂发育及分布特征研究的基础上,通过对馆三段火山岩盖层断接厚度与其封油气所需最小断接厚度相对大小的比较和对油气渗漏断裂凸面脊的确定,预测了南堡1号构造馆三段断盖配置油气渗漏部位;并结合油气分布,对断盖配置油气渗漏部位对油气成藏与分布的控制作用进行了研究。结果表明,南堡1号构造馆三段断盖配置发育10处油气渗漏部位,其中：F2及分支断裂油气渗漏部位最发育,有3处油气渗漏部位;其次是F1、F6断裂,有2处油气渗漏部位;F3、F4、F5和F7断裂仅各发育1处油气渗漏部位。这些油气渗漏部位及附近有利于下伏东一段油气在上覆馆三段之上聚集成藏,应是造成南堡1-1断鼻、南堡1-3断块和南堡1-5断鼻北部油区油气既可以分布在下伏东一段又可分布在馆三段之上,而南堡1-5断鼻南部油气仅分布在下伏东一段的根本原因。  相似文献   

16.
末次间冰期以来对宁黄土剖面的热释光测年   总被引：2，自引：0，他引：2  
利用细颗粒热释光技术对陇西黄土高原会宁黄土剖面末次间冰期以来黄土、古土壤的8个样品进行了年龄测定,并在此基础上分别利用线性内插和多项式回归方法建立了会宁剖面深度-年代时间模式,以2种模式计算的S0/L1、L1/S1、S1/L2界线年龄与SPECMAP深海氧同位素1/2、4/5、5/6阶段的界线年龄可较好对比,这为末次间冰期以来会宁地区古气候演化的深入研究提供了基本时间框架。  相似文献   

17.
This paper describes the creation of two new reference samples of black shale, SCHS-1 and SLg-1, collected in the Bodaibo Region of Irkutsk District (Siberia, Russia). These samples have been developed as State Standard Samples to meet the requirements of Russia's Normative Documents, so that they can be recognised by the Russian State Certification Agency and included on the State Register of certified reference materials. SCHS-1 was produced from shale of the Khomolkho suite; SLg-1 represents the average composition of the Sukhoy Log gold deposit (within Au mineralisation). The homogeneity was assessed by applying the concept of potential inhomogeneity, and the inhomogeneity uncertainties (σinhom) for the indicator elements that were estimated experimentally by silicate XRF analysis. It was found that a majority of the indicator elements was characterised by σinhom/Δp < 1/8 (Δp is the permissible certification uncertainty), and so σinhom was neglected for the indicator elements and all other elements that were included in their respective group. The value of σinhom calculated for Fe (σinhom,Fe/Δp > 1 /8) was taken into consideration for the noble metals and their associated elements (e.g., Ag, As, Au, etc.). More than fifty laboratories (thirty-seven from Russia) were involved in the interlaboratory experiment (ILE) to analyse these reference samples. The data obtained from the ILE allowed SCHS-1 and SLg-1 to be certified for, fifty-one and forty-three elements, respectively, as State Standard Samples.  相似文献   

18.
We have measured 87Sr/86Sr and 143 Nd/144 Nd isotope ratios in different batches and aliquots of the new US Geological Survey (USGS) reference materials (RMs) BCR-2, BHVO-2, AGV-2 and GSP-2 and the original USGS RMs BCR-1, BHVO-1, AGV-1 and GSP-1 by thermal ionisation mass spectrometry. In addition, we also analysed the eight Max-Planck-Institut-Dingwell (MPI-DING) reference glasses. Nearly all isotope ratios obtained in the different aliquots and batches agree within uncertainty limits indicating excellent homogeneity of the USGS powders and the MPI-DING glasses. With the exception of GSP-2, the new USGS RMs are also indistinguishable from the ratios found in the original USGS RMs (87Sr/86Sr: 0.704960, 0.704958 (BCR-1, -2), 0.703436, 0.703435 (BHVO-1, -2), 0.703931, 0.703931 (AGV-1, -2); 143 Nd/144 Nd: 0.512629, 0.512633 (BCR-1, -2), 0.512957, 0.512957 (BHVO-1, -2); 0.512758, 0.512755 (AGV-1, -2)). This means that for normalisation purposes in Sr and Nd isotope geochemistry BCR-2, BHVO-2 and AGV-2 can well replace BCR-1, BHVO-1 and AGV-1 respectively.  相似文献   

19.
The analysis of granitic pegmatites still remains a challenge because suitable natural reference materials are scarce or not available. Two new reference materials were prepared at the Smithsonian Institution, to provide an avenue to pursue the geochemical analysis of micas and feldspars in granitic pegmatites: STL-1, the Stewart lepidolite (NMNH 174041) and ZA-1, the Zapot amazonite (NMNH 174042). STL-1 was prepared from lepidolite collected from the lithium-rich Stewart pegmatite, San Diego County, California (33°22'52'N, 117°03'41'W). ZA-1 was prepared from an amazonite from the topaz-bearing Zapot pegmatite, Mineral County, Nevada, (38° 41'N, 118 °33'W). The results of this study indicated that STL-1 and ZA-1 are homogeneous and could be used as reference materials that would allow the expansion of calibration curves in XRF analysis up to 16000 μg g−1 for Rb, 2000 μg g−1 for Cs and 100 μg g−1 for Tl. STL-1 and ZA-1 also contain unusually high concentrations of Ga and Tl, and STL-1 of Nb.  相似文献   

20.
Fractal models for the fragmentation of rocks and soils: a review   总被引：22，自引：0，他引：22  
Fragmentation, the process of breaking apart into fragments, is caused by the propagation of multiple fractures at different length scales. Such fractures can be induced by dynamic crack growth during compressive/tensile loading or by stress waves during impact loading. Fragmentation of rocks occurs in resoonse to tectonic activity, percussive drilling, grinding and blasting. Soil fragmentation is the result of tillage and planting operations. Fractal theory, which deals with the scaling of hierarchical and irregur systems, offers new opportunities for modeling the fragmentation process. This paper reviews the literature on fractal models for the fragmentation of heterogeneous brittle earth materials. Fractal models are available for the fragmentation of: (1) classical aggregate; (2) aggregates with fractal pore space; and (3) aggregates with fractal surfaces. In each case, the aggregates are composed of building blocks of finite size. Structural failure is hierarchical in nature and takes place by multiple fracturing of the aggregated building blocks. The resulting number-size distribution of fragments depends on the probability of failure, P(1/bi) at each level in the hierarchy. Models for both scale-invariant and scale-dependent are reviewed. In the case of scale-invariant P(1/bi)< 1, theory predict: Df = 3 + log [P(1/bi)]/log[b] for classical aggregates; Df=Dm+log[P(1/bi)]/log[b] for aggregates with fractal pore space; and Df=Ds for aggregates with fractal surfaces. where b is a scaling factor and Df, Dm and Ds are the fragmentation, mass and surface fractal dimensions, respectively. The physical significance of these parameters is discussed, methods of estimating them are reviewed, and topics needing further research are identified.  相似文献   

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