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1.
发射光谱法测定勘查地球化学样品中银硼锡钼铅   总被引:21,自引:13,他引:21  
张雪梅  张勤 《岩矿测试》2006,25(4):323-326
以K2S2O7、NaF、Al2O3和炭粉为缓冲剂,Ge为内标,电弧发射光谱法测定勘查地球化学样品中Ag、B、Sn、Mo、Pb。方法检出限为Ag0.013μg/g、B0.83μg/g、Sn0.23μg/g、Mo0.073μg/g、Pb0.37μg/g。方法精密度(RSD,n=12)为Ag4.2%~11.3%、B3.2%~6.5%、Sn2.6%~7.1%、Mo2.9%~6.3%、Pb1.57%~5.18%。测定了国家一级地球化学标准物质,结果与标准值相符。  相似文献   

2.
在原子荧光光谱法传统样品前处理的基础上,提出了悬浮液进样技术。用琼脂作为悬浮剂,水溶液作为校正曲线,对土壤标准样品和实际样品进行测定,结果令人满意,并且省去了冗长的样品化学前处理过程。检出限分别为砷0.33μg/L、锑0.13μg/L、硒0.06μg/L;相对标准偏差分别为:砷3.92%~6.32%、锑1.76%~3.11%、硒3.08%~5.54%;回收率分别为砷98.7%~105.7%、锑99.5%-103.3%和硒94.6%-107.2%。国家一级标准物质的测定结果与标准值相符,实际样品的测定值与传统消化法相比较,结果基本一致。  相似文献   

3.
深孔电极载体蒸馏光谱法测定化探样品中八个易挥发元素   总被引:2,自引:2,他引:2  
熊艳 《岩矿测试》2007,26(5):425-427
以碘化铵、硫酸钠、硫粉、碳粉、氧化钙、二氧化硅混合物为缓冲剂,深孔电极,截取曝光,以谱带背景作内标,一次摄谱同时测定化探样品中As、Sb、Bi、Ag、Pb、Cd、Tl、Sn等微量元素。方法精密度(RSD,n=10)为1.2%-5.0%,检出限为0.013—1.0μg/g。方法经国家一级标准物质验证,测定结果与标准值基本相符。  相似文献   

4.
采用充氩电荷注入检测器(CID)-电感耦合等离子体原子发射光谱仪结合HF—HNO3-HClO4-H3PO4密封溶样法,建立了适用于多目标地质调查中土壤、水系沉积物等地质样品中B、As、S的同时测定方法。方法的特点是通过加入少量H3PO4避免了易挥发元素B的挥发损失;采用Se 196.0nm谱线为内标,对残留空气对超紫外区谱线测定中的强度漂移影响起到了很好的补偿作用;该方法还可同时测定Cu、Pb、Zn、Cr、Ni、Li、Mn和V等微量元素。B、As、S的仪器检出限(3SD,μg/mL)分别为0.01、0.008、0.03,方法检出限(10SD,DF=100,μg/g)分别为2.61、3.28、9,58。用国家标准物质土壤GBW 07401-07408,水系沉积物GBW 07309-07312验证了测定B、As、S的准确性及精密度,允许误差范围之内,测定值与标准值接近,样品10次测定的RSD为4.34%~25.0%。  相似文献   

5.
研究了碘化钾-甲基异丁基甲酮(KI—MIBK)萃取-火焰原子吸收分光光度法连续测定地球化学样品中痕量银、镉和铊的主要条件。通过对火焰原子吸收分光光度计气路控制系统及雾化器的改进,较大地改善了萃取-火焰原子吸收分光光度法测定银、镉和铊的稳定性和灵敏度。选择萃取酸度为1.2mol/L HCl、水相和有机相体积配比为3:1~4:1,方法精密度(RSD,n=12)为Ag4.5%~9.6%、Cd1.5%~7.9%、T14.5%~5.4%,检出限(3s)为Ag0.004μg/g、Cd0.007μg/g、T10.011μg/g,符合多目标地球化学调查样品测试及质量监控要求。用国家一级标准物质和密码组合标准物质进行验证,测试结果令人满意。  相似文献   

6.
发射光谱法快速测定银锡铜铅锌钼铍   总被引:4,自引:9,他引:4  
叶晨亮 《岩矿测试》2004,23(3):238-240
使用两台摄谱仪同时接收光谱,以K2S2O7、NaF、Al2O3为缓冲剂,Ge、Sb为内标,测定化探样品中7项元素,检出限(μg/g)分别是:Ag0.02,Sn0.5,Cu 1,Pb 2,Zn 10,Mo 0.2,Be 0.5;精密度(RSD,n=20)在2.9%~16.8%。采用国家一级标准物质验证方法可靠性,测定结果与标准值一致。  相似文献   

7.
多目标地球化学调查土壤样品中氮和碳的快速测定   总被引:2,自引:1,他引:2  
详细研究了元素分析仪的工作条件,建立了直接固体进样同时测定多目标地球化学调查土壤样苎支氮、碳的方法。方法简便、快速,检出限为氮14.5μg/g、碳0.013%。经土壤国家一级标准物质分析验证,测定值与标准值相符,精密度(RSD,n=12)为氮1.49%-3.27%、碳0.64%~3.63%。  相似文献   

8.
王洪彬 《岩矿测试》2007,26(6):503-504
样品用硝酸-高氯酸混合酸消解,考察了氢化物发生-原子荧光光谱法测定面粉中微量砷的实验条件,包括混合酸和还原剂硼氢化钾的用量。方法测定砷的线性范围为0.0—30.0μg/L,仪器的检出限为0.26μg/L,加标回收率为94.0%-104.0%,方法的精密度(RSD,n=11)为1.16%。方法操作简便、快速、灵敏度高。  相似文献   

9.
原子吸收法连续测定铋及氧化铋中铜铅铁镉镍   总被引:7,自引:2,他引:7       下载免费PDF全文
张耀春 《岩矿测试》2003,22(1):70-72
HNO3分解样品后,直接用火焰原子吸收法测定铋及氧化铋中铜、铅、铁、锡、镍。方法的检出限分别为Cu 0.22μg/g,Pb1.5μg/g,Fe0.39μg/g,Cd0.11μg/g,Ni0.34μg/g。与国标方法进行比较,分析结果基本一致,精密度试验,各元素的RSD(n=6)≤5.2%。  相似文献   

10.
陈世忠 《岩矿测试》2003,22(3):228-230
报道了以NH4H2PO4为基体改进剂,采用悬浮体制样石墨炉原子吸收光谱法直接测定琥珀中微量铅的方法。试验了影响测定的主要因素。在优化实验条件下。方法的检出限为0.038μg/g,Pb的质量浓度为0~80μg/L时,工作曲线线性关系良好。对于ω(Pb)=5.71μg/g样品的测定,相对标准偏差(RSD,n=5)为6.83%。  相似文献   

11.
Komatiites are mantle-derived ultramafic volcanic rocks. Komatiites have been discovered in several States of India, notably in Karnataka. Studies on the distribution of trace-elements in the komatiites of India are very few. This paper proposes a simple, accurate, precise, rapid, and non-destructive wavelength-dispersive x-ray fluorescence (WDXRF) spectrometric technique for determining Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Ba, Pb, and Th in komatiites, and discusses the accuracy, precision, limits of detection, x-ray spectral-line interferences, inter-element effects, speed, advantages, and limitations of the technique. The accuracy of the technique is excellent (within 3%) for Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Zr, Nb, Ba, Pb, and Th and very good (within 4%) for Y. The precision is also excellent (within 3%) for Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Ba, Pb, and Th. The limits of detection are: 1 ppm for Sc and V; 2 ppm for Cr, Co, and Ni; 3 ppm for Cu, Zn, Rb, and Sr; 4 ppm for Y and Zr; 6 ppm for Nb; 10 ppm for Ba; 13 ppm for Pb; and 14 ppm for Th. The time taken for determining Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Ba, Pb, and Th in a batch of 24 samples of komatiites, for a replication of four analyses per sample, by one operator, using a manual WDXRF spectrometer, is only 60 hours.  相似文献   

12.
本文拟定了一种以熔融法制备样片,用X射线荧光光谱测定硅酸盐类样品中Si、Fe、Al、Tj、Mn、Ca、Mg、K、Na、P等元素的分析方法。在对不同靶材X光管和分光晶体实验对比的基础上,选择了最佳的测量条件。该法具有快速、准确,测量范围广,检测限低,价格便宜等优点。经过近百个各种类型标样或管理样品的分析对比表明,本法不仅适用于硅酸盐类岩石样品的分析,还适用于铁矿、铝土矿、碳酸盐类岩矿样品以及水泥、耐火材料等样品的分析。  相似文献   

13.
最新的流行病学研究表明,空气中较高浓度的悬浮细颗粒可能对人类的健康有不利的影响。根据该项研究显示,由于心脏病、慢性呼吸问题和肺功能指标恶化而导致死亡率的升高与细尘粒子有关。这些研究结果已经促使欧盟于1999年4月出台了限制空气中二氧化硫、二氧化氮、氧化氮、铅和颗粒物含量的法案(1999/30/EC),对各项指标包括对可吸入PM10颗粒的浓度提出了新的限制性指标。PM10颗粒是指可以通过预分级器分离采集的气体动力学直径小于10μm的细颗粒。目前研究的兴趣重点逐步偏向PM2.5这些更细微颗粒物,PM2.5这种颗粒物对健康有明显的不利影响。在欧盟指令2008/50/EC中,对PM10和PM2.5都提  相似文献   

14.
This paper reports the first results of a study of 11 isotope systems (3He/4He, 40Ar/36Ar, 34S/32S, 65Cu/63Cu, 62Ni/60Ni, 87Sr/86Sr, 143Nd/144Nd, 206–208Pb/204Pb, Hf–Nd, U–Pb, and Re–Os) in the rocks and ores of the Cu–Ni–PGE deposits of the Norilsk ore district. Almost all the results were obtained at the Center of Isotopic Research of the Karpinskii All-Russia Research Institute of Geology. The use of a number of independent genetic isotopic signatures and comprehensive isotopic knowledge provided a methodic basis for the interpretation of approximately 5000 isotopic analyses of various elements. The presence of materials from two sources, crust and mantle, was detected in the composition of the rocks and ores. The contribution of the crustal source is especially significant in the paleofluids (gas–liquid microinclusions) of the ore-forming medium. Crustal solutions were probably a transport medium during ore formation. Air argon is dominant in the ores, which indicates a connection between the paleofluids and the atmosphere. This suggests intense groundwater circulation during the crystallization of ore minerals. The age of the rocks and ores of the Norilsk deposits was determined. The stage of orebody formation is restricted to a narrow age interval of 250 ± 10 Ma. An isotopic criterion was proposed for the ore-bearing potential of mafic intrusions in the Norilsk–Taimyr region. It includes several interrelated isotopic ratios of various elements: He, Ar, S, and others.  相似文献   

15.
Mining induced subsidence can significantly affect mining costs where major surface facilities and natural environment need to be protected. Overburden grout injection is a technology used to control coal mine subsidence by injecting the mine waste material extracted from the coal back into the inter-burden rock during longwall mining. The flowing slurry is here categorised as a nonlinear viscous cohesive (Bingham plastic) fluid. During longwall mining the grout slurry is pumped into the separated beds of the rock mass through a central vertical borehole, which is drilled deep into the inter-burden rock strata above the coal seam. However, a blockage can occur in the injection system when the slurry velocity falls below a certain critical threshold velocity, indicating a material phase change from cohesive-viscous to cohesive-frictional. In situ field injection tests through boreholes have been simulated at a smaller scale at the CSIRO laboratory in Brisbane by pumping the slurry through a radial disk (gap = 4 mm) from its centre. Laboratory experiments indicate a general, nonlinear, cohesive, viscous, frictional model for shear behaviour of the slurry, in which the material shear parameters are functions of the disk radial distance. Complete dimensional and dimensionless analytical solutions have been developed based on an approach related to Bingham–Herschel–Bulkley fluid mechanics. The derived formulae include relations for minimum pump pressure, local pressure and pressure gradient, wall shear stress, volume rate, velocity and velocity gradient. The theoretical results match the experimental measurements. The experiments covered slurries with maximum particle sizes of 0.5 to 2 mm with about 50% being larger than 100 µm. The viscosities at the various solids concentrations were measured with a standard torsion viscometer. This study differs from the previous research in several distinct aspects, namely, consideration of the variable shear parameters rather than fixed values, inclusion of total nonlinear behaviour, and implementation of a friction function to mimic behaviour of the deposited and consolidating stiff slurry, which can cause a significant pressure rise as a result of the increased shear resistance.  相似文献   

16.
本文介绍样品经四硼酸锂熔融制成玻璃小饼。采用Lachance模式和理论a系数来校正元素间的效应,由3080E型X-射线荧光谱仪和DF-350B数据处理系统完成硅酸盐中十三个项目的测定。  相似文献   

17.
岩石密度和超高压岩石折返速率   总被引:1,自引:3,他引:1  
在常温常压条件下对中国大陆科学钻CCSD主孔100-3000米岩心样品进行了密度测量,建立了密度连续剖面,并界定了不同超高压岩石的密度值。通过对比高温高压物性实验资料,岩石密度随着退变程度增强而降低,榴辉岩密度变化序列为3.52g/cm3→3.49g/cm3→3.07g/cm3→2.93g/cm3。超高压长英质岩石密度变化序列为3.00g/cm→2.80g/cm3→2.65g/cm3。上述实验资料是讨论不同折返阶段岩石所受浮力的基础,为研究折返速率大小提供了基本参数。本文通过折返板块运动平衡时,上浮力与粘滞力平衡这一关系式,定量研究了大陆俯冲板块的折返速率,认为密度差产生上浮力从而引起折返,温度对板块折返速率的影响最为显著;密度差大小、折返角度、折返板块大小对折返速率也有直接的影响。定量模拟分析表明,在温度高于850℃时,板块的折返速率可以超过100mm/a;当温度降至700℃时,折返速率则低于1.5mm/a。作者认为在折返早期,温度较高,板块快速折返至60-70km榴辉岩相深度;随着传导散热,温度降低,板块以较慢的速率折返至中下地壳。折返速率的估算表明,浮力是板块折返第一阶段(从>100km深部折返至<40km的中下地壳)的主要驱动力。  相似文献   

18.
Bellechester, Minnesota, is a small community of approximately 155 residents located on the county line between Goodhue and Wabasha counties in southeast Minnesota's karst region. Bellechester is served by a 21-year-old wastewater treatment facility (WWTF) consisting of three waste-stabilization ponds. On 28 April 1992 six sinkholes were discovered to have drained cell 2 of the WWTF resulting in the loss of approximately 8.7×106 1 of partially treated effluent and about 600 m3 of soil into previously undetected subsurface voids of unknown dimensions. In the week following the collapse, approximately 200 water wells located within a 5-km radius of the WWTF were sampled in an after-the-fact, emergency sampling program. Twelve samples with elevated fecal coliform levels, 18 samples with nitrate-nitrogen greater than the 10 mg/1 standard, and no samples with elevated chlorides were found. However, the elevated levels could not be unambiguously attributed to the WWTF collapse. This is the third WWTF to fail by sinkhole collapse in southeast Minnesota since 1974. All three collapsed lagoons have been located in similar geomorphic and stratigraphic settings. However, at least two lagoons have collapsed in the adjacent area in northeast Iowa, and these lagoons are located at different stratigraphic positions. Twenty-two WWTFs constructed in southeast Minnesota's karst region in the last 25 years have been identified as subject to potential sinkhole collapse. An unknown but significant number of manure storage lagoons, flood control structures, etc., have also been constructed in the karst region and are at risk. Public agencies are beginning to develop plans to deal with the risk associated with existing and future waste lagoons in this environment. The critical hydrogeologic parameters that can be used to prioritize the risk of collapse at existing facilities include: (1) the lithology of the first bedrock beneath each lagoon, (2) the thickness of surficial materials between the lagoon and the bedrock surface, (3) the presence and construction of liners (seepage rate), and (4) the proximity to existing sinkholes.  相似文献   

19.
The Kuskokwim River at Bethel, Alaska, drains a major mercury-antimony metallogenic province in its upper reaches and tributaries. Bethel (population 4000) is situated on the Kuskokwim floodplain and also draws its water supply from wells located in river-deposited sediment. A boring through overbank and floodplain sediment has provided material to establish a baseline datum for sediment-hosted heavy metals. Mercury (total), arsenic, antimony, and selenium contents were determined; aluminum was also determined and used as normalizing factor. The contents of the heavy metals were relatively constant with depth and do not reflect any potential enrichment from upstream contaminant sources.  相似文献   

20.
滇东南锡、银、铅、锌多金属矿床主要分布在个旧、白牛厂、都龙3个矿区,而滇东南较大的3个花岗岩体又分别出露在3个矿区或附近.花岗岩体均形成于燕山晚期,岩石化学、矿物成分相似,富含锡、银、铅、锌、钨、铜等成矿元素.矿床主金属元素组合与岩体之间的距离由远而近出现由锡、钨、(铍、铌、钽)→锡、钨、(铁)、铜、铟→锡、铅、锌、银、铟、(锑)有规律的变化.花岗岩浆是成矿物质来源和成矿热源.岩浆侵入初期使上覆地层隆起产生背斜(凹陷部位成向斜);同时使地层产生一系列裂隙、压性断层或层间断裂;岩浆侵入晚期,这些断层再次活动,表现为张性,岩浆产生的含矿热液沿由其活动所造成的断裂迁移、充填、交代、沉淀而形成矿床.  相似文献   

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