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1.
建立了二氯甲烷溶剂辅助微波消解-电感耦合等离子体质谱法测定原油中V、Cr、Fe、Ni、Cu、Zn、Mo、Co、Pb等16种微量金属元素。研究表明,用CH2Cl2分散原油样品,以浓HNO3-H2O2为消解体系,采用CEM微波消解系统消解样品,各元素线性关系良好,相关系数≥0.9995;检出限可达ng/L;方法精密度较高,相对标准偏差(RSD,n=3)<5.0%;回收率为92%~110%。以w(Ni)/w(V)与w(Fe)/w(V)比值为变量参数对不同原油样品进行聚类分析,表明国内与国外不同地区原油样品中各金属元素含量差异较大。  相似文献   

2.
常量金野外快速分析方法   总被引:2,自引:0,他引:2  
1 方法提要 本法基于聚氨酯泡沫塑料对金具很强的吸附性,将现场采集的金矿样品经人工粉碎后,以HNO3-NaCl溶矿,聚氨酯泡沫塑料吸附金经灼烧,溶解后以氢醌滴定. 2 溶样条件试验: HNO3用量试验 称取GBW(E)70015标样10.0 g,固定加25% NaCl 100 ml,改变HNO3用量按本矿石分析手续操作,标样Au含量为10.0 g/t,试验说明选用15 ml HNO3较合适(表1).表1 硝酸用量 编号 1 2 3 4 5 HNO3 (ml) 5 10 15 20 30 Au(g/t) 6.4 8.6 9.7 9.8 9.6 NaCl用量试验 称取GBW(E)70015标样10.0 g加100ml水,固定加15 ml HNO3,改变NaCl用量,按本文矿石…  相似文献   

3.
新矿物——铊明矾   总被引:9,自引:1,他引:9  
铊明矾 (lanmuchangite ,TlAl[SO4]2 ·12H2 O)是在贵州滥木厂铊 (汞 )矿床富铊矿体氧化带中发现的一种铊的硫酸盐新矿物。该矿物为产于氧化带的次生矿物 ,其共生矿物为水绿矾、镁铝矾、钾明矾、黄钾铁矾、石膏、自然硫、砷华及某些未知矿物。其矿物集合体大小一般为 2~ 10mm ,集合体多为致密块状 ,单晶呈他形粒状 ,4 0~ 90 μm ,偶见平行柱状集合体 ,半自形至自形柱状晶体 ,直径 15~ 65 μm。白色至淡黄色 ,玻璃光泽 ,透明 ,易溶于水。偏光显微镜下无色 ,均质体 ,实测折光率为 1.4 95。维氏硬度为 94~ 12 4kg/mm2 ,摩氏硬度为 3 .1~ 3 .4 ,实测密度 2 .2 2 g/cm3。平均化学成分 :Tl2 O =3 3 .2 5 % ,Al2 O3=8.0 7% ,SO3=2 5 .19% ,SiO2=0 .10 % ,K2 O =0 .3 5 % ,CaO =0 .0 8% ,MgO =0 .0 6% ,FeO =0 .0 4 % ,H2 O =3 3 .4 6% ,总和 10 0 .60 % ,除结晶水由热重分析 (TG)求得 ( 3件样品平均 )外 ,其余成分均由电子探针分析 ( 6点平均 )求得。化学式为(Tl1.0 0 K0 .0 5) 1.0 5(Al1.0 1Si0 .0 2 Ca0 .0 1Mg0 .0 1Fe0 .0 1) 1.0 6 [SO4]2 .0 2 ·11.86H2 O ,理论式为TlAl[SO4]2 ·12H2 O。X射线粉末衍射主要强线 [d(I,hkl) ]为 :0 .4 3 14 ( 10 0 ,2 2 0 ) ,0 .2 80 1( 70 ,3 3 1) ,0 .70 3 ( 5 4 ,1  相似文献   

4.
阮琼  黄章杰  尹家元 《岩矿测试》2000,19(3):235-237
在pH为 2~ 3的HAc介质中 ,4 - ( 2 -羟基 - 4 -硝基苯偶氮 ) - 1 -苯基 - 3-甲基吡唑啉酮 (HNAPMP)与钍反应生成 2∶1的稳定络合物 ,λmax=540nm ,ε=4 .96× 1 0 4L·moL- 1·cm- 1,Th质量浓度在 0~ 2 .8mg/L内符合比尔定律。方法用于钍钨合金中钍的测定 ,相对标准偏差 (n =5)小于 1 % ,加标回收率为 97%~ 1 0 2 %。  相似文献   

5.
原子荧光光谱法测定地质样品中的痕量锗   总被引:7,自引:1,他引:7  
分析了溶矿过程中HNO3、H2SO4、HClO4、H3PO4等对Ge的影响,采用AgNO3滤气装置消除气相干扰,测定了地质样品中的痕量锗,方法检出限为0.06μg/g,用土壤国家一级标准物质GBW 07401~GBW 07408验证方法,结果与标准值相符,其相对标准偏差(RSD,n=12)为3.66%~6.11%。  相似文献   

6.
鲁东南岚山头榴辉岩的变质作用演化PTt轨迹及地质意义   总被引:10,自引:0,他引:10  
《岩石学报》1999,15(1):37-47
岚山头含柯石英榴辉岩呈透镜状块体产于晚元古代含霓石花岗质片麻岩中.榴辉岩的典型矿物平衡共生可划分为四个阶段:(1)前柯石英榴辉岩相阶段(M1);(2)柯石英榴辉岩相阶段(M2);(3)第一退变质阶段(M3);(4)第二退变质阶段(M4).M2阶段典型的矿物共生组合为石榴石+绿辉石+柯石英±蓝晶石.其石榴石中Pyr组分17.9%~31.7%, 绿辉石中Jd组分29.1%~52.8%.各阶段的变质温压条件是:M1阶段P≤1.56GPa,T=700℃;M2阶段P>2.74~2.95GPa,T=722℃~981℃;M3阶段P=1.34~1.54GPa,T=568℃~589℃;M4阶段P=0.61~1.04GPa,T=469℃.M2变质阶段单颗粒锆石207Pb-206Pb年龄为613.3Ma±30.4Ma,M4阶段的多硅白云母的 40Ar-39Ar坪年龄为313.49Ma.据上述资料可重塑一个较完整的顺时针PTt轨迹的变质作用演化.退变质作用的两个阶段反映榴辉岩折返可分为两个阶段.  相似文献   

7.
高压密闭罐溶样-氢化物原子荧光法测定环境样品中的硒   总被引:2,自引:0,他引:2  
使用浓HNO3 HF混合液和浓HNO3液分别在高压密闭罐中消解土壤、沉积物、岩石和植物样品,6 mol/L HCL加热还原样品后用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的硒.使用该法对土壤标准参考物质GSS-4、GSS-5、GSS-6、GSS-7和植物标准GSV-1、GSV-3进行了分析,硒的测定结果与推荐值一致.加标回收实验的回收率在98.0%~101.4%,平均为99.8%.实测样品中的硒与中子活化分析(NAA)和氢化物-多接受杯质谱计(HG-MC-ICP- MS)的分析结果基本一致,表明该法平行样的重现性好,分析速度快,提高了硒分析的准确度和分析精度.  相似文献   

8.
样品用HNO3-HCIO4-HF湿法消解,通过聚氨酯泡塑吸附,利用电感耦合等离子体质谱测定地球化学样品中的铊。通过实验确定了仪器最佳操作条件,同时选用铼作为内标元素,有效地监控和校正仪器信号的长期漂移,降低了基体效应的干扰。方法线性范围为0~2μg/mL,检出限为0.003μg/g,精密度(RSD,n=11)为2.50%~4.98%。该方法通过国家一级标准物质的验证,结果准确、可靠。  相似文献   

9.
偶氮氯膦—mA光度法测定铌   总被引:6,自引:0,他引:6  
研究了显色剂偶氮氯膦 -mA在酸性介质中与Nb(Ⅴ )的显色反应。在HNO3 介质中 ,阿拉伯树胶存在下 ,偶氮氯膦 -mA与铌形成 2∶1的络合物 ,其最大吸收波长为 63 0nm ,摩尔吸光系数为 9.0 9× 1 0 4L·mol-1·cm-1,铌的质量浓度在 0~ 0 .40mg/L符合比尔定律。试验了3 0多种共存离子的影响 ,结果表明大多数离子对测定铌无影响 ,且体系可允许 1 0余倍量的Ta(Ⅴ )存在。方法经标准样品分析验证 ,铌的测定结果与标准值相符 ,标样及样品分析的RSD≤7.3 % (n =8)。  相似文献   

10.
原子吸收光谱法测定茶叶中微量元素   总被引:2,自引:1,他引:1  
采用火焰原子吸收光谱法对江西庐山"云雾"茶叶中的铜、锌、锰、铁四种元素进行了含量测定,详细地研究了消解酸的种类、HNO3和HF的比例、消解酸的体积及消解时间对测定结果的影响.用HNO3-HF-HClO4处理样品,测定结果表明茶叶中含有丰富的人体必需的微量元素,采用此方法回收率为93.70%~102.40%,相对标准偏差小于10%.其方法简便、精密度和灵敏度高,结果令人满意.  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.
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   

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.
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   

15.
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   

16.
17.
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   

18.
《Applied Geochemistry》2001,16(2):137-159
Five hundred and ninety-eight samples of terrestrial moss (Hylocomium splendens and Pleurozium schreberi) collected from a 188,000 km2 area of the central Barents region (NE Norway, N Finland, NW Russia) were analysed by ICP-AES and ICP-MS. Analytical results for Al, B, Ba, Ca, K, La, Mg, Mn, Na, P, Rb, Si, Sr, Th, U and Y concentrations are reported here. Graphical methods of data analysis, such as geochemical maps, cumulative frequency diagrams, boxplots and scatterplots, are used to interpret the origin of the patterns for these elements. None of the elements reported here are emitted in significant amounts from the smelting industry on the Kola Peninsula. Despite the conventional view that moss chemistry reflects atmospheric element input, the nature of the underlying mineral substrate (regolith or bedrock) is found to have a considerable influence on moss composition for several elements. This influence of the chemistry of the mineral substrate can take place in a variety of ways. (1) It can be completely natural, reflecting the ability of higher plants to take up elements from deep soil horizons and shed them with litterfall onto the surface. (2) It can result from naturally increased soil dust input where vegetation is scarce due to harsh climatic conditions for instance. Alternatively, substrate influence can be enhanced by human activity, such as open-cast mining, creation of ‘technogenic deserts’, or handling, transport and storage of ore and ore products, all of which magnify the natural elemental flux from bedrock to ground vegetation. Seaspray is another natural process affecting moss composition in the area (Mg, Na), and this is most visible in the Norwegian part of the study area. Presence or absence of some plant species, e.g., lichens, seems to influence moss chemistry. This is shown by the low concentrations of B or K in moss on the Finnish and Norwegian side of the (fenced) border with Russia, contrasting with high concentrations on the other side (intensive reindeer husbandry west of the border has selectively depleted the lichen population).  相似文献   

19.
We have developed a set of four synthetic standards for the rare earth and high field strength elements designed for use in the determination of those elements in silicates. The base material is a glass nominally at the eutectic of the MgO-Al2O3-SiO2 ternary system. The nominal doping level was 2 wt% of the elements as oxides. To avoid problems associated with peak interference, the elements were doped in four separate glasses.  相似文献   

20.
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   

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