共查询到20条相似文献，搜索用时 54 毫秒
1.
目前,广泛应用于大量区域化探样品分析的电弧水平电极撒样法光谱半定量分析,具有快速简便、易挥发和中等挥发元素的分析灵敏度高、重现性好等优点,但对一些难激发元素的测定灵敏度低、重现性差和受基体成分影响大。为克服这些缺点,我们制定了交流电弧-低压火花水平撒样法,其灵敏度列于表1。 相似文献
2.
地质化探试样中微量钨钼的光谱定量测定 总被引：1，自引：0，他引：1
发射光谱法直接测定地质比探试样中钨的灵敏度较低,一般为3—5ppm,不能满足地质化探佯品分析的要求。本方法采用高浓度的氯化镉溶液代替固体粉末缓冲剂滴加于装样电极头上来处理试样,利用大量镉盐的蒸发控制电弧温度,致使W、Mo和其它难挥发元素分馏和Cl~-在电极中辅以一定的氯化作用的办法,有效地改善了W、Mo等元素的蒸发行为,降低了光谱背景,将两元素 相似文献
3.
植物样品中无机元素分析的样品前处理方法和测定技术 总被引：11，自引：5，他引：6
植物样品中无机元素的分析测定在环境地球化学和生物地球化学的研究中起着重要作用。植物样品中元素含量一般较低,须选用科学合理的前处理技术和灵敏度高、精密度好、检出限低的测定方法。本文针对植物样品前处理方法和无机元素分析测定技术的研究进展、优势与不足进行评述。前处理方法主要根据样品和待测元素的性质进行选择:干法灰化所用试剂少、空白值低,但组织致密型的样品不易灰化完全、高温下易造成元素挥发损失;湿法消解样品消解较为完全,但试剂消耗大、空白值高、操作繁琐;微波消解可以防止部分易挥发元素损失,用酸量少、消解速度快,但称样量相对较小,不适于需要大称样量的样品分析。几乎所有针对元素分析的仪器分析技术都可以用于植物样品分析,主要根据仪器适用的元素、必要的干扰校正以及基体改进等方面进行选择:电感耦合等离子体质谱法可同时测定植物样品中40种以上的元素,高分辨质谱的检出限可达fg/mL;电感耦合等离子体发射光谱法适用于某些植物样品中含量较高的P、K、Na等元素的测定;原子吸收光谱法可分析元素达70余种,是普及程度最高的仪器分析技术之一;原子荧光光谱法与氢化物发生技术的联用,在元素含量较低的植物样品分析中技术优势更加明显;新兴的激光诱导击穿光谱技术已被应用于植物样品分析,无需复杂的样品前处理,操作简单快速,可实现原位、在线、实时、多元素同时检测;其他选择性强、灵敏度高的分析技术,满足了一些特定元素不能用常规分析技术测定的需求。当前主流分析技术的样品前处理方法都存在着缺陷,固体进样技术将成为植物样品分析领域的发展方向之一。 相似文献
4.
本法是在样品中加入适量的缓冲剂,使难发挥元素Be形成易挥发的氟化物,与B、Pb、Mo、Sn、Cu、Ag、Zn等元素在同一时间内蒸发,利用深电孔极的分馏效应,有效地降低光谱背景以及被测元素的检出限。加入内标元素,提高了方法的准确度和精密度。采用深孔电极,取样量大,代表性好。一次摄谱,同时检测多个元素,大大提高了工作效率,又减少了测试费用。方法操作简便,适合于大批量样品的测试。检出限ω(B)/10-6分别达到:Be:0.50、B:0.91、Sn:0.50、Ag:0.02等,均满足《覆盖区多目标地球化学调查样品测试及质量监控暂行规定》规定。 相似文献
5.
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
6.
7.
电感耦合等离子体质谱法(ICP-MS)测定化探样品中的Ag时,由于受到Zr、Nb氧化物离子91Zr16O和93Nb16O的严重干扰,直接测定时低含量Ag的分析结果误差较大,需要将干扰元素分离才能得到较准确的结果。当前应用P507萃淋树脂分离样品溶液中Zr和Nb等干扰元素已经成功应用于化探样品中Ag的测定。本文将此方法进一步改进,用氢氟酸、硝酸、高氯酸和逆王水敞开溶样,通过P507负载泡塑进行振荡吸附,实现了化探样品中Ag和内标元素Rh与干扰元素Zr的有效分离,应用ICP-MS可同时测定Ag、W和Mo。标准样品的测定结果准确可靠,方法检出限为Ag 0.0045μg/g,W 0.023μg/g,Mo 0.060μg/g,均低于多目标地球化学调查(1∶250000)样品分析的检出限。P507负载泡塑分离流程操作简便,无交叉污染,一次振荡可处理100件样品,其分析效率显著优于P507萃淋树脂交换柱,更加适合大批量化探样品Ag与W、Mo及微量元素的同时测定。 相似文献
8.
E5000型全谱直读型电弧发射光谱仪研制及其在地球化学样品分析中应用 总被引：2，自引：2，他引：0
在地球化学样品检测工作中,Ag、B、Sn等难分析元素通常采用传统的交流电弧发射光谱法(摄谱仪),随着地球化学样品数量的增加以及对检测结果质量要求的提高,该方法操作复杂、分析过程繁琐的问题与日常大量样品分析的矛盾日益突出,多道式电弧直读发射光谱也开始在行业内应用。本文基于先进的数字光源技术和CCD全谱型光谱仪技术,改进了电弧发生系统、分光系统和检测系统,将电弧激发光源与Paschen-Runge型全谱CCD光谱仪结合,研制了一款新型的台式全谱直读型电弧发射光谱仪E5000。E5000型电弧发射光谱仪通过激光定位结合程控电极技术,自动调整电极位置,提高了采谱过程的精度控制;利用CCD全谱技术获得了激发样品的全谱信息,可轻易实现光谱信号的背景扣除和干扰校正;且无需再次测定黑度,直接获得分析结果;同时结合内标法和标准加入法,可以进一步提高复杂基体样品的分析精准度。应用研制的光谱仪对水系沉积物和土壤样品进行检测,Ag、B、Sn元素的检出限分别达到了0.01μg/g、0.65μg/g、0.16μg/g,在分析水系沉积物、土壤时检测精密度基本小于10%,优于当前的摄谱法和多道电弧直读光谱法,满足了地球化学样品检测质量要求。 相似文献
9.
X射线荧光光谱法(XRF)已经应用于石膏等非金属矿物的测定,但由于石膏标准物质匮乏、硫含量较高且在高温易挥发损失,给测定带来了一定困难。本文采用石膏标准物质、高纯硫酸钙和其他国家一级标准物质(土壤、水系沉积物、碳酸盐)配制人工标准物质拟合校准曲线,优化稀释比、熔矿温度等熔融制样条件,用理论α系数校正基体效应,建立了采用XRF同时测定石膏矿中10个主次量元素(硅铝铁钙镁钾钠钛硫锶)的分析方法。样品与四硼酸锂-偏硼酸锂熔剂的稀释比为1∶9,在1050℃温度下样品熔融完全。方法检出限为4~135μg/g,精密度(RSD,n=12)小于3.0%。本方法配制的人工校准样品加强了样品基体的适应性,使用的四硼酸锂-偏硼酸锂熔剂在样品熔融过程中可有效地结合硫,抑制了硫的挥发损失,适用于批量分析硫含量高达12.60%~51.91%的实际石膏矿物。 相似文献
10.
11.
Heating experiments relevant to the depletion of Na,K and Mn in the Earth and other planetary bodies
《Chemie der Erde / Geochemistry》2019,79(4):125540
We have studied the evaporation of Na, K and Mn from Al-Na-K- and Mn-rich silicates at various conditions. Total alkali oxide contents ranged from 5 to 20%. The evaporation rate of Na increases with temperature and decreasing oxygen fugacity and decreases with duration of heating. The loss of K is in all cases less pronounced than for Na. Heating in an evacuated vacuum furnace is more effective in removing Na and K from melt droplets than in furnaces with one atm gas flow of air or gas mixtures controlling the oxygen fugacity. The strong pumping required to keep the vacuum removes Na and K atoms very effectively. In all experiments, the rate of evaporation is determined by quasi-equilibrium between a thin layer of Na and K rich gas above the molten silicates. The results of the experiments are in agreement with several other studies.In experiments with more than one sample in the furnace, equilibration of Na- and K-rich samples with Na- and K-poor samples occurred rapidly, mediated by the ambient gas phase.The results of experiments with Mn in starting compositions showed much stronger losses of Na than Mn under a variety of conditions.Thus the nearly chondritic Mn/Na ratios in the Earth cannot be the result of evaporation of Na and Mn in Earth-making materials, as the Mn/Na ratios in evaporation residues would be much higher than chondritic ratios. Such evaporation processes may have occurred in the parent material of Moon, Vesta and Mars.The data suggest, in agreement with earlier hypotheses, that the high and variable contents of Na and K in chondrules require a gas phase high in Na and K equilibrating with chondrule melts. The volume of nebular gas parental to a certain type of chondrites was heated and Na and K were lost from the chondrule precursors to the gas phase. Subsequently the nebular parcel was compressed leading to higher partial pressures of Na and K. Flash heating then produced chondrule melts which incorporated some of the gaseous Na and K and then cooled rapidly. The large range of Na and K contents in chondrule melts reflects very local enrichments of Na and K in the gas phase. Despite these variations bulk chondritic meteorites have well defined bulk Na and K contents, implying a closed system during formation of chondrules and matrix. 相似文献
12.
Some Observations on the Determination of Gold and the Platinum-Group Elements in Black Shales 总被引：2，自引：0，他引：2
Valentin N. Mitkin Alexander A. Galizky Tamara M. Korda 《Geostandards and Geoanalytical Research》2000,24(2):227-240
This research compares various ways of applying oxidative chemical decomposition to the analysis of gold-bearing black shale ores from the Russian Natalka and Sukhoj Log deposits. This study was conducted as part of the certification program for the Russian candidate black shale reference materials SLG-1 and SCHS-1 and also because of the paucity of data available on the determination of the platinum group elements (PGE) in analogous sample types. We report direct evidence of PGE volatilisation from black shale materials when processed in the presence of oxygen. We also developed a comprehensive analytical scheme for the quantitative determination of PGE in all phases (gaseous and ash) produced during slow combustion of carbonaceous materials in oxygen.
This study has shown that during combustion in oxygen at 600 °C, PGE contained in the Natalka black shale ores are lost as gaseous reaction products. Thus, the volatilized PGE (recovered in traps) account for up to 14% Pt, 40% Pd, 40% Ru and 10 % Ir relative to their total concentrations in a carbonaceous concentrate. It was also established that in the process of combustion, Au quantitatively remains in the ash cake.
In order to avoid the deleterious effects of oxygen on the volatility of the PGE, we propose a new comprehensive sample decomposition method based on the application of fluoroxidants such as BrF3 and KBrF4 . This method was validated using samples of black shale ores and their processing products by comparing our results with those obtained independently using sealed autoclave processing of the same materials. It was shown that PGE in black shale ores and their processing products not only exist in commercially exploitable quantities but that a small proportion of PGE compounds are soluble in alcohol. We propose that in gold-bearing black shale ores, PGE are present as organometallic compounds. 相似文献
This study has shown that during combustion in oxygen at 600 °C, PGE contained in the Natalka black shale ores are lost as gaseous reaction products. Thus, the volatilized PGE (recovered in traps) account for up to 14% Pt, 40% Pd, 40% Ru and 10 % Ir relative to their total concentrations in a carbonaceous concentrate. It was also established that in the process of combustion, Au quantitatively remains in the ash cake.
In order to avoid the deleterious effects of oxygen on the volatility of the PGE, we propose a new comprehensive sample decomposition method based on the application of fluoroxidants such as BrF
13.
富锂氟含稀有矿化花岗质岩石的对比和成因思考 总被引：31，自引：5，他引：31
Li-F花岗质岩石以超酸性、过铝、富含H2O、F、B、P等挥发性组分和富含Li、Rb、Cs、Be、Ta、Nb、Sn、W等亲石稀有金属元素为主要特征，以黄玉－锂云母－钠长石花岗岩为典型代表。从该类岩石地质产状的多样性和可对比性、空间分布的规律性、矿物岩石的结构构造、硅酸盐－熔体包裹体特征以及实验岩石学的研究成果等方面，综合论证该类岩石主要是从经过分异演化而形成的残余熔浆中直接结晶而在的；充分的分离结晶作用，是产生这种残余熔浆的主要机制；岩体的空间分带特征和各带之间的渐变过渡关系，为分离结晶作用的途径和演化方向提供了重要信息；熔体中挥发性组分的大量存在，是分离结晶作用能充分进行的关键因素；亲石稀有金属元素在流／熔配分中倾向于进入熔体相，是残余熔体中逐步富集这些稀有金属元素的主要原因；岩浆－热液过渡阶段出溶的流体相与已晶出的共存固相之间的相互作用，造成了广泛的交代蚀变现象；残余熔浆在不同地质和物理化学环境中的侵位、结晶和演化，造成了Li-F花岗质岩石在产状、结构构造和矿物组合等方面的多样性。 相似文献
14.
Antonella Buccianti 《Mathematical Geology》1997,29(3):349-359
Chlorine concentration has been determined by chemical methods in 97 samples of basic rocks collected at Etna volcano (Sicily,
Southern Italy), Sao Miguel (Azores Islands), and Lanzarote (Canary Islands). The samples have been processed together with
data related to specific magmatic and tectonic conditions, drawn from the literature. Thus, the contents of SiO2, K2O, and P2O5 of 228 samples have been used to investigate Cl distribution in the considered environments, using principal component analysis.
The log-centered variance-covariance matrix has been processed in order to overcome the closure constraints. The results indicate
that a clear distinction between continental and oceanic regions can be obtained in the components space. A preliminary discriminant
diagram involving chlorine thus can be proposed. 相似文献
15.
This paper reviews several bolt numerical simulating methods which are being used at present, and does a special research to the theory and applicability of the three-dimensional bolt elements which takes the tangential mechanics properties of the grout into account. By means of the FEM and the models mentioned，the program is developed to simulate the bolt and the structure. Through an example, it make sspecial research on bolt’s mechanical characteristics. The calculations illustrate the capabilities of the elements. 相似文献
16.
Geochemistry and origin of elements in some UK coals 总被引：3，自引：0，他引：3
Twenty-four UK coals ranging in rank with 4.6%–37.6% volatile matter were analysed for 46 major and trace elements. The samples were obtained from the UK Coal Bank and are representative of the major UK coal fields. The major element distributions are interpreted in terms of the mineralogical variations—quartz and kaolinite are largely responsible for the Si and Al, carbonates for Ca and Mg and pyrite for Fe. Also exerting an influence in some samples are siderite, Al-phosphate minerals and illite. Based on statistical relationships with the major elements, Rb, Cr, Th, Ce, Zr, Y, Ga, La, Ta, Nb and V are thought to be mainly present in the clay minerals, and As, Mo, Sb, Tl, Se and Bi and Pb are probably present in pyrite. Strontium and Ba are concentrated in a restricted number of samples related to the phosphate minerals. Germanium is the only element for which a major organic association can be demonstrated. Elements with an indirect association with the organic matter are Na, Cl, and Br in porefluids and possibly Te. The ash content is controlled mainly by the detrital input and the trace elements related to the ash content are therefore those elements associated with the clay minerals. Variations with rank would appear to be mainly related to the moisture content (porefluids). The trace elements associated with the quartz and clay minerals are thought to be dominantly detrital in origin. The non-detrital elements, essentially those contained in pyrite, are thought to have been incorporated in the depositional environment from waters with enhanced salinities through seawater ingress, hence there are positive relationships between S and trace element concentrations. 相似文献
17.
18.
19.
Chemical Analysis of Iron Meteorites by Inductively Coupled Plasma-Mass Spectrometry 总被引：2，自引：0，他引：2
Iron meteorites were analysed for nineteen siderophile and chalcophile elements by conventional inductively coupled plasma-mass spectrometry with the specific aim of demonstrating that this technique is an effective alternative to the more routine, yet complex, methodologies adopted in this field such as instrumental or radiochemical neutron activation analysis. Two aliquots of each meteorite sample, in the form of small shavings, were dissolved, one in 6 mol l-1 HNO3 and the other in aqua regia , and diluted to a final concentration of 1 mg sample per 1 ml of solution, without pre-concentrating the analytes. Nitric acid solutions were used for the determination of the elements Cr, Co, Ni, Cu, Ga, Ge and As; aqua regia solutions were analysed for the elements Mo, Ru, Rh, Pd, In, Sn, Sb, W, Re, Ir, Pt and Au. Samples were analysed by external calibration, carried out using synthetic multi-elemental solutions, and internal standardisation (with Be, Rb and Bi selected as internal standards). The results obtained from the analyses of nine geochemically well-characterized iron meteorites (Canyon Diablo, Odessa, Toluca, Coahuila, Sikhote-Alin, Buenaventura, Tambo Quemado, Gibeon, NWA 859) with widely variable chemical compositions are in good agreement with literature values for most elements. Detection limits were generally below the lowest concentration observed in iron meteorites. The most notable exception is for Ge, which cannot be successfully determined in the low-Ge meteorites of groups IVA, IVB and IIIF and a number of ungrouped irons. A test of the overall reproducibility of the adopted method, undertaken by repeatedly analysing the same Odessa IAB meteorite specimen, yielded relative standard deviations (1 s ) of between 1 and 6% for all elements except Cr (40%). 相似文献
20.
G. J. Chakrapani 《Environmental Geology》2005,48(2):189-201
Chemical weathering and resulting water compositions in the upper Ganga river in the Himalayas were studied. For the first time, temporal and spatial sampling for a 1 year period (monthly intervals) was carried out and analyzed for dissolved major elements, trace elements, Rare Earth Elements (REE), and strontium isotopic compositions. Amounts of physical and chemical loads show large seasonal variations and the overall physical load dominates over chemical load by a factor of more than three. The dominant physical weathering is also reflected in high quartz and illite/mica contents in suspended sediments. Large seasonal variations also occur in major elemental concentrations. The water type is categorized as HCO3––SO42––Ca2+ dominant, which constitute >60% of the total water composition. On an average, only about 5–12% of HCO3– is derived from silicate lithology, indicating the predominance of carbonate lithology in water chemistry in the head waters of the Ganga river. More than 80% Na+ and K+ are derived from silicate lithology. The silicate lithology is responsible for the release of low Sr with extremely radiogenic Sr (87Sr/86 Sr>0.75) in Bhagirathi at Devprayag. However, there is evidence for other end-member lithologies for Sr other than carbonate and silicate lithology. Trace elements concentrations do not indicate any pollution, although presence of arsenic could be a cause for concern. High uranium mobilization from silicate rocks is also observed. The REE is much less compared to other major world rivers such as the Amazon, perhaps because in the present study, only samples filtered through <0.2 m were analysed. Negative Eu anomalies in suspended sediments is due to the excess carbonate rock weathering in the source area. 相似文献