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本方法建立了以多硫化合物、多碘化合物为缓冲剂(液体缓冲剂),上电极为光谱纯石墨电极、下电极为光谱纯石墨加罩电极的方式,采用控制试样法绘制工作曲线,电弧发射光谱法同时测定区域地球化学样品中As、Sb、Bi、Cd、Tl、In等6元素的测定方法。方法检出限为As1.0μg/g,Sb0.2μg/g,Bi0.1μg/g,Cd0.05μg/g,Tl0.1μg/g,In0.01μg/g;精密度(RSD,n=12)为As8.36%,Sb7.17%,Bi7.60%,Cd7.39%,Tl7.13%,In6.76%。方法用于测定国家一级标准物质GSD-1～GSD-12中As、Sb、Bi、Cd、Tl、In,测定值与标准值或参考值吻合。通过对1:50000区域地球化学调查样品中As、Sb、Bi、Cd、Tl、In实际分析,结果成图效果良好,具有简便快捷、成本低、检出限低、精度高等特点。 相似文献
2.
以氢气发生器为氩-氢火焰提供纯净、稳定的氢气,原子荧光光谱法测定土壤中水溶态和可交换态Sb(Ⅲ)和Sb(Ⅴ)已有应用,本研究进一步将此方法用于测定土壤样品中的As(Ⅲ)和As(Ⅴ)。在0.3mol/L NaH2PO4-Na2HPO4缓冲液中,采用氢化物发生-原子荧光光谱法测定土壤中水溶态As(Ⅲ)和总砷的含量,通过差减法计算As(Ⅴ)的含量。实验考察了0.02～0.4 mol/L NaH2PO4-Na2HPO4对As(Ⅲ)和As(Ⅴ)测定的影响,结果表明0.3 mol/L NaH2PO4-Na2HPO4可以有效掩蔽As(Ⅴ)。As(Ⅲ)的检出限为2.92 ng/g,总砷的检出限为2.35 ng/g;As(Ⅲ)和As(Ⅴ)的加标回收率分别为96%～104%和101%～103%。本方法不再依靠化学反应产生氢气来点燃并维持氩氢火焰,可在发生氢化反应的任何介质中测定砷,且不需要考虑酸度问题。方法操作简便,准确度高,能满足大批量样品分析要求。 相似文献
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4.
电感耦合等离子体发射光谱法测定磷矿石中微量有毒元素铅砷镉 总被引：8，自引：6，他引：2
用电感耦合等离子体发射光谱法测定磷矿石中微量有毒元素铅、砷和镉,并对溶样条件及共存元素干扰和仪器工作条件进行了试验。方法检出限为Pb0.042mg/L、As0.053mg/L、Cd0.006mg/L;相对标准偏差为(RSD,n=11)Pb0.86%、As1.36%和Cd1.08%;回收率为Pb109.3%、As94.0%和Cd90.0%。方法用于分析磷矿石标准样品和出口磷矿石检验样,分析结果与其他方法一致,能够满足日常检验的要求。 相似文献
5.
土壤和水系沉积物地球化学样品经氢氟酸-硝酸-高氯酸敞开酸溶消解,王水提取,试液直接用高分辨率电感耦合等离子体质谱法(HR-ICP-MS)同时测定其中的Li、Be、P、Sc、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、Ga、Rb、Sr、Nb、Mo、Cd、In、Sb、Cs、Ba、Hf、Ta、W、Tl、Pb、Bi、Th、U、Na2O、MgO、Al2O3、K2O、CaO、TFe2O3等36种组分。对各元素的测定同位素及分辨率进行优选,有效消除了绝大多数多原子及双电荷离子干扰的影响。痕量元素的方法检出限(6σ)在0.002～2.031μg/g之间,主量元素的检出限(6σ)在10.0～100μg/g之间(稀释因子=1000),所有元素的相对标准偏差(RSD,n=12)均小于10%。方法经国家一级地球化学标准物质验证,测定值与标准值吻合。 相似文献
6.
氢化物发生原子荧光光谱法测定土壤中络合态锑 总被引：5，自引：0，他引：5
采用酒石酸作提取剂，氢化物发生原子荧光光谱法测定土壤中络合态Sb(Ⅲ）和Sb(Ⅴ）。研究了氢化物发生原子荧光光谱测定土壤中络合态Sb(Ⅲ）和Sb(Ⅴ）的浸提和还原条件及对测定结果的影响。Sb(Ⅲ）和总Sb检出限分别为0.11μg/L和0.09μg/L。相对标准偏差（RSD，n=11)分别为5.4%和6.1%，加标回收率在82.5%-101.9%。 相似文献
7.
冶炼副产品硫酸镍组成成分复杂,准确分析杂质元素As、Zn、Co含量对设计硫酸镍提纯工艺有重要意义。采用硝酸-盐酸-氢氟酸-高氯酸体系对样品进行前处理,优化仪器工作条件,建立了电感耦合等离子体发射光谱法(ICP-AES)测定冶炼副产品硫酸镍中As、Zn、Co的方法。本实验分别以As 189.042nm,Zn 206.200nm,Co 228.616nm为分析谱线。实验结果表明:待测溶液中20g/L硫酸镍基体及1g/L Cu、20mg/L Cd、Cr、Fe、Sb、Ca、Mg、Al、Mn、Sn、Bi等共存杂质元素对As、Zn、Co的测定结果基本无影响。As、Zn、Co的标准曲线线性相关系数均在0.9999以上,方法检出限为0.0021～0.026mg/L,方法定量限为0.0063～0.078mg/L。采用实验方法测定冶炼副产品硫酸镍实际样品中As、Zn、Co,所得结果的相对标准偏差(RSD,n=11)介于1.51%～2.77%之间,加标回收率在89.6%～108.4%之间。 相似文献
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提出了一种氢化物发生—原子荧光光谱法测定地质样品(水系沉积物)中Sb(Ⅲ)和Sb(Ⅴ)的方法.选取4.8 mol/L HC1为提取剂,采用超声波辅助提取,以6 g/mL柠檬酸钠作为Sb(Ⅴ)的掩蔽剂,在0.24 mol/L的HC1介质中选择性测定Sb(Ⅲ),用差减法求得Sb(Ⅴ).Sb(Ⅲ)的方法检出限为0.075×10-6,Sb(Ⅴ)的方法检出限为0.097×10-6.对40 ng/mL的Sb(Ⅲ)和Sb(Ⅴ)分别连续测定11次,得到相对标准偏差分别为1.1％和0.64％.应用该方法对地质样品中的Sb(Ⅲ)和Sb(Ⅴ)进行分析测定,并与王水溶解值相比较,该方法测定的总Sb提取率在80％以上,Sb(Ⅲ)和Sb(Ⅴ)的加标回收率分别为83％ ～ 107％和98％ ～ 114％. 相似文献
9.
电解二氧化锰废渣中的重金属元素在雨水淋滤下,通过地表径流对下游水生态系统及农业生态系统造成不同程度的环境污染和安全隐患,因此,准确测定电解二氧化锰废渣浸出液中的重金属元素含量具有重要的现实意义。电解二氧化锰废渣浸出液中的重金属元素含量通常很低,采用原子吸收光谱法、电感耦合等离子体发射光谱法测定,检出限通常难以满足测定要求。采用电感耦合等离子体质谱法(ICP-MS)测定,消除复杂质谱干扰面临挑战。本文采用电感耦合等离子体串联质谱(ICP-MS/MS)测定电解二氧化锰废渣浸出液中的重金属元素含量。电解二氧化锰废渣中6种重金属元素Cr、Ni、As、Cd、Hg、Pb经硫酸和硝酸混合酸浸出后直接采用ICP-MS/MS进行测定,利用串联质谱的O_2反应模式消除分析过程中Cr、Ni、As、Cd受到的质谱干扰,通过考察不同分析模式下~(52)Cr、~(60)Ni、~(75)As、~(111)Cd的背景等效浓度(BEC),评价质谱干扰对分析结果的影响。结果表明:在MS/MS模式下选择O_2为反应气,采用质量转移法和原位质量法可以消除~(52)Cr、~(60)Ni、~(75)As、~(111)Cd的所有质谱干扰。Cr、Ni、As、Cd、Hg、Pb检出限分别为3.06、9.31、3.50、2.72、2.03、1.89ng/L,加标回收率在95.6%～106.2%之间,相对标准偏差(RSD)≤3.9%。所建立的方法已应用于电解二氧化锰废渣浸出液中重金属元素的测定。 相似文献
10.
土壤中重金属有效态分析方法研究 总被引：2，自引：0，他引：2
土壤中重金属的不同形态决定了对于生物的有效性。自然界的重金属元素参与生态迁移能够被生物吸收利用的部分为生物有效态。土壤重金属可交换态的研究可以为其生物有效态研究提供参考。本文对于土壤中砷、汞、铬、镉、铅和铊的酸溶态、络合态和盐溶态这几种单一提取方式的可交换态的分析方法进行了研究比较,以其提取效率高的为有效态的表现方式,以p H值7.5为土壤酸碱度的界限,建立了土壤中的砷、汞、铬、镉、铅和铊在不同酸碱度下的分析方法。本方法的Cr的方法检出限为4.65ng/g;Cd的方法检出限为0.49ng/g;Pb的方法检出限为9.73ng/g;As的方法检出限为21.89ng/g;Hg的方法检出限为0.30ng/g;Tl的方法检出限为0.54ng/g。采用GBW7412,GBW7413,GBW7416这三个国家一级标准物质样品测得的方法精密度范围6.01%~19.3%。本方法适用于土地质量评估的要求。 相似文献
11.
David J. Grimes Walter H. Ficklin Allen L. Meier John B. Mchugh 《Journal of Geochemical Exploration》1995,52(3)
Ground-water, alluvium, and bedrock samples were collected from drill holes near the Chimney Creek, Preble, Summer Camp, and Rabbit Creek disseminated gold deposits in northern Nevada to determine if Au and ore-related metals, such as As, Sb, and W, are being hydromorphically mobilized from buried mineralized rock, and, if they are, to determine whether the metal-enriched ground water is reacting with the alluvial material to produce a geochemical anomaly within the overburden.Results of chemical analyses of drill-hole water samples show the presence of hydromorphic dispersion anomalies of Au, As, Sb, and W in the local ground-water systems associated with these deposits. Background concentrations for Au in the ground water up-gradient from the buried deposits was less than 1 nanogram per liter (ng/L), near the deposits the Au values ranged from 1 to 140 ng/ L, and in drill holes penetrating mineralized rock, concentrations of Au in the ground water were as high as 4700 ng/L. Highest concentrations of Au were found in ground-water samples where the measured Eh and the distribution of arsenic species, arsenite [As(III)] and arsenate [As(V)], indicated oxidizing redox potentials. Similarly, As, Sb, and W concentrations in the ground water near the deposits were significantly enriched relative to concentrations in the ground water up-gradient from the deposits. In general, however, the highest concentrations of As, Sb, and W occurred in ground-water samples where the measured Eh and the distribution of arsenic species indicated reducing conditions. Arsenic concentrations ranged from 9 to 710 micrograms per liter (μg/L); Sb, from less than 0.1 to 250 μg/L; and W, from 1 to 260 μg/L.In addition, analysis of sequential dissolution and extraction solutions of drill cuttings of alluvium and bedrock indicate geochemical anomalies of gold and ore-related metals in the overburden at depths corresponding to the location of the present-day water table. This relationship suggests that water-rock reactions around these buried deposits are active and that this information could be very useful in exploration programs for concealed disseminated gold deposits. 相似文献
12.
Concentrations of Au, Ag, As, Cd and Sb in aquatic bryophytes collected from the Dolgellau Mineral Belt, North Wales, U.K. are reported. One aquatic liverwort, Scapania undulata (L) Dum. and two mosses, Fontinalis squamosa Hedw. and Racomitrium aciculare (Hedw.) Brid. were collected from sites upstream and downstream of the recently reopened Gwynfyndd Au mine. There was little inter-species variation in metal contents for these three bryophytes, but Scapania undulata appeared the most sensitive to changes in water concentrations of Ag, As and Sb. Gold concentrations varied little between the contaminated and control sites. Concentrations in the range < 4–18 ng Aug g−1 D.W. were typical background levels, while bryophytes collected immediately below the mine contained 6–45 ng Au g−1. Silver and Sb both showed more pronounced ( 5–10 fold) elevations above control concentrations in samples collected downstream of the mine. Background concentrations for these elements were 5–85 ng Ag g−1 and 0.15–1.3 μg Sb g−1.Arsenic concentrations downstream of the mine (160–1080 μg g−1) greatly exceeded the background range of 9–32 μg g−1. It is suggested, therefore, that As may be an ideal ‘pathfinder’ element when prospecting for auriferous deposits using aquatic bryophytes. 相似文献
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Angela Johnson 《Geochimica et cosmochimica acta》2011,75(7):1773-1784
We investigate the degassing of volatile heavy metals from natural basalt and dacite and synthetic rhyolite melts doped with Bi, Pb, Tl, Au, Re, Sb, Sn, Cd, Mo, As, Cu in Pt capsules over a range of temperatures (1200-1430 °C) exposed to air at 0.1 MPa. We also investigated the effects of ligands on degassing by adding known concentrations of Cl and S. During the experiments concentration gradients normal to the melt/gas interface arose for the trace metals Au, Tl, As, Cd, Re, Bi and Pb, as shown by measurements by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) on the quenched glasses. In contrast, erratic concentration gradients occurred for Cu, Mo, Sn, Sb due to the development of compositional cords in the glass for those elements. The diffusivities for Au, Tl, As, Cd, Re, Bi and Pb (in decreasing order of volatility) followed an Arrhenius relationship with log D at 1260 °C varying from −12 to −17. The addition of Cl and S were shown to increase by two-to five-fold the volatilities of all metals, with S having a more profound effect. Diffusivities from the experiments were applied in a bubble growth model to examine the behavior of Tl and Pb in volcanic gases. The Tl/Pb ratio in gases shows much greater variation than can be explained by partitioning and magma composition alone, with diffusion serving to drastically enrich or deplete the Tl/Pb of gases to values significantly different from that of the melt. 相似文献
14.
氢化物发生-电感耦合等离子体发射光谱法同时测定土壤中痕量砷锑铋汞 总被引：4，自引：4，他引：0
土壤样品用水浴加热王水溶解1 h,在10%的盐酸介质下,用0.5 L/min的载气流量,10 g/L的硼氢化钠-氢氧化钠作为还原剂,将自行设计的一种新型氢化物发生器与电感耦合等离子体发射光谱法(ICP-AES)联用测定痕量砷、锑、铋、汞,一次溶样即可实现多元素在同母液同条件下同时测定。方法检出限为0.01～0.06 ng/g,加标回收率为92.0%～102.0%,精密度(RSD)低于5%。此方法通过加入抗坏血酸-硫脲溶液预先将砷和锑还原,汞的测定不受还原剂的影响,同时解决了目前多元素分次测量带来的不便和试剂消耗多等问题,样品前处理及测量过程快速、简单,无记忆效应的影响,适合环境样品中痕量砷、锑、铋、汞的同时测定。 相似文献
15.
Analytical data are reported for As, Bi, Sb, Se and Te in fifty five geological reference materials (RM). The method used is based on hydride generation inductively coupled plasma-mass spectrometry (HG-ICP-MS) following digestion of the samples in the mixed acid attack of HF-HClO4-HNO3-HCl. Analytes were separated from potential interferences by coprecipitation with La(OH)3. This scheme results in method detections limits of: 1 ng g?1 for Bi and Te; 6 ng g?1 for Sb and Se; and 10 ng g?1 for As. The average relative standard deviation (RSD) for three 0.5 g subsamples of each RM analysed by this method are: 3.7% for As in the range 0.35-187 μg g?1; 5.6% for Sb in the range 0.03-22 μg g?1; 6.8% for Bi in the range 0.002-48 μg g?1; 7.2% for Se in the range 6-3610 ng g?1; and 9.0% for Te in the range 2-445 ng g?1. 相似文献
16.
云浮黄铁矿利用过程中微量毒害元素的环境化学活动性 总被引：13，自引：3，他引：13
为了解云浮黄铁矿利用过程中微量毒害元素的环境地球化学行为，客观评价它们对环境质量的影响，利用元素结合形态的连续提取实验方法，分析了云浮黄铁矿及其工业废渣中Co,Ni,Cu,Zn,As,Se,Cd,Sn,Sb,Pb和Tl等11种毒害元素的形态及化学活动性。结果表明，黄铁矿中大部分微量毒害元素都有着极强的化学活动性，各元素活动态浸出比例依次为Co96.3%,Se91.9%,Cu90.3%,Cd90.0%,Pb89.7%,Zn88.6%,Sb82.5%,Ni80.6%，Sn70%,Tl55.1%和As31.9％，元素As和Tl主要赋存于硫化物和硅酸盐矿物相中，另有少量的Cu,Pb和Sb可能赋存于碳酸盐矿物相中，其他元素则主要赋存于硫化物矿物相中。与黄铁矿相比，飞灰和灰渣中各元素可交换态和碳酸盐结合态所占的比例明显减少。废渣中各元素的化学活动性表现出很大的差别，其中Cu,Zn和Cd的化学活动性最强，活性态浸出比例在90％以上；其次是Co,Ni,Se,Pb和Tl，浸出比例在50％左右；Sb,As和Sn的稳定性较高，浸出比例分别为1％、5％和14％左右；飞灰中微量毒害元素的活动性均高于灰渣。 相似文献
17.
Raimundo Jiménez Ballesta Paz Conde Bueno Juan A. Martin Rubi Rosario Garcia Giménez 《Central European Journal of Geosciences》2010,2(4):441-454
To evaluate trace element soil contamination, geochemical baseline contents and reference values need to be established. Pedo-geochemical baseline levels of trace elements in 72 soil samples of 24 soil profiles from the Mediterranean, Castilla La Mancha, are assessed and soil quality reference values are calculated. Reference value contents (in mg kg?1) were: Sc 50.8; V 123.2; Cr 113.4; Co 20.8; Ni 42.6; Cu 27.0; Zn 86.5; Ga 26.7; Ge 1.3; As 16.7; Se 1.4; Br 20.1; Rb 234.7; Sr 1868.4; Y 38.3; Zr 413.1; Nb 18.7; Mo 2.0; Ag 7.8; Cd 4.4; Sn 8.7; Sb 5.7; I 25.4; Cs 14.2; Ba 1049.3; La 348.4; Ce 97.9; Nd 40.1; Sm 10.7; Yb 4.2; Hf 10.0; Ta 4.0; W 5.5; Tl 2.3; Pb 44.2; Bi 2.2; Th 21.6; U 10.3. The contents obtained for some elements are below or close to the detection limit: Co, Ge, Se, Mo, Ag, Cd, Sb, Yb, Hf, Ta, W, Tl and Bi. The element content ranges (the maximum value minus the minimum value) are: Sc 55.0, V 196.0, Cr 346.0, Co 64.4, Ni 188.7, Cu 49.5, Zn 102.3, Ga 28.7, Ge 1.5, As 26.4, Se 0.9, Br 33.0 Rb 432.7, Sr 3372.6, Y 39.8, Zr 523.2, Nb 59.7, Mo 3.9, Ag 10.1, Cd 1.8, Sn 75.2, Sb 9.9, I 68.0, Cs 17.6, Ba 1394.9, La 51.3, Ce 93.5, Nd 52.5, Sm 11.2, Yb 4.2, Hf 11.3, Ta 6.3, W 5.2, Tl 2.1, Pb 96.4, Bi 3.0, Th 24.4, U 16.4 (in mg kg?1). The spatial distribution of the elements was affected mainly by the nature of the bedrock and by pedological processes. The upper limit of expected background variation for each trace element in the soil is documented, as is its range as a criterion for evaluating which sites may require decontamination. 相似文献
18.
Thirty-four springs were sampled on five different source rocks in the upper Ecker watershed of the Northern Harz Mountains (Germany) four times during the course of 1995. The analyses included 41 cations and the major anions. Approximately 90% of the rocks in the upper Ecker watershed are low in basic cations, which inhibit the neutralisation of hydrogen-ion loading. As a consequence, the concentrations of Al, Fe, Mn, Zn, Pb, Y, Ce, As, La, Nd, Cd, Be, Co, Sb, Pr, Gd, Dy, Yb, Er, Sm, U, Tl, Ho and Tb of the Ecker dam water (pH=5.1) exceed those of the nearby Söse Dam water (pH=6.5) by almost one order of magnitude or more. With the exception of the spring waters on gabbro (pH up to 7.7) all waters on the highly siliceous rocks (quartzite, granite and gneiss) are dominated by sulfate anions with a pH range of 4–6. The concentrations of major conservative ions show a progressive increase with decreasing catchment elevation and decreasing average precipitation. Trace elements such as Sr, Be, Zn, Cd, Ba, Y, La, lanthanides, U, Li, Ni, Al, Mn, Co, Cu, Pb, As, Sb and Tl are increased in the low acid neutralizing capacity (ANC(aq)) spring waters. The behaviours of Sr, Be, Zn, Cd, Ba, Y, La, lanthanides and U resemble that of the major cations. The highest concentrations of Li and Ni are found on quartzite. Al, Mn, Co and Cu exhibit no clear correlation with catchment elevation and one particular bedrock. The concentrations of V and Cr show a distinct increase in high ANC(aq) spring waters on gabbro. Pb, As, Sb and Tl are characterized by being found in relatively high concentrations on granite at higher altitudes. Pb, As and Sb are affected by contaminated soils. The extreme variability of trace element concentrations of low ANC(aq) spring waters cannot be explained by the rock data. It is mainly controlled by the topography-dependent weathering rates of the different rock-types and the decreasing dilution with decreasing catchment elevation. 相似文献