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氢化物发生-原子荧光光谱法测定地球化学样品中痕量碲 总被引:4,自引:4,他引:4
采用焙烧富集分离地球化学样品中痕量Te,并用氢化物发生原子荧光光谱法测定。通过实验确定出方法的最佳实验条件,在此条件下获得的检出限为0.005μg/g,线性范围0.025~10μg/g,精密度(RSD,n=8)为5.03%~9.24%。方法已用于国家一级地球化学标准物质中痕量Te的测定,结果与标准值基本相符。 相似文献
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氢化物发生-原子荧光光谱法直接测定多金属矿中的硒和碲 总被引:8,自引:4,他引:4
用硝酸-氢氟酸-高氯酸分解多金属矿物样品,在6 mol/L盐酸介质中,以Fe3+盐为减缓剂,直接在双道原子荧光光度计上同时测定多金属矿中硒和碲。该方法用同一混合酸一次分解样品,不经分离富集,同时测定硒和碲,过程简单快捷,适合于批量样品的检测。将样品与标准曲线同时分解至冒高氯酸白烟,从而准确地测定多金属矿物样品中硒和碲的含量。方法检出限为硒0.032μg/g,碲0.023μg/g;方法精密度(RSD,n=8)为硒<4.0%,碲<7.0%。经国家一级标准物质GBW 07283、GBW 07233、GBW 07234验证,硒和碲的测定值与标准值吻合。 相似文献
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用冷蒸气原子荧光法测量地球化学样品中痕量汞,对载气流量、试液酸度、硼氢化钾浓度等进行了试验。工作曲线线性范围为0~4μg/L,方法检出限为0.002 3μg/g,精密度RSD%为1.1~5.0。方法用国家一级地球化学标准物质中汞的测定,结果与标准值一致。 相似文献
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蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇 总被引:1,自引:1,他引:0
建立了蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇的分析方法。进行了蒸馏温度和时间、氧化剂、吸收液等条件的选择,消除了等离子体质谱法测定钌和锇的干扰。样品用过氧化钠熔融,酸化后以高锰酸钾-过硫酸钾-氯化钠作为同时蒸馏钌和锇的氧化剂,采用20 mL 50 g/L水合肼溶液同时吸收从混合物中分离出来的痕量钌和锇,用电感耦合等离子体质谱法测定。方法的检出限Ru为0.020 ng/g,Os为0.015 ng/g;方法加标回收率Ru为94.0%~102.7%,Os为96.0%~102.4%;精密度为4.72%~9.58%(n=12)。方法经国家一级标准物质验证,钌和锇的测定结果与标准值相符。 相似文献
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建立了HF—HN03密封酸溶以及Na2O2熔融处理样品,乙醇增强灵敏度,电感耦合等离子体质谱直接测定地质样品中微量和超痕量碲的方法。样品溶液中加入乙醇(φ=4%),在0.85L/min的载气流速下,碲信号可增强2.5倍以上。碲的方法检出限(100,DF=1000)为0.02μg/g。用土壤和水系沉积物国家一级标准物质验证了方法的准确度,标准物质的绝大多数分析结果与标准值的误差在允许范围内。分析了大洋多金属结核样品及深海沉积物样品中的微量碲,结果与其他方法相符,精密度试验RSD(n=3)<10%。 相似文献
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氢化物-无色散原子荧光光谱法测定黄铁矿及地球化学样品中微量碲,采用硝酸,盐酸,高氯酸分解样品,用浓盐酸将六价碲还原成四价碲,再用硼氢化钾继续还原使碲形成氢化物TeH2,在AFS1201C原子荧光光谱仪进行测定碲的检示限为0.18μg/g精密度RSD%为6.8%,该方法操作简便,快速,准确,费用低,可应用于大批量地球化学样品的分析。 相似文献
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动能歧视模式ICP-MS测定地球化学样品中14种痕量元素 总被引:5,自引:4,他引:1
应用传统ICP-MS法测定勘查地球化学样品中Ag、Cd等痕量元素,基体效应和多原子离子干扰严重,准确测定的难度较大。本文基于当前ICP-MS消除干扰技术,分析了ICP-MS标准模式(STD)及动能歧视模式(KED)测定地球化学样品中Ag、Cd等14种痕量元素的有效性,通过比较这两种模式的测定效果,在此基础上确定了各元素的有效测定模式。结果表明:在KED模式下,基体元素如Zr、Nb氧化物的产率降低,基本上消除了Zr、Nb氧化物对痕量元素Ag、Cd的多原子离子干扰。KED模式提高了信噪比,降低了方法检出限,如Ag、Cd的检出限分别为0. 004mg/kg、0. 005mg/kg,其他12种元素的检出限也低于多目标地球化学调查76种元素分析方案中的检出限。测定痕量元素的准确度显著优于STD模式。实验中采用简单的硝酸-氢氟酸-高氯酸消解样品,残渣用王水复溶,结合KED模式下优选出干扰较小的同位素作为测定同位素,以Rh作为内标校正仪器产生的信号漂移,将样品溶液稀释至1000倍,基体效应降低至最小。本方法经国家一级标准物质的验证,测定结果与认定值相符,可为勘查地球化学提供高质量数据。 相似文献
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抗坏血酸为基体改进剂石墨炉原子吸收光谱法测定金矿区植物样品中的痕量金 总被引:3,自引:3,他引:0
应用石墨炉原子吸收光谱法(GFAAS)测定地球化学样品中的低含量金具有较高的准确度,但用于测定植物样品中痕量金时,传统方法的称样量较大(20 g),样品在马弗炉中灰化不完全,检出限较高(0.29ng/g)。本文确定了应用GFAAS分析金矿区植物样品中痕量金的测定条件,石墨炉的升温程序为:金的灰化温度1000℃,原子化温度2000℃,以抗坏血酸为基体改进剂,瓷坩埚为灰化器皿,且将样品的灰化温度降低到500℃,灰化时间2.0 h,确保了样品灰化完全且待测元素不发生挥发损失。本方法称样量较小(5.0 g),检出限为0.03 ng/g,精密度为6.8%~11.9%,加标回收率为83.8%~104.7%。经过金矿区实际植物样品试验,发现不同植物对金的富集能力相差较大,其中玉米植株对金的富集能力强。 相似文献
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电感耦合等离子体质谱法直接同时测定地球化学样品中镓铟铊 总被引:6,自引:7,他引:6
报道了用HF—HNO3—HClO4分解样品,以^103Rh为内标元素,采用电感耦合等离子体质谱法直接同时测定地球化学样品中痕量镓、铟、铊的方法。方法检出限(6s)Ga、In、Tl分别为0.059、0.002、0.004μg/g,方法精密度(RSD,n=12)为2.6%—5.3%。用国家一级标准物质进行验证,测定结果与标准值吻合。 相似文献
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Allison Forrest Richard Kingsley Jean-Guy Schilling 《Geostandards and Geoanalytical Research》2009,33(2):261-269
Promising methods have been developed recently for the determination of selenium (Se) and tellurium (Te) in geological materials at ng g−1 and lower levels, using hydride generation-inductively coupled plasma-mass spectrometry. Here we report on a new isotope dilution-hydride generation-inductively coupled plasma-mass spectrometry (ID-HG-ICP-MS) method for the simultaneous determination of Se and Te, which is applied to basalts, and modified compared to previous work. The basalts were attacked and dissolved with hydrofluoric and nitric acid, spiked with enriched isotopes, and passed through a cation exchange column (AG 50-X8 100–200 mesh) to separate the major cations that interfere with Se and Te detection (e.g., Fe). The detection limits of this method were 0.010 ng g−1 for Se and 0.0030 ng g−1 for Te, well below the concentrations of Se and Te expected in basalts. The precision of the method for Se was 12.2 to 15.1% and for Te was 4.6 to 7.2% RSD from replicate analyses of basalt reference samples. The accuracy for Se determinations was 61 to 94% and for Te 28 to 100% of values previously reported in the literature for selected USGS reference materials. 相似文献
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双硫代比林甲烷是近年来合成的新试剂,它是二安替比林甲烷的衍生物。在分析化学中的应用已有专门论述,它已用于多种元素的光度测定,其中应用较多的是铋、金、碲,但国内尚未见用于测定碲的报导。本文在前人的基础上试验了双硫代比林 相似文献
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M17树脂分离富集原子荧光测定岩矿中痕量碲 总被引:4,自引:1,他引:4
本文研究了不同种类树脂对Te的吸附能力,提出了在3mol/L HCl介质中,用M_(17)二甲胺树脂吸附,然后用水洗脱的新途径,使Te有效且无污染地得到分离和富集,实现了原子荧光测定地质试样中ppb级痕量Te。经地矿部标准参考样GSR7-12考察,分析结果与推荐值相符。 相似文献
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The chemistry and mode of occurrences of native tellurium in the epithermal gold ores from Teine, Kobetsuzawa, Mutsu, Kawazu, Suzaki and Iriki in Japan are examined. Mineral assemblages in contact with native tellurium are: quartz‐sylvanite at Teine, quartz‐hessite‐sylvanite‐tellurantimony at Kobetsuzawa, quartz at Mutsu, quartz‐stutzite‐hessite‐sylvanite‐tetradymite at Kawazu, quartz at Suzaki, and quartz‐goldfieldite at Iriki. The peak patterns of XRD for native tellurium from these six ores are nearly identical to that of JCPDS 4–554. Their chemical compositions of Te range from 98.16 to 100.73 wt.%, showing nearly pure tellurium. Other elements detected are: Se of 0–0.85 and Cu of 0–0.74 at Teine, Sb of 0.45–0.47 and Se of 0.19–0.27 at Kawazu, Se of 0.22–1.11 and Sb of 0–0.49 at Suzaki, and Cu of 0.69–0.98, As of 0.22–0.28 and Bi of 0–0.22 wt.% at Iriki. No other elements are detected in the ores of Kobetsuzawa and Mutsu. The ranges of associated minor compositions are consistent with those of the experimental phase. The differences would be related to associate minerals. The mineral assemblages in these ores agree well with the previously proposed experimental phase relations in Au‐Ag‐Te ternary system for 120–280°C. The Suzaki ore has high Te‐Au assemblage: from calaverite‐sylvanite‐krennerite via native tellurium to petzite, with changing mineralization stage, whereas the Kobetsuzawa and the Kawazu ores have high Te‐Ag assemblage of tellurium‐hessite, and native tellurium‐stutzite‐hessite‐sylvanite, respectively. The Teine ore has intermediate assemblage of native tellurium‐sylvanite. The mineral assemblages in the Au‐Ag‐Te system are related to the hydrothermal environment especially to the pH condition, i.e. Au rich assemblages under acidic and Ag rich assemblages under intermediate pH conditions, being supported by alteration mineral species. The other telluriferous epithermal gold deposits not in association with native tellurium such as Agawa, Date, Takeno, Chugu, Chitose, Sado and Kushikino are estimated to have been formed under higher pH conditions as adularia and calcite occur in these deposits. The pH‐Eh diagram for aqueous tellurium species and tellurium minerals at 250°C indicates that the region of native tellurium occurs between those of aqueous telluride and tellurous species at lower pH, being consistent with their mineral assemblages in ores and alteration envelopes. 相似文献
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