氢化物发生-四通道原子荧光光谱法同时测定高纯金中的痕量铋、锑、硒和碲

用乙酸乙酯萃取分离金,分液还原后应用氢化物发生-四通道原子荧光光谱法测定高纯金中的痕量铋、锑、硒和碲。在最佳条件下,方法对铋、锑、硒和碲的检出限分别为0.04,0.05,0.03,0.03 ng/mL(3δ);测定精密度(RSD)分别为0.98%,0.93%,0.94%,0.99%(对10 ng/mL Bi、Sb、Se和Te混合标准,n=7)。用所建立的方法对实际样品中的铋、锑、硒和碲进行了同时测定,测定结果与用标准方法测定所得结果之间无明显差异,各元素的加标回收率在95%～105%。结果表明,此方法能同时精确测定高纯金中的痕量铋、锑、硒和碲的量,且检出限较低,测定结果与国家标准方法一致。     

原子荧光光谱法测定染料产品中砷、汞、锑、硒

采用原子荧光光谱法对染料产品中砷、汞、锑、硒的量进行测定。结果表明：砷、汞、锑的检出限均远小于GB 20814中的检出限,硒的检出限只有0.02μg/L,四种元素的相对标准偏差都在10%以内,回收率均90%～110%之间。该方法可用于染料产品中砷、汞、锑、硒的量的分析测定。     

碲铋锑物料分离回收碲、铋的研究

碲铋基固溶体合金在温差发电和半导体制冷领域应用十分广泛。加工过程产生的边角料及多年来积累的大量已失效的热电制冷器件中的碲铋锑废料是回收碲铋的重要原料。为此,本文以热力学分析为基础,对溶液的酸度以及电位对碲铋锑的分离效果进行了研究。结果表明,液固比4︰1,酸度在4 mol/L以上,电位340～360 mv时,铋、锑的浸出率达98%以上,碲回收率达98%以上。     

电感耦合等离子体发射光谱(ICP-OES)法测定铅烟灰中铋、铟、锑、锡

研究了准确快速测定铅烟灰中铋、铟、锑、锡的分析方法，分析了仪器观察高度、研究内标引入方式、定容体积、主量基体元素对测定结果的影响。最终确定了径向最佳观察高度为10 mm、采用过氧化钠高温熔融试样、提前引入内标、无需准确定容的方式，建立了电感耦合等离子体发射光谱(ICP-OES)法同时测定铅烟灰中铋、铟、锑、锡的方法。铋、铟、锑、锡的方法检出限分别为0.0039%、0.0062%、0.0097%、0.0060%,加标回收率在96.0%～104.0%,相对标准偏差(n=11)<2%。方法缩短了检测周期，提高了多元素检测的效率。     

氢化物发生-原子荧光光谱法在化探样品测试中的应用进展

综述了近10年(2010～2019年)氢化物发生-原子荧光光谱法(HG-AFS)在化探样品中痕量元素测定方面的最新进展,涉及砷、锑、铋、汞、碲、硒、锡、镉等多种痕量元素的测定;同时也对该项分析技术的未来发展作了展望。     

水浴消解—原子荧光法同时测定沉积物中锑与硒

建立了王水水浴消解—原子荧光同时测定沉积物中锑与硒的方法,研究了同时测定锑与硒的实验条件并对方法检出限、线性范围、精密度、准确度等进行实验。结果表明:锑、硒的检出限分别为0.003 mg/kg、0.011 mg/kg;对锑和硒的标准样品6次测定的相对标准偏差分别为5.01%、2.90%。4份GSS系列锑和硒标准样品测定结果均在推荐值范围之内。结果准确可靠,灵敏度高、操作简便快速,有推广应用价值。     

水浴消解-原子荧光法测定土壤中硒、锑的研究

采用(1+1)王水-沸水浴体系对土壤样品进行前处理,原子荧光光谱法测定样品中硒、锑含量。在仪器最佳工作条件下,硒和锑的方法检出限分别为0. 01 mg/kg和0. 009 mg/kg;相对标准偏差:硒为2. 00%～5. 38%,锑为1. 92%～3. 21%;加标回收率:硒为89. 0%～105%,锑为89. 5%～98. 0%。用国家标准物质验证其准确度,结果均在不确定度范围内。该法成本低、准确度高且操作简便,适用于大批量土壤样品的分析测试要求。     

石墨炉原子吸收光谱法直接测定铁镍基高温合金中的银、砷、铋、铅、硒、碲

采用石墨炉原子吸收光谱仪,实现了铁镍基高温合金中痕量银、砷、铋、铅、硒、碲元素的直接测定,分析过程简便快捷,测定结果准确可靠。为了有效消除基体干扰,基于仪器纵向交流塞曼效应扣除背景这一优点,选用铁镍基标准样品建立工作曲线,并在该方法条件下考察了溶样酸和石墨炉温度制度条件。试验结果表明,各元素在其试验条件下均获得了较好的工作曲线,其线性相关系数R2均高于0.998;试验测得样品GBW01631中银、砷、铋、铅、硒、碲元素的回收率在94.4%~110%之间;样品GBW01632和GBW01634中各元素的相对标准偏差RSD(n=6)分别介于1.6%~9.6%和0.85%~6.4%之间,即试验获得了良好的准确度和精密度。     

原子荧光法检测水中砷的方法验证

采用《水质汞、砷、硒、铋和锑的测定原子荧光法》 HJ694-2014,从人、机、料、法、环、测方面评定实验室开展水中砷检测的能力,即进行方法验证。验证的主要内容包括方法检出限、精密度和准确度。     

碱浸渣综合利用新工艺研究

介绍了从碱浸渣中综合回收稀贵金属及其它有价元素的新工艺:用萃取法先把稀有元素碲与其它元素分离,然后分别回收碲、铜、锑、铋、铅和金银.碲、金、银的回收率均在95%以上,铜、锑、铋的回收率大于90%,铅的直收率大于80%.主产品Te02和PbS04的纯度在98%以上.     

石墨炉原子吸收法测定硝酸银中的痕量元素

感光级硝酸银样品经一系列的化学处理后,上清液采用石墨炉原子吸收分光光度法测定其中Bi,Cd,Cr,Cu,Fe,Mn,Ni,Pb,Sb,Sn,Te,Se,Zn元素的含量,本方法测定Bi,Cd,Cr,Cu,Fe,Mn,Ni,Pb,Sb,Sn,Te,Se,Zn各元素均能得到良好的标准曲线,即r=0.99~1;Cu、Cr、Ni、Sb、Sn、Mn、Te、Se的回收率较好,一般可达到95%~110%,Zn、Bi、Cd、Pb的回收率较低,经常只有50%~60%。     

Electrodeposition of lead alloys from fluoborate baths

The codeposition of some elements with lead from fluoborate baths has been studied in order to obtain lead alloys with a low concentration of a second metal. The metals considered were As, Bi, Cu, Sb, Se, Sn and Te. The chemical analysis of alloys obtained in various electrolysis conditions permitted an investigation of the kinetic behaviour of the metals codeposited with lead. The results showed that only Bi, Sb, Se and Te attain a limiting value of discharge current density and that the codeposition is regular for all metals. SEM observation of the deposits revealed that Sb and Se have a marked influence on the crystal morphology while the remaining metals induce only minor modifications.     

氢化物发生技术在煤炭分析中的应用

针对煤中微量元素的含量及目前检测手段，详细阐述了氢化物发生技术在检测As、Se、Sb、Bi、Ga、Ge、Sn、Pb、Te、Hg中的应用，以及氢化物发生技术的原理、优缺点、发生方法、使用技术等。     

The variation of element contents in triticale during vegetative growth

The variation of N, P, K, Ca, Mg, Fe, Mn, Zn, Cu, B, Ba, Be, Bi, Sn, Sr, Sb, Ti, Te, V, Se, As and Hg concentrations was studied under field conditions in triticale. The samples were collected every 10 days from tillering to full ripening stage using plant material from 0.5 m² per plot. The concentrations generally decreased from early growth to harvest. The elemental concentrations in triticale differed from the other cereals, but the variation's trend was similar.

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Zusammenfassung Es wurden die Schwankungen in den Konzentration von N, P, K, Ca, Mg, Fe, Mn, Zn, Cu, B, Ba, Be, Bi, Sn, Sr, Sb, Ti, Te, V, Se, As und Hg in Triticale unter Feldbedingungen untersucht. Von der Bestockung bis zur Vollreife wurden alle 10 Tage von je 0.5 m² pro Parzelle Pflanzenproben genommen.In allgemeinen haben die Konzentrationen von Frühjar bis zur Ernte abgenommen.Der elementengehalt in Triticale war demjenigen der übrigen Getreidearten verschieden, aber der Trend der Änderungen war ähnlich.

     

Selective oxidation of light alkanes over hydrothermally synthesized Mo-V-M-O (M=Al, Ga, Bi, Sb, and Te) oxide catalysts

Selective oxidations of ethane to ethene and acetic acid and of propane to acrylic acid were carried out over hydrothermally synthesized Mo-V-M-O (M=Al, Ga, Bi, Sb, and Te) complex metal oxide catalysts. All the synthesized solids were rod-shaped crystallites and gave a common XRD peak corresponding to 4.0 Å d-spacing. From the different XRD patterns at low angle region below 10° and from the different shape of the cross-section of the rod crystal obtained by SEM, the solids were classified into two groups: Mo-V-M-O (M=Al, possibly Ga and Bi) and Mo-V-M-O (M=Sb, and Te). The former catalyst was moderately active for the ethane oxidation to ethene and to acetic acid. On the other hand the latter was found to be extremely active for the oxidative dehydrogenation. The Mo-V-M-O (M=Sb, and Te) catalysts were also active for the propane oxidation to acrylic acid. It was found that the grinding of the catalysts after heat-treatment at 600°C in N₂ increased the conversions of propane and enhanced the selectivity to acrylic acid. Structural arrangement of the catalytic functional components on the surface of the cross-section of the rod-shaped catalysts seems to be important for the oxidation activity and selectivity.     

The underpotential deposition of bismuth and tellurium on cold rolled silver substrate by ECALE

Thin-layer electrochemical studies of the underpotential deposition (UPD) of Bi and Te on cold rolled silver substrate have been performed. Different approaches have been employed to investigate the influence of silver oxide film on Bi UPD. As a result, the precedent deposition of a little bismuth can effectively prevent silver from surface oxidation. The voltammetric analysis of underpotential shift demonstrates that the first Te UPD on Bi-covered Ag and Bi UPD on Te-covered Ag fit UPD dynamics mechanism. Thin film of bismuth telluride was formed using an automated flow deposition system, by alternately depositing Te and Bi. The electrochemical conditions necessary to form Bi₂Te₃ deposits of 50 cycles on cold rolled silver by ECALE are described here. X-ray diffraction indicated the deposits were Bi₂Te₃. EDX quantitative analysis gave the 2:3 stoichiometric ratio of Bi to Te, which is consistent with XRD result. Electron probe microanalysis of the deposits showed a worm-like network structure. The map of Te and Bi element indicated the distribution of both Te and Bi is homogeneous and locates the same sites, which is favorable to Te-Bi binary system. The composition analysis of structural expanded image also showed the approximately constant composition of Te:Bi ≈ 3:2 has taken place.     

Electrodeposition of Sb, Bi, Te, and their alloys in AlCl3-NaCl-KCl molten salt

The Electrochemistry of Sb, Bi, and Te in AlCl₃-NaCl-KCl molten salt containing SbCl₃, BiCl₃, and/or TeCl₄ at 423 K was investigated by voltammetry, and electrodeposition of the three metals was performed under constant potential control in the melt. The voltammogram on a glassy carbon (GC) electrode in a melt containing 0.025 mol dm⁻³ [M] SbCl₃ showed a couple of redox peak corresponding to the Sb/Sb(III) redox reaction, and a stable layer of pure Sb was deposited under the constant potential control. The voltammograms in the melt containing 0.025 M BiCl₃ or 0.025 M TeCl₄ showed several redox couples. Stable deposit layers of pure Bi and Te were not obtained under the constant potential control, as the deposited layers detached from the electrode and immediately dissolved into the molten salt. Binary alloy deposition was possible in a melt containing BiCl₃ and SbCl₃, and also with BiCl₃ and TeCl₄. A stable Bi-Sb alloy deposit of metallic Sb and Bi-Sb solid solution was obtained at 0.8 and 0.9 V versus Al/Al(III) in the melt containing BiCl₃ and SbCl₃. The atomic ratio of Bi in the deposit was 37% at 0.9 V and 57% at 0.8 V. A stable Bi-Te alloy deposit was also obtained with the molten salt containing BiCl₃ and TeCl₄. The deposited Bi-Te alloy consisted of a mixture of Bi₂Te₃, BiTe, and Bi₂Te. The alloy deposit had good crystallinity and the preferential orientation was the (1 1 0) plane.     

ICP-MS法测定磷酸二氢钾中杂质元素

建立了电感耦合等离子体质谱（ICP-MS）法测定磷酸二氢钾中铍、镁、镍、铜、锌、砷、硒、镉、锑、铊、铅等11种杂质元素的分析方法。样品经硝酸消解后进行分析,选用锂、铋、铟、铑元素为内标混合液校正基体干扰。研究结果表明,该方法对11种待测元素的加标回收率范围为86.00%～118.77%,相对标准偏差范围为3.79%～8.60%,方法的准确度和精密度均符合要求。该方法简便、快速,能满足磷酸二氢钾中多种杂质元素同时测定的分析需求。     

Doped Ni Catalysts for Methane Reforming with CO<Subscript>2</Subscript>

Pb, Sb, Bi and Te doped Ni catalysts were prepared and used for methane reforming with CO₂ in order to diminish coke deposition. It was found that small amounts of Pb doped Ni catalysts exhibited excellent coke resistance ability with minor loss of the reforming activity. As the added amount of Pb increased from 0 to 0.015 (mole ratio between Pb/Ni), coke formation rate decreased from 166.7 mg-coke/g-cat h (on Ni/SiO₂) to 0, while the reforming activity decreased slightly from 73.2% to 63.3% (conversion of CO₂) at 800 °C, 60,000 ml(STP)/g-cat·h (CH₄ CO₂=1:1, no dilution gas in feed). Higher amounts of Pb and Sb, Bi, Te made Ni catalyst deactivated for methane reforming with CO₂.     

Recent development and application of thin-film thermoelectric cooler

Recently, the performance and fabrication of thin-film thermoelectric materials have been largely enhanced. Based on this enhancement, the thin-film thermoelectric cooler (TEC) is becoming a research hot topic, due to its high cooling flux and microchip level size. To fulfill a thin-film TEC, interfacial problems are unavoidable, as they may largely reduce the properties of a thin-film TEC. Moreover, the architecture of a thin-film TEC should also be properly designed. In this review, we introduced the enhancement of thermoelectric properties of (Bi,Sb)₂(Te,Se)₃ solid solution materials by chemical vapor deposition, physical vapor deposition and electrodeposition. Then, the interfacial problems, including contact resistance, interfacial diffusion and thermal contact resistance, were discussed. Furthermore, the design, fabrication, as well as the performance of thin-film TECs were summarized.