Determination of and differentiation between cassimerite and silicate-bound tin in silicate rocks containing traces of tin

A simple, sensitive and reproducible method is described for the determination of tin in silicate rocks at the ppm level. By applying a selective decomposition it seems possible to differentiate between tin present in the silicate lattice, in readily-accessible cassiterite (SnO(2)) and in cassiterite enclosed in the silicate. The final determination is made by extraction and photometry with phenylfluorone. Results for total tin agree well with those obtained by X-ray fluorescence.     

Fast determination of the tin content in cassiterite ores by photon activation method

Photon activation analysis has been success-fully applied to the fast and non-destructive analysis of tin in cassiterite ores based on the 159.7 keV gamma line of^123mSn produced in the¹²⁴Sn/γ, n/^123mSn reaction. In order to improve the accuracy of analytical results, corrections for self-absorption and pile-up effects were performed. Under typical conditions /15 μA electron beam current, 15 MeV bremsstrahlung energy, 5 min irradiation time and 10 min measurement/ the sensitivity of the analysis is 10 ppm. The proposed method can be used for routine analysis of tin in geological samples.     

乙二醇甲醚中电解锡电解液直接水解制备纳米SnO2

采用锡金属为阳极，在无隔膜电解槽中，电化学溶解锡于乙二醇甲醚中制备得到纳米SnO2前驱体Sn(OCH2CH2OCH3)4，将电解液直接水解经溶胶-凝胶法制备纳米SnO2，前驱体通过拉曼和红外光谱进行表征.纳米SnO2采用X射线粉末衍射(XRD)和透射电子显微镜(TEM)进行表征.实验表明,电解合成的Sn(OCH2CH2OCH3)4能够溶解于乙醇中, 适宜作为溶胶-凝胶(sol-gel)法制备纳米SnO2的原料，制得的纳米SnO2经600 ℃煅烧后呈球形单分散结构，晶型为四方锡石型, 比表面为62.58 m2·g－1，平均粒径在(10.0±0.4) nm左右.产率为89.3％，电流效率为86.9％.     

Quantitative determination of In and Sn in cassiterites by instrumental neutron activation analysis

Indium (10–15,000 ppm) and tin (20–90%) are quantitatively determined in cassiterite samples by instrumental (thermal) neutron activation analysis, using semiconductor detectors and gamma spectroscopy. Precision is 7% or better for In and 5% or better for Sn. The detection limit is 2 ppm for In and 0.4% for Sn in Mexican cassiterites.     

Determination of tin in ores and concentrates

A method is described for the determination of tin in cassiterite and stannite ores. The method is based on an ammonium iodide fusion of the ore under controlled heating conditions and the subsequent determination of tin by classical iodimetric technique.     

The spectrochemical determination of indium in cassiterite

In order to determine the indium content of cassiterite specimens, a spectrochemical method, using tin as internal standard and the cathode-layer carbon arc, has been employed. The precision of the procedure is approximately 5 %.     

Über die Darstellung und die Eigenschaften von σ-Organylwolframpentachloriden

Tungsten hexachloride reacts with dimethyl zinc or diphenyl zinc forming green methyl or phenyl tungsten pentachloride. However, tungsten hexachloride is reduced to tungsten tetrachloride on addition of zinc dialkyls with longer alkyl groups. Furthermore, alkyl tungsten pentachlorides can be prepared from tungsten hexachloride and tin tetraalkyls or boron trialkyls.     

熔融制样-X射线荧光测定钨钼锡矿中的主次成分

采用熔融制样-X射线荧光光谱法测定矿物中的Cu、Pb、Zn、Mo、W、Al、Fe、Si、K、Na、Ti、Ca、Sn等13种主次量元素,采用混合均匀的三混熔剂,以硝酸锂为氧化剂、溴化锂为脱膜剂,进行实验条件优化选择。在650℃下对样品进行预氧化,在1100℃下高温熔融,熔融时间为300 s,最后制成均匀透明,表面光滑无气孔的熔片,以部分国家一级标准物质和自制的钨钼锡标准样品,熔融制片进行测定,线性拟合建立标准曲线,并通过测定谱线选择、基体校正,使钨钼锡的测定范围扩宽,从微量到主量均能进行测定,并且适用于多种不同矿石的测定。样品的组成和含量变化会对分析线强度造成吸收、增强以及谱线重叠的影响,采用经验系数和理论α系数结合来校正其产生的基体效应。相同条件下熔融10个标准样品进行测定,其相对标准偏差(RSD)均小于5%,表明方法的准确度、精密度均满足国家相关质量标准的要求。选用一些含量不同的标准样品进行测定,最终的测定结果与标准值相符,表明方法可用于钨钼锡矿的测定。     

Extractive separation and spectrophotometric determination of tungsten as ferrocyanide

Tungsten, in amounts ranging from micrograms to milligrams, can be extracted into isoamyl alcohol, as the tungsten(V) ferrocyanide complex obtained by reduction of tungsten(VI) with tin(II) in 4M hydrochloric acid containing ferrocyanide. It can thus be separated from iron, cobalt, chromium, manganese, arsenic, antimony, bismuth, silicon, calcium and copper, their precipitation being prevented by addition of glycerol and, in the case of iron, sulphosalicyclic acid. Molybdenum, vanadium and nickel are not separated from tungsten, however. Tungsten can also be determined spectrophotometrically as tungsten(V) ferrocyanide. The absorbance of the brown complex is measured in aqueous solution or preferably after extraction into isoamyl alcohol. As many alloying elements interfere, they should be separated by the ferrocyanide extraction or other suitable method. Both the separation and the determination methods give satisfactory results with an overall error of not more than 0.5% in the analysis of practical samples containing low or high percentages of tungsten.     

Determination of traces of carbon, nitrogen and oxygen in molybdenum and tungsten

The determination of carbon and nitrogen in molybdenum and of carbon, nitrogen and oxygen in tungsten, is described. The analytical techniques applied were charged-particle activation (carbon, nitrogen and oxygen), photon activation (carbon and oxygen), combustion (carbon) and vacuum-fusion extraction (nitrogen and oxygen). Chemical methods yielded upper limits in the 2-5 mug/g range. Activation analysis yielded 100 and 8 ng/g for carbon in molybdenum and tungsten respectively, 500 and 74 ng/g for nitrogen in molybdenum and tungsten respectively and 70 ng/g for oxygen in tungsten. The results obtained by charged-particle and photon activation agreed satisfactorily.     

Minimizing the effect of organic matrices in the analysis of tin-containing extracts by electrothermal atomic absorption spectrometry: Determination of Tin in rocks

The effect of the nature of the extracted complex and of the organic solvent on the sensitivity of the extraction/atomic absorption determination of tin in a graphite-furnace atomizer is investigated. It is recommended that extracts of tin as its chloride complex, or chelates with N-benzoyl-N-phenylhydroxylamine or 8-quinolinol, in organic solvents which do not contain chlorine should be used. The depressive effect of the organic matrix can be significantly decreased by using ascorbic acid as matrix modifier, by atomization from a graphite platform, and by using an atomizer coated with tungsten carbide. The procedure developed is applied to the determination of tin in rocks. For tin concentrations of 0.1–10 μg g^?1, the relative standard deviation does not exceed 10%.     

用改进的因子分析-光度法同时测定含有锗钼钨锡的混合物体系

本文通过模拟纯谱及非零截距的引入,改进了因子分析-光度法。用该法探讨了以对硝基苯基荧光酮及溴代十六烷基三甲铵作为试剂的多元络合物体系同时测定锗、钼、钨、锡的最佳条件。实验证实用该法测定合成样品及钢样,结果满意。     

Bestimmung des in Form von Kassiterit vorkommenden Zinns

Zusammenfassung Zur Ermittlung des in Gesteinen als Kassiterit vorliegenden Zinnanteils wird die gemahlene Probe mit Ammoniodid in einem Reagensglas zweimal sublimiert und anschließend in wäßriger Weinsäure/Ascorbinsäure gelöst. Nach Dekantieren und Waschen des unlöslichen Rückstandes erfolgt die Zinnbestimmung mit Hydrid-AAS aus weinsaurer Lösung; die Querstörungen dieser Endbestimmung sind als gering zu bezeichnen. Hauptproblem sind Kontaminationen aus den Gefäßen, die durch Spülen bzw. Stehenlassen mit verdünnter Weinsäure vermieden werden können.Die Selektivität des Verfahrens wird durch Anwendung auf Mineralien dokumentiert, wobei als Referenzmethode die spektrographische Bestimmung des Gesamtgehalts dient.In Schwermineralfraktionen wurden 53–79% des Zinns als in Kassiterit vorkommend gefunden.

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Determination of tin occurring bound in cassiterite

Summary For the determination of the amount of tin being present in rocks as cassiterite, the powdered sample is sublimed twice with ammonium iodide within a test tube, and subsequently dissolved in aqueous tartaric/ascorbic acid. After decantation and washing of the insoluble residue, the determination of tin is performed by hydride-AAS from tartaric acid solution; the cross interferences of this final determination are small. The chief experimental problem has been the contamination from vessels, which can however be avoided by rinsing and soaking with diluted tartaric acid. The selectivity of the procedure is documented by the application to some minerals, in comparison with the spectrographic determination of the total amount of tin as a reference.In fractions of the heavy minerals, 53–79% of the total tin has been found to be present as cassiterite.

     

Sb掺杂SnO_2(ATO)纳米晶的水热合成和导电性能

以Sn和SbI_3为主要原料，在120-170 ℃温和水热条件下合成了具有导电能力 的Sb掺杂SnO_2(ATO)透明导电纳米粉体，运用FT-IR， XRD， BET， TEM等手段对 粉体的形成过程进行了分析表征。实验结果表明，所合成的纳米ATO粉体均为四方 锡石结构，无其他杂相存在，晶粒大小在4-7nm之间，粉体呈单分散状态。比表面 积在137-184m~2·g~(-1)之间，随水热温度的升高，晶粒长大，比表面积下降，粉 体导电性能提高。该方法对于其他透明导电氧化物纳米粉体的合成具有借鉴意义。     

高频红外碳硫分析仪测定含碳化硅耐火材料中碳化硅含量

采用对试样进行灼烧预处理的方法,除去游离碳,用锡粒、纯铁、钨粒作为助熔剂,并以钢铁标准样品校正仪器,高频燃烧红外吸收法测定含碳化硅耐火材料中的碳化硅含量,测定结果的相对标准偏差为1.07%(n=6),该法与化学法的测定结果较接近,精密度和准确度均满足化学分析的要求。     

锡钼(钨)异多核金属配合物研究进展

描述了锡钼(钨)异多核金属配合物近年来的研究进展.根据中心金属锡及钼(钨)周围配体的不同,该类配合物表现出不同的结构特征和反应活性.     

Determination of tungsten and tin ions after preconcentration by flotation

A highly sensitive and selective combined method of flotation followed by spectrophotometry/d.c. polarography for the determination of tungsten and tin ions in acid and alkaline waste waters and hydrometallurgical solutions is presented here. Both kinds of ions are coprecipitated in the analyte solution with zirconium hydroxide after addition of ZrOCl₂ solution and ammonia. Afterwards, the collector precipitate is separated from the aqueous phase and preconcentrated by flotation for which sodium oleate and a frother are added. The precipitate is dissolved in a small amount of acid, with the organic reagents being destroyed by oxidation. The enrichment factor of the proposed technique is 100, with variations possible. Recovery is 94% for tungsten and 99% for tin. Spectrophotometry of the thiocyanate complex and d.c. polarography are applied as determination techniques for tungsten and tin, respectively. Detection limits attainable by this technique are 6 ng · ml^–1 for tungsten and 5 ng · ml^–1 for tin for the initial sample.     

Adsorption of Ions on the Surface of Tin Dioxide and Its Electrokinetic Characteristics in 1 : 1 Electrolyte Solutions

Adsorption and electrokinetic characteristics of tin dioxide (cassiterite) are studied as a function of pH in aqueous NaCl and KCl solutions. The dissociation constants of surface groups, formation constants of ion pairs, and the adsorption potentials of ions are calculated in terms of the 2-pK model; capacities and potentials of the electrical double layer are determined; the dissociation degree of surface groups in the point of zero charge and in the isoelectric point are also estimated. It is shown that the 2-pK model in combination with the Graham model can be applied in the studied systems for describing the experimental results.     

分光光度法测定钨矿中微量钨

提出了一种测定钨矿中微量钨的分光光度法。该法摩尔吸光系数ε为9.6× 1 0 4 L· mol-1· cm-1,相对标准偏差 <2 % ,加标回收率为 95%～ 1 0 4 %。WO3 含量在 0～ 30 μg/50 m L 范围内满足比尔定律     

红外吸收测定铝质耐火材料中碳

试验以锡粒、纯铁、钨粒为助熔剂,用红外吸收测定铝质耐火材料中碳。通过加入碳酸钙进行回收率试验,回收率在９５％～１０５％内,ＲＳＤ在１％以下。在没有标样情况下,用合成标样或标准加入法计算样品结果与化学分析法基本一致。