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    Cluster Harvesting by Successive Reduction of a Metal Halide with a Nonconventional Reduction Agent: A Benefit for the Exploration of Metal-Rich Halide Systems
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    Abstract:
    The preparation of thermally labile compounds is a great temptation in chemistry which requires a careful selection of reaction media and reaction conditions. With a new scanning technique denoted here as Cluster Harvesting, a whole series of metal halide compounds is detected by differential thermal analysis (DTA) in fused silica tubes and structurally characterized by X-ray powder diffraction. Experiments of the reduction of tungsten hexahalides with elemental antimony and iron are presented. A cascade of six compounds is identified during the reduction with antimony, and five compounds or phases are monitored following the reduction with iron. The crystal structure of Fe2W2Cl10 is reported, and two other phases in the Fe-W-Cl system are discussed.
    In this paper a sensitive and rapid method for the determination of lead in antimony and antimony compounds by HG AFS is developed. The matrix of antimony is vaporized with hydrobromic acid during sample pre treatment. The detection limit of this method for lead is less than 1×10 -6 . The precision for the samples with w (Pb)=0.045×10 -2 is better than 2.0% RSD ( n =4). The recovery of the method is 95%~105%. The method has been applied to the determination of trace lead in antimony and antimony products. The analytical results are in agreement with those from AAS analysis.
    Hydrobromic acid
    Matrix (chemical analysis)
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    ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTDetermination of Antimony in Lead-Antimony Alloys of Low Antimony ContentLeaon I. Shaw, Charles F. Whittemore, and Thor H. WestbyCite this: Ind. Eng. Chem. Anal. Ed. 1930, 2, 4, 402–403Publication Date (Print):October 1, 1930Publication History Published online1 May 2002Published inissue 1 October 1930https://pubs.acs.org/doi/10.1021/ac50072a023https://doi.org/10.1021/ac50072a023research-articleACS PublicationsRequest reuse permissionsArticle Views49Altmetric-Citations2LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail Other access options Get e-Alerts
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    Abstract Antimony belongs to Group 15 (VA) of the Periodic Table, which also includes arsenic and bismuth. Antimony ore bodies are small and scattered throughout the world. Nearly all of the world's primary antimony is mined in China, Bolivia, and Russia. World reserves of antimony are estimated to be ∼1.8 million tons. Antimony is a silvery white, brittle solid. It is ordinarily quite stable and not readily attacked by air. The antimony content of commercial ores ranges fro 5 to 60%, and determines the method of treatment, either hydrometallurgical or pyrometallurgical. The U.S. is not self‐sufficient in its requirements for antimony and is heavily dependent on imports of both ore and metal. Metallic antimony can be handled freely, without danger, but direct skin contact should be avoided. Most antimony compounds are poisonous. Antimony uses are as follows: in flame retardants, transportation including batteries, and ceramics, glass, and solar cells
    Bismuth
    Antimony trioxide
    Bis (2-nitrobenzaldoximato)tri( meta -tolyl)antimony ( 1 ), µ 2 -oxo- bis [(2-nitrobenzaldoximato)-tri( meta -tolyl)antimony] ( 2 ) and bis (2-nitrobenzaldoximato)tri( ortho -tolyl)antimony ( 3 ) have been obtained by the reactions of tri( meta -tolyl)antimony and tri( ortho -tolyl)antimony with 2-nitrobenzaldoxime in the presence of an oxidizing agent (hydrogen peroxide or tert -butyl hydroperoxide). Compounds 1–3 have been characterized by X-ray diffraction analysis.
    Oxidizing agent
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    Procedures for the preparation of antimony sample solutions for the differentiation of antimony(III) from antimony(V) by extraction with ammonium tetramethylenedithiocarbamate (ammonium pyrrolidinedithiocarbamate, APDC) were examined. It was found that, when APDC is added to the antimony(V) solution of pH less than ca. 3, the antimony(V)-APDC complex is partially co-extracted with antimony(III) over the pH range 3.5–10. Further, the mixing of antimony(III) solution with acidic antimony(V) solution, prepared by oxidising antimony(III) potassium tartrate solution, leads to the incomplete extraction of antimony(III). A standard procedure for removing the interferences was established.
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    A method for the determination of water-soluble antimony (III) and antimony (V) in Leigongteng using ultrasound-assisted extraction by hydride generation inductively coupled plasma atomic emission spectrometry was developed in the present paper. Affecting parameters of ultrasound extraction, the pH of antimony species, the operation condition of hydride generation and inductively coupled plasma atomic emission spectrometry were investigated and optimized. The effect of coexisting ions on the determination of antimony was also investigated. The detection limits are 0.3 and 2.4 ng x mL(-1) for antimony (and antimony (V), respectively, and with RSD 3.9% for antimony (III) and 4.5% for antimony (V). The recovery is in the range of 93% to 105%.
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