Preparation of Antimony

Preparation of Antimony. Put a thoroughly dried mixture of 12 g of antimony sulphide, 5 g of reduced powdered iron, 1.5 g of sodium sulphide, and 0.5 g of powdered charcoal into a chamotte or porcelain crucible and roast it in a muffle furnace at 800 °C. After the entire mixture softens, continue the heating for another 20-30 minutes. Next cool the crucible, break it, and extract the antimony bead. 

Test the reaction of metallic antimony with hydrochloric, sulphuric, and nitric acids. What position does antimony occupy in the electrochemical series of the metals  

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Nowak M, Szperlich P, Tilak E, Szala J, Rzychon T, Stroz D, Nowrot A, Solecka B (2010) Sonochemical preparation of antimony subiodide. Ultrason Sonochem 17(1) 219-227... 

Alexander Mikhailovich Butlerov, 1828-1886. Russian organic chemist. He worked with K. K. Klaus on the preparation of antimony at the University of Kazan and later studied organic chemistry under N. N. Zinin. After working with some of the most famous chemists in Europe and serving as professor of chemistry at the University of Kazan he was appointed ordinary professor of chemistry at the University of St. Petersburg. See ref. (94). 

To prepare arsenic hydride, assemble an apparatus as shown in Fig. 140 and perform this experiment as described under the heading Preparation of Antimony Hydride in Sec. 31.2. Write the equations of all the reactions proceeding in this experiment and explain them. 

Preparation of Antimony(V) Oxide. Treat 0.25 g of powdered metallic antimony with 2-3 ml of concentrated nitric acid in a porcelain howl while heating it in a water hath. Consider oxidation to he completed if a sample of the obtained white powder dissolved in an alkali will not reduce an ammonia solution of silver. When oxidation is completed, dilute the reaction mixture with water and separate the precipitate by decantation. Dry the precipitate in a water bath until it is dry, and then in a sand bath (275 °C). What is observed when it is treated with concentrated hydrochloric acid and a sodium hydroxide solution Write the equations of the reactions. How can antimony(lll) oxide be prepared ... 

Preparation of Antimony(III) Iodide. (Perform the experiment in the presence o/ your instructor in a iume cupboard, away from a flame ) Assemble an apparatus (see Fig. 119a). Place 1 g of finely triturated metallic antimony into a three-neck flask and add 25 ml of benzene. Prepare a solution of 4 g of iodine in 75 ml of benzene and pour it into dropping funnel 4. Heat the mixture in flask 1 in a water bath with stirring until it boils (use an electrical stove with an enclosed coil ). 

The furnace is subjected to a temperature/time treatment according to the specifications given in the tables for the respective compound. For the preparation of antimony(III) iodide sulfide, the furnace is cooled uniformly from 480-250°C. for a period of 10 days. ... 

Preparation of Antimony Trifluorodichloride (SbF3Cl2). This is made in the steel reaction vessel, described on p. 59. A known quantity of antimony fluoride is placed in the vessel the vessel is evacuated, the needle valve is closed, and the whole is weighed. Connection is established to a chlorine cylinder, and the needle valve is opened to permit qhlorine to fill the vessel. Part of it is absorbed rapidly by the salt, with evolution of heat. Soon the reaction slows down as indicated by the rate of pressure fall when the needle valve is dosed. Weighing indicates the amount of chlorine present in the vessel. When the absorption practically ceases, the valve is closed, and the connection with the chlorine tank is removed. The reaction vessel is alternately heated gently, then allowed to cool in order to permit SbFsCl2, which is a viscous liquid, to flow and expose fresh surfaces of crystalline antimony trifluoride. The operation is ended after the absorption of the desired quantity of chlorine. 

Write equations for all reactions involved in the preparation of antimony pentasulphide from stibnite. 

Three following general methods have been employed for the preparation of antimony pentaalkoxides (i) reaction of alcoholates with SbCl5, (ii) oxidation of (RO)3Sb with bromine to form (RO)3SbBr2 and treatment of the bromo compound with alcoholates and (iii) alcoholysis of (RO)5Sb246 250). 

The final preparation of antimony we will briefly examine is that of the so-called Star Regulus of Antimony. This preparation is considered to be an advanced alchemical work as there is some danger involved and requires the operator to have developed laboratory skills. Many of the ancient sages describe this operation in extremely veiled terms. 

Supplementary Experiments and Syntheses 1. Preparation of Antimony (276). 2. Preparation of Antimony(V) Oxide (277). 3. Preparation of Antimony(lll) Iodide (277). 4. Preparation of Bismuth and Studying of Its Properties (277). Appendix 1. Selected Tables... 

Porcher s Resources was a monumental work. Listing some 35,000 native plants, Porcher believed that 410 had medicinal value. Moreover, he gave an exhaustive list of native substitutes for imported drugs. For gum arabic (acacia), for example, he recommended slippery elm. Citing McKeown, Porcher suggested that a teaspoonful of the powdered [pleurisy] root in hot water, often repeated, acts as a safe and useful substitute for the preparations of antimony Porcher had particular favorites and tended to give them in running lists. A typical commentary ran as follows ... 

The method has been used for the preparation of antimony derivatives (equation 45) However, the method has not been used frequently in recent years. 

M. Kogure, T. Sato, T. Tanaka, S. Yasujima, T. Suzuki and H. Ohya, Preparation of antimony acid cation exchange membranes by using metal alkoxide-gel method, Bull. Chem. Soc. Jpn., 1991, 1991, 1618 H. Ohya, R. Paterson, T. Nomura, S. McFadzean, T. Suzuki and M. Kogure, Properties of new inorganic membranes prepared by metal alkoxide methods. Part I A new permselective cation exchange membrane based on Si/Ta oxides, J. Membr. Sci., 1995, 105, 103-112. 

Basil Valentine was well acquainted with the starred surface of pure metallic antimony, and remarked that the starred and the unstarred antimony had exactly the same composition, and that the starred one was due to the use of iron in its preparation while, in opposition to this idea, other chemists of the period traced the cause of the starred one to the favourable conjunction of stars. He also knew that antimony did not possess the full character of a metal, and for this reason he called it lead of antimony. Furthermore, he noticed that spiessglas contained sulphur, and he was acquainted with sulphur aura turn (a mixture of SbjSj and 8 285). He gave distinct recipes for the preparation of antimony trichloride (butter of antimony), powder of algaroth (basic chloride of antimony), antimony trioxide, potas.sic antimoniate. In his time antimony was used for the preparation of printers type, mirrors, and bells, and was also used as medicine. 

Preparations of antimony, as emetic tartar, antimonl-um tartarizatum, wine of antimony. James s powder. 

Fig. 204. Preparation of antimony (III) chloride, r) Glass tube, straight section about 60 cm. long. Inside diameter 1.5 cm., 0.8 cm. in constricted section. Walls 1.5-2 mm. thick.

Alloys are prepared in batches by adding weighed components to an agitated kettle. In the case of antimony, antimonial lead of highly variable composition is often available from the reduction of antimony rich slags, and is used for the preparation of antimonial alloys. Composition is checked by spectrographic analysis and is adjusted and re-checked before casting. 

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