Antimony/ions/salts determination

Antimony pyrogallate, Sb(C6H503). Antimony(III) salts in the presence of tartrate ions may be quantitatively predpitated with a large excess of aqueous pyrogallol as the dense antimony pyrogallate. The method fadlitates a simple separation from arsenic the latter element may be determined in the filtrate from the predpitation of antimony by direct treatment with hydrogen sulphide. 

Determination of silver as chloride Discussion. The theory of the process is given under Chloride (Section 11.57). Lead, copper(I), palladium)II), mercury)I), and thallium)I) ions interfere, as do cyanides and thiosulphates. If a mercury(I) [or copper(I) or thallium(I)] salt is present, it must be oxidised with concentrated nitric acid before the precipitation of silver this process also destroys cyanides and thiosulphates. If lead is present, the solution must be diluted so that it contains not more than 0.25 g of the substance in 200 mL, and the hydrochloric acid must be added very slowly. Compounds of bismuth and antimony that hydrolyse in the dilute acid medium used for the complete precipitation of silver must be absent. For possible errors in the weight of silver chloride due to the action of light, see Section 11.57. 

The blue solid prepared by Rulf et al. (9) in 1906 and thought to be (SbF5)aI was probably a mixture of an la fluoroantimonate salt, and some Sb(III)-containing material. Pure crystalline la SbaFu has recently been prepared by the reaction of iodine with antimony pentafluoride in liquid sulfur dioxide as solvent (11). After removal of insoluble SbFg, deep blue crystals of la SbaFi were obtained from the solution. An X-ray crystallographic structure determination showed the presence of the discrete ions la and SbaFu . Crystalline solids that can be formulated as la SbaFu and Ia TaaFii have also been prepared by Kemmitt et al. (4) by the reaction of iodine with antimony or tantalum pentafluorides in iodine pentafluoride solutions. 

The reaction of toluene-3,4-dithiol(3,4-dimercaptotoluene) and antimony trichloride in acetone yields a yellow solid Sb2(tdt)3, where tdt is the toluene-3,4-dithiolate anionic ligand (51). With the disodium salt of maleonitriledithiol ((Z)-dimercapto-2-butenedinitrile), antimony trichloride gives the complex ion [Sb(mnt)2]- , where mnt is the maleonitriledithiolate anionic ligand. This complex has been isolated as a yellow, crystalline, tetraethyl ammonium salt. The structures of these antimony dithiolate complexes have apparendy not been unambiguously determined. 

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