RESUMO
New methods are described for the iodometric microdetermination of arsenic in organic compounds after wet digestion or oxygen flask combustion. After evaporation of the arsenic solution to dryness and dissolution of the residue in water, acetone is added and the solution is treated with iodide-iodate and the iodine liberated (by the interfering acids and the first dissociation step of arsenic acid) is reduced with thiosulphate. The KH(2)AsO(4) left is then reacted with zinc sulphate in presence of excess of KI and KIO(3). Acetone is added and the liberated iodine is titrated with thiosulphate. This titration corresponds to the second and third dissociation steps of arsenic acid and is used to calculate the arsenic content of the compound. When arsenicals not containing sulphur are decomposed by the oxygen flask method, the arsenic acid solution obtained is reacted directly with zinc sulphate in presence of KI and KIO(3) and the iodine released is titrated with thiosulphate. In this case, the titration corresponds to all three dissociation steps of arsenic acid. The average recoveries obtained by the two methods are 99.5 and 99.9%, respectively.
RESUMO
A method for the microdetermination of organic compounds containing halogens, by a polarographic finish, is reported. After the combustion of the organic sample in the oxygen flask, the products are absorbed in a suitable absorbent and chemically treated to produce Cl(-), Br(-), BrO(3)(-) or IO(3)(-) ions in solution before the polarography. The method is applicable to partially, highly, and fully halogenated aromatic and aliphatic compounds, whether solid or liquid. The results are generally within the acceptable limits of error.
