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Um sistema de analise por injecao em fluxo com deteccao espectrofotometrica e proposto para determinacao de cloreto em eletrolito de bateria chumbo-acido, utilizando a reacao com tiocianato de mercurio(II) em meio contendo ferro(III). A formacao de gradientes de indice de refracao no centro da zona de amostra foi evitada utilizando um elevado volume de amostra. Interferencia devida a sulfato foi investigada e a correlacao entre os equilibrios quimicos envolvidos e os sinais transientes gerados foi utilizada para desenvolver uma estrategia para a quantificacao de cloreto. Amostras contendo de 2,2 a 3,7 mol L -1 de acido sulfurico podem ser determinadas utilizando a mesma curva analitica, sem efeitos matriciais ou qualquer tratamento previo. O limite de deteccao e o desvio padrao relativo das medidas foram estimados em 0,37amg Cl - L -1 (nivel de confianca de 99,7 %) e 1,6%a(n = 10), respectivamente. A frequencia de amostragem foi 45 h -1 . Porcentagens de recuperacao entre 95,9 e 108% foram obtidas para adicoes de cloreto (2,00 a 8,00 mg L -1 ) nas amostras. A flow injection spectrophotometric system is proposed for determining chloride in lead-acid battery electrolyte by using the displacement reaction between mercury(II) thiocyanate and chloride in a medium containing iron(III). The employment of a large sample volume was effective to avoid refractive index gradients in the central part of the sample zone. Sulfate interference was studied and the correlation between the chemical equilibria involved and the transient signals was used to develop a strategy for chloride quantification. Samples containing from 2.2 to 3.7 mol L -1 of sulfuric acid can be determined by using the same analytical curve, without matrix interference or any previous treatment. The detection limit and the relative standard deviation were estimated in 0.37 amg Cl - L -1 (99.7% confidence level) and 1.6% (n = 10), respectively. The sampling rate was 45 h -1 . Recoveries between 95.9 and 108% were obtained for additions of chloride (2.00 to 8.00 mg L -1 ) in the samples.

journal of the brazilian chemical society

Overcoming the schlieren effect in flow injection spectrophotometry by introduction of large sample volumes: determination of chloride in the electrolyte of lead-acid batteries