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Previous issue date: 2017-07-28 === Ag?ncia Nacional de Petr?leo - ANP === O cloreto ? considerado um dos principais contaminantes do petr?leo, pois interfere no processo de transporte e refino e pode ser transferido para os produtos derivados finais. Durante o refino, a presen?a de cloreto pode levar a forma??o de HCl, causando s?rios problemas de corros?o. Nesse sentido, foi desenvolvida uma metodologia para determina??o de cloro em amostras de petr?leo, preparadas sob a forma de emuls?es, por espectrometria de absor??o molecular de alta resolu??o com fonte cont?nua atrav?s da mol?cula diat?mica MgCl no comprimento de onda 377,01 nm. O preparo da emuls?o foi otimizado atrav?s de um planejamento experimental Centroid-Simplex. As condi??es ?timas de preparo das emuls?es foram: 0,5mL HNO3 5% (v/v), 0,5mL de xileno e 2 mL de uma mistura dos solventes n-Propanol/ Triton X-100 na propor??o 5:1. A massa de amostra de petr?leo foi de cerca de 0,20g. Magn?sio foi usado como precursor da mol?cula de MgCl, e a concentra??o otimizada foi de 10 g L-1. Os estudos da propor??o entre Mg e Cl para favorecimento da forma??o da mol?cula mostraram que para garantir a m?xima forma??o da mol?cula de MgCl ? necess?rio utilizar uma raz?o em massa de pelo menos 500 Mg:1 Cl. Uma massa de 5 ?g de Pd foi introduzida ? cada ciclo de inje??o como modificador qu?mico, para aumentar a estabilidade t?rmica da esp?cie molecular. As temperaturas de pir?lise e vaporiza??o otimizadas foram 800 ?C e 2300 ?C, respectivamente. Para an?lise de cloro, foram utilizadas oito amostras de petr?leo da Bacia Potiguar e dois materiais de refer?ncia certificados, ?leo lubrificante aditivado (NIST 1848) e a de ?leo combust?vel (NIST 1634c), foram utilizados para a verifica??o da exatid?o do m?todo. A estrat?gia de calibra??o contra padr?es aquosos foi poss?vel, obtendo-se o LOD de 5 mg kg-1. Testes de adi??o/recupera??o foram realizados e os valores obtidos ficaram na faixa entre 92 e 117%. A metodologia proposta mostra-se simples, r?pida com preparo de amostra simplificado. === Chloride is considered an important contaminant of petroleum as it interferes with the process of transportation and refining and can be transferred to the final product derivatives. During refining, the presence of chloride may lead to the formation of HCl, causing serious corrosion problems. A methodology for the determination of chlorine in petroleum samples prepared by emulsions was developed by high resolution molecular absorption spectrometry with continuum source through the diatomic molecule MgCl, in the wavelength 377.01 nm. The preparation of the emulsion was optimized through centroid-simplex design. The conditions of preparation of the emulsions were: 0.5 mL of 5% (v / v) HNO3, 0.5 mL of xylene and 2 mL of a mixture of n-Propanol / Triton X-100 solvents in the ratio 5:1. The crude oil mass used was about 0.20 g. Magnesium was used as the precursor of the molecule, the optimized concentration was 10 g L-1. The proportional studies between Mg and Cl for the formation of molecules show that to ensure the formation of a MgCl molecule is required for a mass ratio of at least 500 Mg: 1 Cl. A mass of 5 ?g of Pd was introduced at each cycle that chemical modifier for increase the thermal stability of the molecular species. The optimized pyrolysis and vaporization temperatures were 800 ? C and 2300 ? C, respectively. For chlorine analysis, eight crude oil samples from the Potiguar Basin and two certified reference materials, lubricated oil (NIST 1848) and fuel oil (NIST 1634c) were used, to verify the accuracy of the method. The calibration strategy against aqueous standards was possible, obtaining the LOD of 5 mg kg-1. Addition / recovery tests were performed and the values obtained were between 92 and 117%, values acceptable analytically. The proposed methodology is simple, fast with simplified sample preparation.
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