Robust flow-batch coulometric/biamperometric titration system: determination of bromine index and bromine number of petrochemicals.
A flow-batch system was constructed and evaluated to perform coulometric titrations with biamperometric end point detection. The flow section of the system is employed for sampling by injecting a sample volume (50-300 microL) in a flow injection-like system. About 1.5 mL of a suitable carrier solution is delivered by a peristaltic pump in order to quantitatively transfer the sample to the system titration cell (2.0 mL total inner volume). The carrier contains the coulometric precursor for the titrant species. The cell contains two pairs of platinum electrodes used for coulometric generation of reagent and biamperometric detection and is actively stirred. The titrant species is generated and the titration is performed by the usual batch procedure with the excess of titrant being detected by biamperometry following the analysis of the titration curve. System operation is computer controlled and all operations are automated, including titration curve analysis and cell cleaning after the titration is ended. The system is characterized by its robustness because its operation does not depend on flow rates, and the work using coulometric methods which generate gases at the counter-electrode is not troublesome. The flow-batch system has been evaluated for determination of bromine index and bromine number (relative to the total reactive olefin content) in petrochemicals according to an ASTM procedure. Typical precision (R.S.D.) is between 0.5 and 6% for different petrochemicals whose bromine number/index vary from 1000 to 10mg of bromine per 100g of sample, respectively. Recoveries for standard additions are between 92 and 123% for 10mg of Br(2) per 100g increments and 98 to 101% for 100mg per 100g increments. Accuracy of the proposed system was evaluated against results obtained by the standard ASTM with no significant difference detected at 95% confidence level.
Pasquini
Celio
C
Instituto de Química, Universidade Estadual de Campinas, Caixa Postal 6154-CEP, 13084-971 Campinas, SP, Brazil.
de Aquino
Emerson Vidal
EV
das Virgens Reboucas
Marcio
M
Gonzaga
Fabiano Barbieri
FB