Analytical Sciences


Abstract − Analytical Sciences, 18(12), 1361 (2002).

Chromium(III) Determination with 1,5-Diphenylcarbazide Based on the Oxidative Effect of Chlorine Radicals Generated from CCl4 Sonolysis in Aqueous Solution
Sivanildo da Silva BORGES,* Mauro KORN,**  and José Luis Fontes da COSTA LIMA***
*Instituto de Qu<ímica, Universidade Federal da Bahia, Campus de Ondina, 40.170-290 Salvador, Bahia, Brazil
**Departamento de Ci<ências Exatas e da Terra, Universidade do Estado da Bahia, Estrada das Barreiras, s/n 41194-000 Salvador, Bahia, Brazil
***CEQUP/Departamento de Qu<ímica-F<ísica, Faculdade de Farmacia, R. Anibal Cunha 164 4050-047 Porto, Portugal
Oxidation of Cr(III) during sonication in carbonated aqueous solutions saturated with CCl4 leads to the quantitative formation of Cr(VI) and provides a simple and rapid method for spectrophotometric chromium determination with 1,5-diphenylcarbazide. The key to this method is the production of chlorine radicals when aqueous solution saturated with CCl4 is exposed to ultrasonic waves of 40 kHz. The effects of sonication period, CCl4 solution volume, acidity, and interferences were discussed. The time required for a single determination is lower than 2 min. The relative standard deviation obtained for aqueous solutions with 1 ug of Cr was <2% (N = 10) and the calculated detection limit (3sigma) was 5 ng of Cr.