RESUMO
A downscaling in true titration based on a simple sequential injection analysis-lab-at-valve (SIA-LAV) has been proposed. A titrant solution was stepwise aspirated into a titration LAV chamber and a titration curve was obtained by monitoring the change in the solution color spectroscopically. This fully-automated SIA-LAV system required less volume of the sample/reagents, only a micro-liter scale, compared to the conventional method. The system was investigated with complexometric titration and acid-base titration. Application of the developed technique to some real samples has been demonstrated.
RESUMO
Flow injection (FI) was coupled to ion-pair reversed phase high performance liquid chromatography (IP-RPHPLC) for the simultaneous analysis of some metal-4-(2-pyridylazo) resorcinol (PAR) chelates. A simple reverse flow injection (rFI) set-up was used for in-line complexation of metal-PAR chelates prior to their separation by IP-RPHPLC. The rFI conditions were: injection volume of PAR 85muL, flow rate of metal stream 4.5mLmin(-1), concentration of PAR 1.8x10(-4)molL(-1) and the mixing coil length of 150cm. IP-RPHPLC was carried out using a C(18)muBondapak column with the mobile phase containing 37% acetonitrile, 3.0mmolL(-1) acetate buffer pH 6.0 and 6.2mmolL(-1) tetrabutylammonium bromide (TBABr) at a flow rate of 1.0mLmin(-1) and visible detection at 530 and 440nm. The analysis cycle including in-line complexation and separation by IP-RPHPLC was 16min, which able to separate Cr(VI) and the PAR chelates of Co(II), Ni(II) and Cu(II).