Determination of sulphate in water and biodiesel samples by a sequential injection analysis--multivariate curve resolution method

Abstract

A spectrophotometric sequential injection analysis (SIA-DAD) method linked to multivariate curve resolution-alternating least squares (MCR-ALS) has been developed for sulphate determination. This method involves the reaction, inside the tubes of the SIA system, of sulphate with barium-dimethylsulphonazo (III) complex, Ba-DMSA (III), displacing Ba(2+) from the complex and forming DMSA (III). When the reaction products reach the detector a data matrix is obtained, which allows a second-order calibration to be developed. The experimental conditions (concentration and sample and reagent volumes) to obtain the highest sensitivity have been chosen applying a 2(4-1) fractional factorial design. The proposed sequential flow procedure permits up to 15 mg SO(4)(2-) L(-1) to be determined with a limit of detection of 1.42 mg L(-1) and it is able to monitor sulphate in samples at a frequency of 15 samples per hour. The method was applied to determine sulphate in natural and residual waters and in biodiesel. The reliability of the method was established for water samples by parallel determination using a standard turbidimetric method for sulphate in natural and residual water samples with results within statistical variation. For biodiesel samples, the method was validated comparing the concentration of some spiked samples with the expected concentration using a test-t.