ABSTRACT
A multisyringe flow injection analysis system was used for the determination of hypochlorite in cleaning agents, by measurement of the native absorbance of hypochlorite at 292 nm. The methodology was based on the selective decomposition of hypochlorite by a cobalt oxide catalyst giving chloride and oxygen. The difference of the absorbance of the sample before and after its pass through a cobalt oxide column was selected as analytical signal. As no further reagent was required this work can be considered as a contribution to environmental friendly analytical chemistry. The entire analytical procedure, including in-line sample dilution in three steps was automated by first, dilution in a stirred miniature vessel, second by dispersion and third by in-line addition of water using multisyringe flow injection technique. The dynamic concentration range was 0.04-0.78 gL(-1) (relative standard deviation lower than 3%), where the extension of the hypochlorite decomposition was of 90+/-4%. The proposed method was successfully applied to the analysis of commercial cleaning products. The accuracy of the method was established by iodometric titration.
ABSTRACT
A novel optical fiber reflectance sensor is coupled to a multisyringe flow injection system (MSFIA) for the preconcentration and determination of 1-naphthylamine (NPA) in water samples using C18 disks (octadecyl groups). NPA, being a first-class carcinogen, is important from a toxicological point of view and, therefore, its quantification is of considerable interest. In this study, the Griess reaction is used for sensitive and selective spectrophotometric determination of NPA. The reaction involves conversion of nitrite into nitrous acid in acidic medium followed by diazotization of sulphanilic acid and formation of a diazonium salt. The diazonium salt is then combined with NPA to form 4-(sulphophenylazo)-1-naphthylamine, an azo dye. This compound is subsequently retained onto a C18 disk followed by spectrophotometric detection at 540 nm, and it is then eluted with methanol in water (80%, v/v), so that the C18 disk is regenerated for subsequent experiments. Under the established optimum conditions, a calibration graph for NPA was constructed. Good linearity was observed within a concentration range from 10 to 160 microg l(-1). The lineal regression equation is A=(0.0027+/-0.0001) [NPA]+(0.0296+/-0.0047), r=0.9991; relative standard deviation values obtained from the analysis of 10 samples of 10, 80 and 160 microg l(-1) are 4.7, 1.2 and 0.6%, respectively. The mean value relative errors for concentrations of 10, 80, 160 microg l(-1) are 3.4, 0.9 and 0.4%, respectively. The detection and quantification limits were 1.1 and 3.7 microg l(-1). A sampling throughput of 14 injections per hour is achieved. The repeatability calculated for five different C18 disks was E(rel)=2.8%. The proposed technique has been validated by replicate analysis (n=6) of several water samples with spiked NPA, giving satisfactory results.
