3.2. Flow system
By considering the main interferences for nitrate determination in waters, the flow system (Fig. 1) was designed to separate nitrate from cationic and neutral species. In the injection step, anions are retained in the ion-exchange column and other species passed directly through the anionic column, being removed by the carrier stream. In the alternative position of the sliding bar injector, the column is inserted into the eluent stream and the analyte is transported towards the flow cell for measurement. It was observed with dye solutions that an intense carryover between sample and previous eluent zones occurred without employing the coil B. Thus, nitrate retention was hindered by the presence of relatively higher concentrations of perchlorate ions in the sample zone. Carryover was minimized by inserting a 300-cm long coil among the sample loop and the column and as showed in Fig. 2, sensitivity and precision were improved in this condition. On the other hand, results in Fig. 2 show that the eluent concentration (initially 0.6 mol L−1) could be reduced to 0.05 mol L−1, improving sensitivity, minimizing reagent consumption, and decreasing the acid concentration of the residues. The effects of eluent and carrier flow-rates were evaluated and the results are shown in Fig. 3. Higher signals were obtained for lower flow-rates indicating that the kinetics of nitrate retention and elution are slow. Flow rates of 1.7mLmin−1 and 4.3mLmin−1 were selected for the eluent and carrier solutions, respectively, as a compromise between sensitivity and sampling rate. It was further verified that the precision was deteriorated by memory effects caused by the incomplete removal of nitrate in the elution step. This drawback was circumvented by increasing the resting time of the injector in the elution position to 150 s.
3.2. ขั้นตอนระบบBy considering the main interferences for nitrate determination in waters, the flow system (Fig. 1) was designed to separate nitrate from cationic and neutral species. In the injection step, anions are retained in the ion-exchange column and other species passed directly through the anionic column, being removed by the carrier stream. In the alternative position of the sliding bar injector, the column is inserted into the eluent stream and the analyte is transported towards the flow cell for measurement. It was observed with dye solutions that an intense carryover between sample and previous eluent zones occurred without employing the coil B. Thus, nitrate retention was hindered by the presence of relatively higher concentrations of perchlorate ions in the sample zone. Carryover was minimized by inserting a 300-cm long coil among the sample loop and the column and as showed in Fig. 2, sensitivity and precision were improved in this condition. On the other hand, results in Fig. 2 show that the eluent concentration (initially 0.6 mol L−1) could be reduced to 0.05 mol L−1, improving sensitivity, minimizing reagent consumption, and decreasing the acid concentration of the residues. The effects of eluent and carrier flow-rates were evaluated and the results are shown in Fig. 3. Higher signals were obtained for lower flow-rates indicating that the kinetics of nitrate retention and elution are slow. Flow rates of 1.7mLmin−1 and 4.3mLmin−1 were selected for the eluent and carrier solutions, respectively, as a compromise between sensitivity and sampling rate. It was further verified that the precision was deteriorated by memory effects caused by the incomplete removal of nitrate in the elution step. This drawback was circumvented by increasing the resting time of the injector in the elution position to 150 s.
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