In this article, we report a new method that involves adsorption, oxygen bomb combustion, and ion chromatography for the preconcentration and determination of adsorbable organic halogen. This method can be divided into four steps, including: macroporous resin adsorption enrichment, optimization, oxygen bomb combustion, and ion chromatography determination. The project studies the macroporous resin adsorb organic halide pollutants and subsequent burn by an oxygen bomb combustion analyzer. The organic halogen in the aerobic environment combusts into hydrogen chloride. The water absorbing hydrogen chloride was then determined by ion chromatography. The influences of some adsorption and combustion parameters, such as the adsorption time, adsorption solution volume, solution pH, hexachlorobenzene acid concentration, combustion oxygen pressure, among others, on their respective adsorption efficiency were investigated. In the optimal condition, the adsorption time was 3.5 h; solution volume was 20 mL; pH was 4; combustion absorption time was 15 min; and the chloride calibration working range was from 1 ppm to 20 ppm (R 2 = 0.9998). Finally, the proposed method was successfully applied to the determination of organic halogen in water samples. The recoveries of chlorine (at spiked concentrations of 10 ppm and 20 ppm into water) in real samples ranged from 92.2% to 101.0%. Intra-day precision (N = 3) in terms of peak area, expressed as relative standard deviation, was found to be within the range of 0.68%–1.97%.
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