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Precipitation reactions of halide ions (Cl−, Br− or I− ion) with Ag ion produce precipitates of characteristic colors AgCl (white), AgBr (creamy), and AgI (yellow). And such characteristic colors of silver halides can be used to identify the existence of each individual halide ion. However, it has not been easy to identify each constituent ion in solutions of various binary/tertiary mixtures of halide ions. While several methods for the separation and determination of halide ions in aqueous samples using electrochemical, optical, and chromatographic, and capillary electrophoretic techniques have been reported, they all require sophisticated devices and involve complex procedures. The proposed method presented in this paper involves a rather simple anion exchange chromatography equipped with a reflectance detector and especially shows its ability to achieve quantitative chromatographic separation of I− ion from its mixtures with Cl− and Br− ions. Analysis System. Figure 1 shows a schematic diagram of the anion exchange chromatography equipped with a reflectance detector. The first channel (A) from a HPLC pump (B) carries deionized water (1.0 mL/min) through a sample injection valve (C, Rheodyne 6-port sample injection valve) equipped with a sample loop of 0.50 mL into the anion exchange column (F, Dionex IonPac AS4A-SC). The effluent from the column meets with the stream of the second channel from a peristaltic pump (D, Ismatec MV) carrying 0.10 M AgNO3 solution (0.10 mL/min) at the mixing Tee. The precipitation reaction between halide ions in the effluent and Ag ion in the second stream begins to take place and is completed while the mixed solution flows through a delay line (Figure 2-B, PTFE tubing of 1 mm i.d., 5 cm in length). Then, the resulting solution containing fine silver halide precipitate particles is introduced into the optical detection system (Figure 2-D, windowless optical cell). And the intensity of reflected light is recorded vs. time at a chart recorder (R). Windowless Optical Detection System. Figure 2 shows the cross sectional view of the windowless optical detection system. The resulting solution containing fine silver halide precipitate particles formed by the reaction between the halide ions in the first stream (A) and Ag ion from the second stream (C) at the mixing T (B) is introduced through a delay line (D) into the optical detection system (housed in a black PVC compartment (J). The formation and falling of droplets (E) of the solution occurs continuously at the bottom outlet of the delay line. The light from the radiation source (I, high luminescence blue light emitting diode) guided through a glass tubing (H, 4.5 mm i.d.) is shed over surface of each droplet (G) throughout its lifetime and the intensities of reflected light are measured at the radiation detector (F, a blue sensitive photodiode) placed on the same side with the radiation source. Two black PVC tubes are connected at the bottom of the compartment to be used for drain. Proper Eluent and Efficiency. The eluent should meet a couple of requirements to be considered useful for the current chromatographic analysis. First, the anion of the eluent must exhibit sufficient affinity towards the anion exchanger used in this study. That is, since the selectivity order of the anion exchanger used in this study was (I− >

Quantitative Separation of Cl-, Br-, and I-Ions by Anion Exchange Chromatography Equipped with a Reflection Detector

Quantitative Separation of Cl^-, Br^-, and I^-Ions by Anion Exchange Chromatography Equipped with a Reflection Detector