Determination of Chlorine Dioxide by UV-1200 Spectrophotometry - Master's thesis - Dissertation

Spectrophotometric Determination of Chlorine Dioxide

Key words: spectrophotometry; chlorine dioxide (ClOâ‚‚); US analytical instrument; V-1200

This method describes a reliable and accurate procedure for the spectrophotometric determination of chlorine dioxide. The process involves the preparation of a standard stock solution, calibration curve development, and sample analysis. (1) **Preparation of Chlorine Dioxide Standard Stock Solution**: To prepare the stock solution, 300 mL of distilled water is placed in Flask A. One end of a glass tube is connected to an air compressor, while the other end is attached to Flask B, a high-strength borosilicate glass bottle equipped with three glass tubes. The first tube introduces air into the flask, the second connects to a dropping funnel, and the third allows gas to escape. Sodium chlorite (10 g) is dissolved in 750 mL of water and transferred into Flask B. A 20 mL portion of 10% sulfuric acid is added to the separating funnel. Flask C contains a saturated sodium chlorite solution, while Flask D, a 2 L borosilicate glass collection bottle, holds 1500 mL of water to absorb the generated ClO₂. The system is placed inside a fume hood for safety. Once the setup is complete, the air compressor is turned on, and 5 mL of sulfuric acid is added every 5 minutes. After the final addition, the airflow continues for an additional 30 minutes. The resulting yellow solution is collected in a brown bottle and stored at 4°C. The concentration should range between 250 mg/L and 600 mg/L. (2) **Preparation of Chlorine Dioxide Standard Solution**: Before use, a measured volume of the stock solution is diluted with double-distilled water to obtain a working concentration of 250 mg/L. (3) **Construction of the Calibration Curve**: A series of standard solutions are prepared by diluting the 250 mg/L solution to concentrations of 0, 10, 25, 50, 100, 150, 200, and 250 mg/L in 100 mL volumetric flasks. Each solution is measured for absorbance at 430 nm using distilled water as the blank. A linear regression is performed between the mass of ClO₂ (in mg) and the corresponding absorbance values, and a standard curve is plotted. (4) **Sample Analysis**: For sample measurement, the disinfectant solution or its diluent is analyzed directly. The absorbance at 430 nm is recorded, with distilled water as the reference. The concentration of ClO₂ in the sample is determined using the standard curve equation. (5) **Calculation**: The chlorine dioxide content (X) in mg/L is calculated using the formula: **X = ρ × (V₁ / V₂)** Where: - ρ is the concentration obtained from the standard curve (mg/L), - V₁ is the volume of the diluted disinfectant (mL), - V₂ is the original volume of the disinfectant (mL). The method has a detection limit of 10 mg/L and a linear range from 10 mg/L to 250 mg/L. The average recovery rate is 103.3%, and the relative standard deviation is less than 10%. This technique is suitable for routine monitoring of chlorine dioxide in water treatment and disinfection applications. Key words: spectrophotometry; chlorine dioxide (ClO₂); US analytical instrument; V-1200

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