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Determination of Chemical Oxygen Demand (COD) In Water and Wastewater 2.0 OBJECTIVE

To determine the amount of organic pollutant in water and wastewater 3.0 INTRODUCTION

Chemical oxygen demand (COD) is used as a measure of oxygen requirement of a sample that is susceptible to oxidation by strong chemical oxidant. The dichromate reflux method is preferred over procedures using other oxidants (e.g. potassium permanganate) because of its superior oxidizing ability, applicability to a wide variety of samples and ease of manipulation. Oxidation of most organic compounds is 95-100% of the theoretical value. The mg/L COD results are defined as the mg of O2 consumed per liter of sample under conditions of this procedure. In this procedure, the sample is heated for two hours with a strong oxidizing agent, potassium dichromate. Oxidizable organic compounds react, reducing the dichromate ion (Cr2O72-) to green chromic ion (Cr3+). When the 3-150 mg/L colorimetric or titrimetric method is used, the amount of Cr6+ remaining is determined. When the 20-1,500 mg/L or 200-15,000 mg/L colorimetric method is used, the amount of Cr3+ produced is determined. The COD reagent also contains silver and mercury ions. Silver is a catalyst, and mercury is used to complex chloride interferences. Test results for the 3 to 150 mg/L range are measured at 420 nm. Test results for the 20 to 1, 5000 and the 200 to 15,000 mg/L range are measured at 620 nm.

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MATERIALS & METHODOLOGY

COD Digestion Reactor Spectrophotometer, HACH DR/2400 @ DR/2800 COD Digestion Reagent Vial LR @ HR COD rack Volumetric pipette, 2 mL Paper towel/Tissue 1. Homogenize 100 mL of sample for 30 seconds in a blender. *For samples containing large amounts of solids, increase the homogenization time. 2. For the 200-15,000 mg/L range or to improve accuracy and reproducibility of the other ranges, pour the homogenized sample into a 250-mL beaker and gently stir with a magnetic stir plate. *If the sample does not contain suspended solids, omit step 1 and step 2. 3. 4. 5. 6. 7. 8. Turn on the COD Reactor. Preheat to 150C. Place the safety shield in front of the reactor. Remove the caps from two COD Digestion Reagent Vials. *Be sure to use vials for the appropriate range. Hold one vial at a 45-degree angle. Use a clean volumetric pipette to add 2.00 mL of sample to the vial. This is the prepared sample. Hold a second vial at a 45-degree angle. Use a clean volumetric pipette to add 2.00 mL de-ionized water to the vial. This is the blank. Cap the vials tightly. Rinse them with de-ionized water and wipe with a clean paper towel. Hold the vials by the cap over a sink. Invert gently several times to mix. Place the vials in the preheated COD Reactor. *The sample vials will become very hot during mixing. 9. 10. Heat the vials for two hours. Turn the reactor off. Wait about 20 minutes for the vials to cool to 120C or less.

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Invert each vial several times while still warm. Place the vials into a rack and cool to room temperature. Touch Hach Programs. Select program 430 COD LR (Low Range) or 435 COD HR (High Range/High Range Plus). Touch Start. Clean the outside of the vials with a damp towel followed by a dry one to remove fingerprints or other marks. Install the 16-mm adapter. Place the blank into the adapter. Touch Zero. The display will show: 0 mg/L COD. When the timer beeps, place the sample vial into the adapter. Touch Read. Results will appear in mg/L COD.

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RESULTS & DISCUSSIONS Sample (different sources) COD, mg/L

Your discussion may include the following questions: 1. Explain the differences of COD values found in the different sources of sample. 2. State the importance to determine COD in water and wastewater, and interpret your test results based on Environment Quality Act 1974 Standard A or B, Sewage & Industrial Effluent. 3. Write the chemical reactions involved in the digestion process in determining COD. 4. A sample is collected for COD analysis and it is to be performed on the following day. Describe two ways which the sample can be preserved. Why it is necessary to preserve the sample? 5. Briefly explain a chemical treatment to reduce COD.

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REFERENCES

Andrew, D. E., Lenore, S. C., Eugene, W. R. & Arnold, E. G. 2005. Standard Methods For The Examination of Water And Wastewater. 21st Edition. USA. Howard, S. P., Donald, R. R. & George, T. 1985. Environmental Engineering. McGrawHill. Singapore. Kasmawati, M. & Lee, K. K. 2007. Methods of Analysis for Water and Wastewater. UiTM. Shah Alam.