3.3 Sample collection
• The samples were collected using plain bottles.
• They were divided into two, drops of nitric acid were added to part of the divided samples to avoid adsorption of the metals to the container wall.
• The samples were transported to the laboratory with cooler and ice pack so as to maintain the temperature of the samples and also to avoid loss of nitric acid by heat.
3.4 Raw Leachate analysis
3.4.1 Determination of COD
Reagent:
- COD standard solution
- COD digestion reagents
- Potassium Acid phthalate
- Sulphuric acid
- Mercuric acid
- Ultra-pure water
PROCEDURE:
1. 50ml of sample was homogenies for 2 minutes in a blender 0 to 15,000 mg/l. The homogenized sample was into a 100ml beaker and it was stirred with a magnetic stirrer.
2. The COD reactor was turned on and it was preheat to 1500c. The plastic shield was placed in front of the reactor.
Caution: ensure Safety devices are in place to protect analyst from splattering should reagent leaking occur.
3. The cap of a COD digestion reagent vial was removed for the appropriate range.
4. The vial was held at angle 450. 2.00ml (0.2 ml for the 0 to 15,000 mg/l) of sample was pipetted into the vial.
5. The vial cap was replaced slightly. The COD vial was rinsed with ultrapure water and the vial was wiped and cleaned with a paper towel.
6. The vial was held by the cap and over a sink. It was inverted gently several times to mix the contents. The vial was placed in the preheated COD reactor.
7. The blank was prepared by repeating steps 3 to 6 substituting 2.00ml (0.2ml for the 0 to 15,000mg/l range) ultra-pure water for the sample
8. The vials was heated for 2 hours
9. The reactor was off. The vial was waited to cool to 1200c at about 20 minutes.
10. Each vial was inverted several times while still warm. The vials was placed into a rack and waited until the vials have cooled to room temperature.
3.4.2 Determination of BOD
Reagents
1. Phosphate buffer solution (1ml each)
2. Magnesium sulphate sodium
3. Calcium chloride solution
4. Ferric chloride solution
5. H2SO4
6. NaOH
7. Sodium sulphite solution
8. Nitrification inhibitor (2-chloro-6-(trichloro methyl) pyridine
9. Glucose glutamic acid solution