FINAL REPORT
FINAL REPORT
FINAL REPORT
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last two steps. If the weighs after heated soils have adifference of 0.0002g or less, then stop<br />
the measurement.<br />
3. Determination of organic matter<br />
Methodology<br />
Organic carbon is determined by means of a potassium dichromate back-titration. A known<br />
excess of K 2 Cr 2 O 7 is added to the sample together with H 2 SO 4 and the organic carbon is<br />
oxidized to CO 2 :<br />
2Cr 2 O 2- 7 + 3C organic +16H + →4Cr 3+ + 3CO 2 + 8H 2 O<br />
In this reaction, 2 moles of dichromate oxidize 3 moles of carbon. The unreacted excess of<br />
dichromate remaining after reaction is determined by back-titration with ferrous sulfate:<br />
Cr 2 O 2- 7 + 6Fe 2+ +14H + →2Cr 3+ + 6Fe 3+ + 7H 2 O<br />
In this titration reaction, 1 mole of dichromate oxidizes 6 moles of Fe 2+ . Organic carbon is<br />
calculated by difference. Ferrous iron (Fe 2+ ), if present in the soil. Will interfere by reacting<br />
with chromate according to the same equations as that shown for the titration reaction above.<br />
Materials<br />
Hot plate<br />
250ml and 100ml conical flasks<br />
Burette<br />
0.4N potassium dichromate solution<br />
0.1N Standard ferrous ammonium sulfate solution<br />
0.2% Phenanthroline indicator<br />
Concentrated sulfuric acid<br />
Experimental procedure<br />
Weight 0.2g of soil, sediment or sludge and place in a conical refluxing flask. Add 10ml of<br />
the potassium dichromate solution and swirl to mix. Carefully add 10ml concentrated sulfuric<br />
acid. Dispense the acid a little at a time since it generates heat, and swirl gently to mix.<br />
Connect the flask to the condenser and turn on cooling water. Cover open end of condenser<br />
with a small beaker. Place on a hot plate and reflux for 5-10 minutes. Cooland rinse down the<br />
condenser with distilled water, collecting the water in the flask. Disconnect flask from<br />
condenser and add about 10ml water. Swirl to mix and add 4 drops of phenanthroline<br />
indicator. Titrate with ferrous ammonium sulfate to the end point, at which the color changes<br />
from blue-green to violet red<br />
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