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Chemical Oxygen Demand (Cod)

Chemical Oxygen Demand (Cod)

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CHEMICAL OXYGEN DEMAND (COD)
 
Chemical oxygen demand (COD) is used as a measure of oxygen requirement of asample that is susceptible to oxidation by strong chemical oxidant. The dichromatereflux method is preferred over procedures using other oxidants (eg potassiumpermanganate) because of its superior oxidizing ability, applicability to a wide varietyof samples and ease of manipulation. Oxidation of most organic compounds is 95-100% of the theoretical value.
Dichromate Reflux Technique Standard Method.
Equipment Required
1.
500-millilitre (ml) Erlenmeyer flask with standard (24/40) tapered glass joints
 
2.
Friedrichs reflux condensers (12-inch) with standard (24/40) tapered glass joints
 
3.
Electric hot plate or six-unit heating shelf 
 
4.
Volumetric pipettes (10, 25, and 50ml capacity)
 
5.
Burette, 50 ml - 0.1 ml accuracy
 
6.
Burette stand and clamp
 
7.
Analytical balance, accuracy 0.001gram (g)
 
8.
Spatula
 
9.
Volumetric flasks (1,000ml capacity)
 
10.
Boiling beads, glass
 
11.
Magnetic stirrer and stirring bars
 
Chemicals Required
1.
Potassium dichromate (K
2
Cr 
2
O
7
) 0.25N
 
2.
Sulphuric acid (H
2
SO
4
) / silver sulphate (Ag
2
SO
4
) solution
 
3.
Mercuric sulphate (HgSO
4
) crystals
 
4.
Ferrous ammonium sulphate (FAS) [Fe(NH
4
)
2
(SO
4
)
2
], approximately 0.01N
 
5.
Ferroin indicator (1, 10-phenanthroline and ferrous ammonium sulphate)
 
Caution:
In carrying out the following procedures, use proper safety measures,including protective clothing, eye protection, and a fume hood. Reagents containingheavy metals (HgSO
4
and Ag
2
SO
4
) should be disposed of as toxic wastes.
 
Chemical Preparation
1.
Dissolve 12.259g of oven-dried (primary standard grade dried at 103
o
C to aconstant weight) potassium dichromate in distilled water and dilute to 1 litrevolume in a volumetric flask.
 
2.
Add 22g of reagent grade silver sulphate to a 4kg bottle of concentratedsulphuric acid (H
2
SO
4
) and mix until the silver sulphate goes into solution.
 
3.
Use 1 g of mercuric sulphate (HgSO
4
) to complex 100 mg chloride (2,000mg/l).
 
 
4.
Dissolve 1.485g of 1,10-phenanthroline monohydrate and 0.695g of ferrousammonium sulphate heptahydrate in distilled water and dilute toapproximately 100ml. (Alternatively, this indicator may be purchased asFerroin Indicator from most scientific suppliers.)
 
5.
Dissolve 39g reagent grade ferrous ammonium sulphate hexahydrate indistilled water. Add 20ml of concentrated sulphuric acid (H
2
SO
4
). Cool anddilute to exactly 1 litre in a volumetric flask using distilled water. The ferrousammonium sulfate (FAS) titrant must be standardized daily by the followingprocedure:Dilute 10ml of standard potassium dichromate (K
2
Cr 
2
O
7
) solution to 100mlwith distilled water. Slowly add 30ml of concentrated sulphuric acid and coolto room temperature. Titrate with ferrous ammonium sulphate titrant, using 2to 3 drops (0.10 to 0.15 ml) of Ferroin indicator.Normality of FAS = (ml K
2
Cr 
2
O
7
)(0.25)ml FAS requiredThe deterioration of FAS can be decreased if it is stored in a dark bottle.
Procedure
1.
Place a 50ml sample or an aliquot diluted to 50ml in a 500ml refluxing flask.The blank is prepared using 50ml of distilled water. This is a precisemeasurement and a 50ml volumetric pipette should be used.Refer to CODRange and Sample Size below for dilution.
 
2.
Add 5 to 7 glass boiling beads.
 
3.
Add 1g of mercuric sulphate (HgSO
4
), 5ml of concentrated sulphuric acid /silver sulphate solution, and mix until the HgSO
4
is in solution. The function of the mercuric sulphate is to bind or complex chlorides. One gram may not berequired if the chloride concentration is low.
 
(Caution: Always add acid slowlydown the side of the flask while mixing to avoid overheating. It may benecessary to use gloves because of the heat generated.)
 
4.
Accurately add 25ml of 0.25 N potassium dichromate (K
2
Cr 
2
O
7
) and mix.
 
5.
Add while mixing, an additional 70ml of concentrated sulphuric acid-silver sulphate solution.
 
6.
After thorough mixing, attach the flask to the reflux condenser, apply heat,and reflux for 2 hours. Refluxing time can be decreased depending on theease of oxidation of organic materials. This time may be determined byrefluxing for periods from 15 minutes to 2 hours and comparing the results.
 
7.
A reagent blank containing 50ml of distilled water treated with the samereagent as the sample should be refluxed with each set of samples.
 
8.
Cool the apparatus to room temperature after the refluxing period. Washdown the interior of the condenser and flask twice with approximately 25mlportions of distilled water.
 
9.
Remove flask from the condenser and dilute to a final volume of approximately 350ml with distilled water.
 
10.
Add 4 to 5 drops of Ferroin indicator and a magnetic stirring bar.
 
 
11.
Place flask on a magnetic stirrer and rapidly titrate with 0.1 N ferrousammonium sulphate to the first red-brown endpoint.
 
Caution:
Use care in titration. The endpoint is very sharp and may bereached rapidly.
 
Formula to determine COD:
COD (mg/l) = (a-b)(N) x 8,000
/
sample size (ml)Where:a = ml Fe(NH4)2(SO4)2 used for blankb = ml Fe(NH4)2(SO4)2 used for sampleN = normality of FAS titrant (Fe(NH
4
)
2
(SO
4
)
2
)ml sample = the actual volume of sample used before dilution
 
Sources of Error 
1.
The largest error is caused by using a nonhomogeneous sample. Every effortshould be made to blend and mix the sample so that solids are never excluded from any aliquot.
 
2.
Always use the largest sample practical and use the largest glassware that isin keeping with good laboratory practice.
 
3.
Use volumetric flasks and volumetric pipettes with a large bore.
 
4.
The K
2
Cr 
2
O
7
oxidizing agent must be precisely measured. Use a volumetricpipette and use the same one each time if possible.
 
5.
When titrating, be certain that the burette is clean and free of air bubbles.
 
6.
Always read the bottom of the meniscus and position the meniscus at eyelevel.
 
COD Range and Sample Size
COD Range(mg/l)50-800100-1500240-3700480-75001200-188002400-370040000-375000Volume of Sample (ml)5025105210.1All samples high in solids should be blended for 2 minutes at high speed and stirredwhen an aliquot is taken. Sample volumes less than 25ml should not be pipetteddirectly, but serially diluted and then a portion of the diluent removed:
 
1.
500ml of sample diluted to 1,000 ml = 0.5 ml sample/ml of diluent, .: 50 ml of diluent = 25 ml of sample.
 
2.
100 ml of sample diluted to 1,000 ml = 0.1 ml sample/ml diluent, .: 50 ml of diluent = 5 ml of sample.
 
Elimination of Interference
One gram of mercuric sulphate (HgSO
4
) will complex 100mg of chloride in a 50mlsample (2,000 mg/l). For samples higher in chloride more HgSO
4
should be used inthe ratio of 10:1 HgSO
4
.
 

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