Expt No: 17 DETERMINATION OF IRON BY PHENANTHROLINE METHOD

Aim: To determine the concentration of iron in the given water sample

Apparatus: Standard volumetric flasks (100mL), Pipettes, Spectrophotometer

Reagents:
1. Hydroxyl hydrochloride solution
2. Ammonium acetate buffer solution
3. 1,10-Phenanthroline solution
4. Stock iron solution

Principle:
In the Phenanthroline method, the ferric form of iron is reduced to ferrous form by
boiling with hydrochloric acid and hydroxylamine hydrochloride. The reduced iron chelates with
1,10 phenanthroline at pH 3.2 – 3.3 to form a complex of orange-red color. The intensity of
colour is proportional to the concentration of iron and obeys beer’s law.

Procedure:

1. Take six 100 mL glass stoppered standard volumetric flasks (five for standards & one for the
sample).
2. Prepare standard iron solutions in the range of 0 to 0.4 mg/L by diluting appropriate
quantities of stock solution to 100 mL with distilled water.
3. Now add stock iron solution of concentration 10mg/L in varied range of 0, 1, 2, 3 and 4mL
to five volumetric flasks to obtain standard iron solution.
4. Add 2mL of Hydroxyl hydrochloride solution and 1mL of sodium acetate solution to each
flask followed by 2mL of 1,10-phenanthroline solution to all five flasks.

5. Make up the contents of each flask exactly to 100mL by adding distilled water and allow
atleast 5-10 minutes for maximum color development.

6. To the sixth standard flask add all the above reagents in the same proportion and make it up
to 100mL using sample.
7. Measure the absorbance using UV-Visible spectrophotometer at 510nm.
8. Using the spectrophotometer values draw a standard graph and calculate the concentration of
 iron in given water sample.

Tabulation:
Concentration of Volume of stock
Sl No. Absorbance
standards solution
1 0
2 0.1
3 0.2
4 0.3
5 0.4
6 Sample

Result:

The concentration of iron in the water sample=

Inference
Comment on your result.
Expt No: 18 DETERMINATION OF CHEMICAL OXYGEN DEMAND (COD)

Aim: To determine the COD of the given wastewater sample

Apparatus:
1. Burette.
2. COD Digestor
3. Conical flask
4. Refluxing flask and condenser

Reagents:
1. Std Potassium-dichromate solution
2. Sulphuric acid containing silver sulfate
3. Std Ferrous ammonium sulphate( 0.1 N)
4. Ferroin indicator
5. Mercuric sulphate (HgSO4)

Principle:
Chemical oxygen demand (COD) is defined as the amount of oxygen required for the
chemical oxidation of organic matter in wastewater with the help of strong oxidizing agents such
as KmnO4 and K2Cr2O7
The intrinsic limitation of the test lies in its inability to differentiate between the biologically
oxidisable and biologically inert material.
COD determination has advantages over BOD determination, the result can be obtained by COD
test within 3 hours, where as it takes 5 days in BOD test. Further the test is relatively easy, gives
reproducible results and is not affected by interferences as in BOD test.
The organic matter gets oxidized completely by K2Cr2O7 in the presence of H2SO4 to produce
CO2 and H2O. The excess K2Cr2O7 remaining after the reaction is treated with Ferrous
Ammonium Sulphate .The dichromate consumed gives the oxygen required for oxidation of the
organic matter.

Procedure:

1. Place 0.4 gm mercuric sulphate in a reflux flask and transfer 20mL of sample.
2. Add glass beads followed by 10mL Std potassium dichromate solution.
3. Add slowly 30mL sulphuric acid containing silver sulphate, mixing thoroughly.
4. Connect flasks to the condenser and mix the contents before heating. Reflux for a minimum
period of 1.5-2 hours, cool and wash down the condenser with distilled water
5. Dilute to about 150mL, cool and titrate excess potassium chromate against FAS solution.
6. Take 50mL of above solution in conical flask and titrate against 0.1 N ferrous ammonium
sulphate solution using ferroin indicator.
7. Colour change from blue green to wine red indicates the end point.
8. Reflux the blank in the same manner using distilled water instead of the sample.

Tabulation:

Volume of Burette Reading Volume consumed in

Sl.No
sample in mL Initial Final mL
1
2
3

Calculation:

COD, mg/lt = (A-B) x N of ferrous ammonium sulphate x 1000 x 8

________________________________________
mL of sample

Where A-mL of titrant consumed for blank

B-mL of titrant consumed for sample

Result:

The amount of COD present in the given sample =

Inference
Comment on your result.