Analytical Chemistry Experiments

Major Experiment

1. To separate a mixture of Ni²⁺ & Fe²⁺ by complexation with DMG and extracting the Ni²⁺- DMG complex in chloroform and determine its concentration by spectrophotometry.
2. Solvent extraction of zirconium with amberliti LA-1, separation from a mixture of iron and gallium.
3. Determination of Na, Ca, Li in cola drinks and fruit juices using flame photometric techniques.
4. Estimation of calcium, magnesium, phosphate, nitrate in soil sample.
5. Determination of pKa values of indicator using spectrophotometry.
6. Determine the composition of the Ferric-salicylate/ ferric-thiocyanate complex by Job’s method.
7. Determination of exchange capacity of cation exchange resins and anion exchange resins.
8. Separation of metal ions from their binary mixture using ion exchange chromatography.
9. Separation of amino acids from organic acids by ion exchange chromatography.
10. To determine conductometrically the second order rate constant for the hydrolysis of ethyl acetate by sodium hydroxide.

Minor Experiment

1. Determination of pH of soil sample and estimate total soluble salt in this soil sample.
2. To determine the specific conductivity of soil sample.
3. Record an absorption spectrum of a substance (KMnO₄/K₂Cr₂O₇) using a spectrophotometer and determine absorption maxima.
4. To verify the Beer-Lambert law for a compound (potassium permanganate, copper sulphate, methylene blue etc.) and determine the concentration of the substance using calibration curve.
5. Chromatographic separation (TLC) and identification on the basis of Rf values of -

1. Mixture of Sudan Yellow and Sudan Red (Azo dyes)
2. Active ingredients of plants, flowers, fruit juices and identify them on the basis of their Rf values.
3. Mixture of organic compounds

Demonstrations

1.  Determination of dissolved oxygen in water.
2.  Determination of chemical oxygen demand (COD).
3.  Determination of Biological oxygen demand (BOD).

Scheme of Examination

The duration of examination will be 4 hrs.

The following exercises will be set in the examination

Major Experiment                                                      38 marks

Minor Experiment                                                      20 marks

Viva                                                                           12 marks

            Total                                                                          70 marks

1.Analytical Chemistry Experiments

The students will be allotted two experiments to perform in the lab. The exercises can be modified by the examiners and the same will be explained to the candidates. However, such modifications

 will not involve any departure from the basic principles over which experiments are prescribed in the syllabus.

Candidates shall be given one major and one minor exercise out of the exercises prescribed in the syllabus. The distribution of marks will be as follows:

                                                 Major                        Minor

• Theory and procedure         8 marks                      4 marks
• Correct observation             8 marks                      5 marks
• Use of correct formula         8 marks                      4 marks
• Calculation                          8 marks                      5 marks
• Result                                  6 marks                      2 marks

No marks for calculation will be awarded to a candidate for not calculating result.

The permissible error will depend on the nature of the experiment. One mark shall be deducted for each + 2% error over permissible limit.

2.Viva

Oral questions shall generally be asked over the work assigned to the candidate. The purpose is to find out as to what extent the candidate has understanding the basic principles.