SET: A

M. Sc. II Analytical Chemistry

(Semester – III)
M. Sc. – AC 311 T: Electrochemical and Thermogravimetric Methods of Chemical
Analysis
Examination -2023 (2021 Credit System Pattern)
Time: 3 Hrs. Max. Marks: 70

Instructions:
1) Question No. 1 and 5 are compulsory.
2) Question No. 2 to 4 and 6 to 8 carry equal marks.
3) Solve any two questions from 2 to 4 and 6 to 8.
4) Figures to right side indicate full marks.
5) Neat and labeled diagrams must be drawn wherever necessary.
6) Answers to two sections should be written on separate answer sheet.

SECTION – I
Q 1) A] Attempt ANY FOUR of the following [8]
i) Define a) Polarization b) Overvoltage
ii) Explain the term Supporting electrolyte.
iii) Define a) Polarography b) Voltammetry
iv) What is diffusion current?
v) What is anodic Stripping method?
B] Write a note on hydrodynamic voltammetry. [3]

Q 2) A] Explain in detail controlled potential coulometry. [6]

B] Attempt ANY TWO of the following [6]
i) The diffusion coefficient of Cd having concentration 3*10 moles per liter is 0.72*10-5
2+ -3

cm2/sec. If the capillary characteristics are t=4 seconds and m=3 mg/sec. Calculate the
diffusion current for cadmium.
ii) Discuss in detail organic application of voltammetry.
iii) Write a short note on dropping mercury electrode.

Q 3) A] Explain in detail amperometry titration. [6]

B] Attempt ANY TWO of the following [6]
i) Draw a neat labelled diagram of voltammogram and explain terms in it.
ii) State Ilkovic equation & explain terms involved in it.
iii) Distinguish between diffusion and migration

Q 4) Attempt ANY THREE of the following [12]

i) Write a note on square wave voltammetry.
ii) Distinguish between working electrode and reference electrode.
 iii) Give comparison between coulometric and conventional titration
iv) Explain cyclic voltammogram of K3[Fe (CN)6]

SECTION – II
Q 5) A] Attempt ANY FOUR of the following [8]
iv) Give factors affecting thermal analysis.
v) Define thermogravimetric analysis.
vi) State the principle of dynamic mechanical analysis.
iv) What is evolved gas analysis?
vi) Distinguish between the term differential and derivative.
B] Write a note on heat flux differential scanning calorimetry. [3]

Q 6) A] Describe the components of differential thermal analysis with schematic diagram. [6]
B] Attempt ANY TWO of the following [6]
i) A mixture of CaCO3 and CaO is analyzed using TGA technique. TG curve of the sample
indicates that there is a mass change from 260.5 mg to 200.3 mg between 600-900oC.
Calculate the percentage of CaCO3 in the sample? [Given Atomic weight Ca = 40.0, C =
12.0, O =16.0 and H = 1.0]
ii) Discuss any one application of thermomechanical analysis.
iii) Explain any one application of simultaneous TG-DTA.

Q 7) A] Explain instrumentation of thermomechanical analysis with diagram. [6]

B] Attempt ANY TWO of the following [6]
i) Explain DTA curve for calcium oxalate monohydrate in nitrogen and air atmosphere.
ii) Write a note on TA infrared.
iii) Draw and explain the thermogram of magnesium hydroxide Mg(OH)2

Q 8) Attempt ANY THREE of the following [12]

v) Discuss apparatus for thermogravimetric analysis with block diagram.
vi) Explain any one application in physical changes and measurement for DTA.
vii) A thermogram of a magnesium compound shows a loss of 45.0 mg from a total of 87.0
mg used for analyte. Identify the compound either as MgO, MgCO3 or MgC2O4. [Atomic
weight Mg = 24.0, C = 16.0 and O = 16.0]
viii) Explain kinetic diversion in thermal analysis.