Course

Unit 1:

Errors, Statistics, and Sampling [10 h]Theoretical principles of qualitative and quantitative analysis. Types of analytical methods – importance of analytical methods in qualitative and quantitative analysis – chemical and instrumental methods – advantages and limitations. Data analysis average deviation, standard deviation, confidence limits, comparison of results – t-test and f-test, rejection of results, calibration curves, and correlation coefficient. Significant figures. Sampling – procedures and statistics.

Unit 2:

Aqueous and Solid Phase Extraction [10 h]Liquid-liquid extraction theory and selection of solvents. Distillation – introduction, types of distillation, and applications. Solid phase extraction (SPE) types, formats and apparatus, method of operation, solvent selection, factors affecting SPE, automation, and on-line SPE. Supercritical fluid extraction instrumentation and applications.

Unit 3:

Chromatography[13 h]Thin layer chromatography – stationary phase, mobile phase, adsorbents, plate preparation, sample application, development, saturation of chamber, detection of spot, Rf values calculation, effect of adsorbent, solvent, solute, quantitative analysis and applications. Column chromatography packing a column and application. Separation of biomolecules electrophoresis, centrifugation of DNA and proteins. Gas chromatography (GC), high-performance liquid chromatography (HPLC), GC-MS and LCMS instrumentation, working principle and application.

Unit 4:

Thermal Analysis [10 h]Principle of thermogravimetry (TGA), differential thermal analysis (DTA), differential scanning calorimetry (DSC) – instrumentation and characteristics of TGA and DTA curves, factors affecting TGA and DTA curves. Applications – determination of purity of compounds by DSC, thermometric titrations, microthermal analyser working principle and applications.

Unit 5:

Surface Characterization Techniques[17 h]Principle, instrumentation, working and applications of the following microscopic techniques- SEM, AFM, STM, STEM, TEM, confocal microscopy and fluorescence microscopy. Elemental composition – energy dispersive spectroscopy, UPS, XPS, Auger electron spectroscopy, selected area diffraction. Particle size analyzers, DLS, zeta potential, BET and electrochemical surface area analysis.

CO1: Evaluate sensitivity, sources of interference, errors, and apply analytical data in terms of statistics.

CO2: Analyze chemical compounds by contemporary separation methods and appropriate selection of instruments

CO3: Explore the principle and working of the range of instrumental methods in analytical chemistry

CO4: Investigate solution behavior using electrochemical methods including potentiometry, conductometry, ion-selective, and cyclic voltammetric techniques.

CO5: Apply different microscopic methods and XRD technique in the analysis of materials

Recommended Reading

1.Karger, B.L., Snyder, L.R. and Horvath, C., 1973. Introduction to separation science.

2.Rousseau, R.W. ed., 1987. Handbook of separation process technology. John Wiley & Sons.

3.Skoog, D.A., West, D.M., Holler, F.J. and Crouch, S.R., 2013. Fundamentals of analytical chemistry. Cengage learning.

4.Skoog, D.A., Holler, F.J. and Nieman, T.A., 1998. Principles of instrumental analysis 5th edition. Saunders College Pub. Co.: Philadelphia.

5.Luo, Z., A Practical Guide to Transmission Electron Microscopy (Volume II).

6.Ul-Hamid, A., 2018. A beginners’ guide to scanning electron microscopy. Cham, Switzerland: Springer International Publishing.

7.Thomas, S., Thomas, R., Zachariah, A.K. and Mishra, R.K. eds., 2017. Microscopy methods in nanomaterials characterization (Vol. 1). Elsevier.