BP701T. INSTRUMENTAL METHODS OF ANALYSIS (Theory)

Unit-I

UV-Visible Spectroscopy:

• Principles and applications of UV-Visible spectroscopy.
• Beer-Lambert’s law and its deviations, factors affecting absorbance.
• Instrumentation:
• Light sources: Tungsten and deuterium lamps.
• Monochromators: Gratings and prisms.
• Sample cells: Quartz and glass cuvettes.
• Detectors: Photomultiplier tube, photodiode array.
• Applications in pharmaceutical analysis: Determination of drug content, dissolution studies, and stability testing.

Fluorimetry:

• Principles of fluorescence, factors affecting fluorescence (pH, solvent effects, temperature).
• Instrumentation:
• Light sources, filters, and detectors.
• Pharmaceutical applications: Assay of vitamins and antibiotics.

Unit-II

Infrared (IR) Spectroscopy:

• Principles, molecular vibrations (stretching and bending), and selection rules.
• Instrumentation:
• Sources: Nernst glower, globar.
• Detectors: Thermocouples, bolometers, pyroelectric detectors.
• Sampling techniques: KBr pellet, ATR (Attenuated Total Reflectance), and thin-film methods.
• Pharmaceutical applications: Identification of functional groups and polymorphic forms.

Atomic Absorption Spectroscopy (AAS):

• Principle, types (flame and graphite furnace), and interferences.
• Instrumentation:
• Hollow cathode lamps, atomizers.
• Applications: Detection of trace metals in pharmaceutical formulations.

Nepheloturbidimetry:

• Principle, comparison with colorimetry, and applications in pharmaceutical testing.

Unit-III

Nuclear Magnetic Resonance (NMR) Spectroscopy:

• Principles, chemical shift, spin-spin coupling, and shielding/deshielding effects.
• Instrumentation:
• Magnet, radiofrequency transmitter, and detector system.
• Applications in pharmaceuticals: Structural elucidation of organic compounds.

Mass Spectrometry:

• Principles, ionization techniques (EI, CI, MALDI), and mass analyzers (Quadrupole, TOF).
• Fragmentation patterns and interpretation.
• Applications in pharmaceutical analysis: Molecular weight determination and impurity profiling.

Unit-IV

Chromatographic Techniques:

• Introduction and classification of chromatographic methods.
• Gas Chromatography (GC):
• Principles, columns (capillary and packed), detectors (FID, TCD), and pharmaceutical applications.
• High-Performance Liquid Chromatography (HPLC):
• Principles, types of columns (reversed-phase, normal phase), detectors (UV, PDA, RI), and pharmaceutical applications.
• Thin Layer Chromatography (TLC):
• Principles, stationary and mobile phases, visualization techniques, and applications in qualitative analysis.
• Supercritical Fluid Chromatography (SFC):
• Principles, instrumentation, and applications.

Unit-V

Electrochemical Methods:

• Potentiometry:
• Principles, reference (calomel, Ag/AgCl) and indicator electrodes, applications in pH determination and titrations.
• Conductometry:
• Principles, types of conductometric titrations (acid-base, precipitation), applications.
• Polarography:
• Principles, dropping mercury electrode, Ilkovic equation, and pharmaceutical applications.

Advanced Techniques:

• X-ray Diffraction (XRD):
• Principles, Bragg’s law, and applications in crystallinity studies.
• Differential Scanning Calorimetry (DSC):
• Principles and applications in studying drug-excipient compatibility and polymorphism.
• Thermogravimetric Analysis (TGA):
• Principles and applications in moisture and thermal stability analysis.
• Capillary Electrophoresis (CE):
• Principles, instrumentation, and pharmaceutical applications.