To provide students with an understanding of the applications of various analytical techniques and their role in modern research. This module will demonstrate the fundamental theoretical principles of selected instrumental analytical techniques (NMR spectroscopy, mass-spectrometry, ICP-OE(MS) spectroscopy, separation and hyphenated techniques) in the context of their roles in industrial and academic research, to include chemical and pharmaceutical analysis.

(LO1) To be able to recognise the current trends in the application of the instrumental analytical methods

(LO2) Demonstrate awareness of the theoretical concepts of NMR spectroscopy, Mass-Spectrometry, Chromatography, hyphenated techniques GC/HPLC-MS, and ICP-based methods

(LO3) To be able to choose an appropriate technique in order to evaluate the structure, properties and potential applications of materials, or a multi-technique approach to find the solution of a selected experimental problem

(S1) Students will develop their chemistry-related cognitive ability and skills, relating to intellectual tasks, including problem solving as required by the Chemistry subject benchmark statement.

(S2) Students will improve their confidence in scientific communication and develop presentation skills of analytical data

Teaching method 1. 16 Lectures
Description: Class-based lectures
Attendance Recorded: Yes

Teaching method 2. Workshops on case/problem-based learning in small groups
Description: 3 problem(case)-based learning workshops with summary presentation in small groups, two are assessed totalling 20% of the final mark.
Attendance Recorded: Yes
Note: Students work in small groups overseen/guided by a demonstrator towards a solution of experimental problems. Upon finding solution, students will prepare and deliver a short presentation with the most important results.

Teaching method 3. Self-directed learning
Description: Self-directed learning using recorded lectures and additional recommended literature sources
Attendance Recorded: No

Introduction (lecture 1)
Analytical Chemistry: absolute and relative analytical methods, calibration (external calibration, standard additions, internal calibration), characteristics of an analytical procedure (accuracy, precision, specificity and selectivity, linearity range, detection and quantitation limits, robustness).

NMR spectroscopy (lectures 2-6)
1. Fundamentals of NMR spectroscopy; sensitivity, resolution, and scope; 1D and 2D NMR methods and techniques. Principal differences between solution and solid-state NMR (magic angle spinning, chemical shift anisotropy, quadrupolar and paramagnetic spins)
2. Applications of NMR spectroscopy
Applications of NMR spectroscopy in synthetic chemistry, catalysis, and materials study

Mass-spectrometry (lectures 7-9)
1. Fundamentals of mass-spectrometry. Ion sources: Electron Impaction Ionization (EI) and Chemical Ionization (CI), Electrospray ionization (ESI), Atmospheric Chemical Ionization (AP CI) and Atmospheric Pressure Ionization (API). Fast atom bombardment (FAB) and Matrix Assisted Laser Desorption Ionization (MALDI) mass-spectrometry. Mass spectrometry detectors: quadrupole, ion trap, time of flight (TOF).
2. Applications of mass-spectrometry in chemistry and biochemistry

Inductively-coupled plasma (ICP)-based methods (lectures 10-11)
1. Fundamentals of ICP; optical emission versus mass-spectrometry detection in ICP spectroscopy; sample preparation and matrixes, standards, speciation analysis, laser ablation.
2. Applications of ICP methods in chemistry and materials studies

Separation science (lectures 12-14)
1. Fundamentals of chromatography
2. Liquid Chromatography: modes of separation, instrumentation used, HPLC vs UHPLC. Ion Chromatography (IC), Size Exclusion Chromatography (SEC). Method development for LC: optimising separation conditions, selecting an appropriate column and detector for the given analysis. LC detectors: UV (photodiode array versus single wave UV), fluorescence, refractive index, electrochemical methods of detection. Conductivity detectors for Ion Chromatography.
3. Gas Chromatography: modes of separation, instrumentation used. Method development for GC: optimising separation conditions, selecting an appropriate column and detector for the given analysis. GC detectors: flame ionisation detector, thermal conductivity detector.
4. Applications of chromatography in chemical and pharmaceutical analysis

Hyphenated Techniques (lectures 15-16)
1. Introduction to hyphenation (GC/MS, HPLC/MS, MS/MS). GC Interfaces: Electron Impaction Ionization (EI) and Chemical Ionization (CI). HPLC Interfaces: Electrospray ionization (ESI), Atmospheric Chemical Ionization (APCI) and Atmospheric Pressure Ionization (API).
2. Applications of hyphenated techniques in chemical and pharmaceutical analysis.