Instrumental Characterisation Techniques

Learning Outcomes

Learning Outcomes

Having successfully completed this module you will be able to:

• Perform basic calculations relating to crystal planes, lattice parameters and sample characteristics
• Understand the advantages of synchrotron and neutron diffraction and the additional information they can provide
• Comprehend the optimisation of chromatographic methods
• Complete a Rietveld refinement and extract crystallographic and sample information
• Interpret data using line positions and profiles
• Critically evaluate the quality and reliability of your acquired instrumental data
• Apply the concepts of unit cells and lattices to describe observed diffraction patterns in reciprocal space
• Recognise the steps involved in acquiring NMR spectroscopic data: from sample preparation to setting appropriate acquisition parameters
• Understand and apply the various types of powder diffraction experiment and appreciate the importance of sample preparation
• Have raised awareness of mass spectrometry applications areas
• Evaluate the differences and synergies of powder and single crystal diffraction
• Understand the basics of X-ray diffraction theory in terms of X-rays, diffraction and Bragg’s Law
• Understand solid-state matter in terms of crystallinity and bonding
• Be aware of and use various crystallographic databases
• Be aware of advanced techniques such as X-ray reflectivity, texture analyse and high-resolution measurements
• Setup data collection strategies and collect data on both a single crystal and powder samples
• Interpret and assign NMR spectroscopic data as a tool for structural elucidation
• Determine appropriate ionisation technique and instrument type for analysis
• Have an awareness of the principles of advanced mass spectrometry techniques
• Understand point and translational symmetry elements and derive symmetry from measured data
• Process data, solve/refine and interpret a single crystal structure
• Have raised awareness of chromatographic applications areas
• Recognise further applications for NMR spectroscopy in probing supramolecular interactions, understanding the thermodynamics of fluxional processes in solution and following reaction kinetics
• Interpret and assign mass spectrometric data as a tool for structural elucidation
• Determine appropriate chromatographic technique and approach for analysis

A. NMR Spectroscopy PART 1 Fundamentals of NMR spectroscopy • Nuclear spin (I = ½, I > ½ nuclei), pulsed RF, relaxation issues: implications for acquisition of data • Chemical shift, integration, spin coupling – interpretation of 1D NMR data • Multinuclear NMR (p-block, transition metals) • Advanced NMR experiments • 2D NMR (homonuclear and heteronuclear) • NOE spectroscopy • VT NMR and fluxionality (both organic and broadband samples) PART 2 Applications of liquid state NMR spectroscopy • Structural elucidation • Stereochemistry: determination and assignment • Binding studies • Kinetics • Practical techniques • Sample preparation • Sample submission and data acquisition • Processing data • Reporting data in literature/reports B. Mass Spectrometry PART 1 Tenets of Mass Spectrometry • Ionisation techniques • Sample Introduction • Analyser types • Low and high mass resolution PART 2 Advanced Mass Spectrometry • MS/MS • Hyphenated techniques • Large molecule MS PART 3. Applications of Mass Spectrometry • Structural elucidation • Qualitative MS • Quantitative MS • Speciation • Isotope ratio mass spectrometry (IRMS) • ‘Omics’ PART 4. Practical techniques • Sample preparation and data acquisition • Strengths and limitations of automation • Data Interpretation • Reporting data in literature/reports C. X-Ray Diffraction PART 1 Basics of Diffraction & Materials Types of bonding and materials, X-rays and Bragg’s Law, unit cells and lattices, reciprocal space, symmetry, space-groups and systematic absences. PART 2 Single crystal diffraction Collecting and processing data, structure solution and refinement, structure validation. PART 3 Powder diffraction Diffraction geometry, indexing, line profile analysis and residual stress, Rietveld, reflectivity and high-resolution diffraction, texture and non-crystalline diffraction. PART 4 Combined Topics Synchrotron diffraction, neutron diffraction, databases. D. Chromatography PART 1. Tenets of chromatography • Retention • Resolution • Selectivity • Efficiency PART 2. Types of chromatography • High performance liquid chromatography (RP & NP) • Gas chromatography • Thin Layer chromatography PART 3. Detectors and advanced applications • Detectors • Ion exchange chromatography • SFC • Quantitative chromatography PART 4. Practical techniques • Sample preparation • Column chemistries • Method development • Advantages and disadvantages

Teaching Methods • Lectures, demonstrations, data analysis workshops, practical sessions, self-study problems Learning Methods • Independent study, student motivated peer-group study, student driven tutor support.

Summative

This is how we’ll formally assess what you have learned in this module.

Referral

This is how we’ll assess you if you don’t meet the criteria to pass this module.