CH3AT2: Advanced Analytical Techniques

Module code: CH3AT2

Module provider: Chemistry; School of Chemistry, Food and Pharmacy

Credits: 20

Level: Level 3 (Honours)

When you'll be taught: Semester 2

Module convenor: Professor Frantisek Hartl, email: f.hartl@reading.ac.uk

Pre-requisite module(s): This module is only available to students in the School/Department of Chemistry. (Open)

Co-requisite module(s):

Pre-requisite or Co-requisite module(s):

Module(s) excluded:

Placement information: NA

Academic year: 2024/5

Available to visiting students: Yes

Talis reading list: Yes

Last updated: 21 May 2024

Overview

Module aims and purpose

This module introduces a range of modern analytical chemistry techniques relevant to the molecular sciences. Mastering these techniques at a comprehensive level offered by the module content adds significantly to the tools expected, and requested, from a capable chemist with academic education. The scheduled lectures and workshops will be delivered by renowned field specialists in an attractive and interactive fashion.

Electrophoretic techniques (complementary with chromatographic techniques, e.g., HPLC) are widely used in medical diagnostic laboratories and in identification and authentication of animal foods as well as plant foods, for example brands of different foodstuffs that have protected geographical status.

Mass spectrometry detects molecules without specialized molecule-specific reagents. This makes it an unbeatable tool for rapid and tailored problem solving. The types of analyses performed are diverse and can include activities ranging from intact mass measurements of small molecules to proteins with a molecular weight over 100kD.

Multi-nuclear magnetic resonance and Electron paramagnetic resonance are important universal spectroscopic techniques used widely in molecular and materials chemistry for descriptive and analytical purposes, encompassing all the periodic table of elements, specifically a range of suited magnetically active naturally occurring isotopes.

Sophisticated voltammetry with ion-selective electrodes and anodic/cathodic stripping voltammetry belong to the most sensitive and selective analytical tools for everyday applications in many areas of human activities. Their role especially in targeted environmental and biomedical analysis is indispensable.

Scanning probe microscopy is a branch of microscopy encompassing several techniques that form images of surfaces using a physical probe that scans the specimen. It was founded with the invention of the scanning tunnelling microscope, an instrument for imaging surfaces at the atomic level. It is extremely important for the areas of nanotechnology and biosensors, offering the advantage of high lateral resolution.

Module learning outcomes

By the end of the module, it is expected that students will be able to:

1. Demonstrate thorough understanding of the advanced analytical techniques covered in the module and appreciate how such techniques can be used independently and in conjunction with other techniques to elucidate molecular structure and identity;
2. Analyse, interpret and present data from a range of analytical techniques in an appropriate format;
3. Express the role of analytical chemistry in science and the position of the taught techniques;
4. Demonstrate ability to solve complex problems and a systematic approach to tasks.

Module content

Electrophoretic Methods of Analysis (4 lectures + 1 workshop + 1 revision workshop)

Electrophoresis and related topics. Survey of the range of electrophoretic techniques available for the separation, purification and analysis of polymers, macromolecules, and biomolecules such as proteins and DNA with an introduction to biomacromolecules.

Advanced Mass Spectrometry (6 lectures + 1 workshop + 1 revision workshop)

Revision of basic principles and instrumentation, fragmentation in protein mass spectrometry and further spectral interpretation, quantitative analysis, hyphenation of other analytical and preparative techniques with mass spectrometry (incl. interfacing chromatographic instrumentation with a mass spectrometer), introduction to modern biological/biochemical mass spectrometry using current application areas, introduction into MS-based ‘omic’ workflows.

Advanced Electroanalytical Techniques (6 lectures + 1 workshop + 1 revision workshop)

Potentiometry with ion-selective electrodes (ISE). Standard addition and multiple standard addition methods in ISE analysis. Diverse types of membranes for selective ion detection and analysis, and multiple-membrane cells for gas sensing. Anodic, cathodic, and adsorptive stripping voltammetry for powerful analysis at ppb resolution.

Multinuclear NMR Spectroscopy (4 lectures + 1 workshop + 1 revision workshop)

NMR spectroscopy of species containing a wide range of NMR-active nuclei. Use of chemical shift and hyperfine coupling information to solve molecular structures and describe bonding properties of organic, inorganic and coordination compounds. Quadrupolar effect and its origin. Isotopic labelling and ways to distinguish between NMR-active isotopes of the same element.

Electron Paramagnetic Resonance Spectroscopy (4 lectures + 1 workshop + 1 revision workshop)

EPR spectroscopy in studying paramagnetic molecules. Instrumentation and comparison with NMR spectroscopy. Analysis of EPR spectra - g values, hyperfine splitting and intensity patterns. Difference in EPR signals of active isotopes of the same element. Isotropic and anisotropic EPR spectra. Spin trapping of short-lived radicals.

Scanning Probe Microscopy (3 lectures + 1 workshop)
Introduction to scanned probe microscopy, resolution and imaging mechanisms. Scanning tunnelling microscopy: image formation in UHV environments, imaging chemical reactions, atomic manipulation and discussion of limits to applications. Atomic force microscopy; cantilever dynamics, contact and non-contact imaging modes, force spectroscopy, chemical force and molecular pulling. Extensions to imaging in liquid environments consideration of cantilever dynamics and new methods and apparatus

Structure

Teaching and learning methods

Module content will be delivered through in-person blocks of 3-6 lectures on a given topic. Each of the six module topics will be accompanied by one formative workshop (compulsory) in which students will apply the theory, principles and concepts of the different analytical methods to solve relevant problems. In addition, a problem-based tutorial sheet, covering Scanning Probe Microscopy in the course, will be issued at the end of the first half of the semester. This tutorial will be summative. Students will submit written answers, which will be marked. The mark will contribute to the overall module mark. Feedback on the marked work will be provided through a tutorial (compulsory) during week 7 of the semester. There will be a total of 5 hours of revision workshops towards the end of the semester in preparation for the written examination that will exclude Scanning Probe Microscopy.  

Study hours

At least 34 hours of scheduled teaching and learning activities will be delivered in person, with the remaining hours for scheduled and self-scheduled teaching and learning activities delivered either in person or online. You will receive further details about how these hours will be delivered before the start of the module.

Please note the independent study hours above are notional numbers of hours; each student will approach studying in different ways. We would advise you to reflect on your learning and the number of hours you are allocating to these tasks.

Semester 1 The hours in this column may include hours during the Christmas holiday period.

Semester 2 The hours in this column may include hours during the Easter holiday period.

Summer The hours in this column will take place during the summer holidays and may be at the start and/or end of the module.

Assessment

Requirements for a pass

Students need to achieve an overall module mark of 40% to pass this module.

Summative assessment

Penalties for late submission of summative assessment

The Support Centres will apply the following penalties for work submitted late:

Assessments with numerical marks

• where the piece of work is submitted after the original deadline (or any formally agreed extension to the deadline): 10% of the total marks available for that piece of work will be deducted from the mark for each working day (or part thereof) following the deadline up to a total of three working days;
• the mark awarded due to the imposition of the penalty shall not fall below the threshold pass mark, namely 40% in the case of modules at Levels 4-6 (i.e. undergraduate modules for Parts 1-3) and 50% in the case of Level 7 modules offered as part of an Integrated Masters or taught postgraduate degree programme;
• where the piece of work is awarded a mark below the threshold pass mark prior to any penalty being imposed, and is submitted up to three working days after the original deadline (or any formally agreed extension to the deadline), no penalty shall be imposed;
• where the piece of work is submitted more than three working days after the original deadline (or any formally agreed extension to the deadline): a mark of zero will be recorded.

Assessments marked Pass/Fail

• where the piece of work is submitted within three working days of the deadline (or any formally agreed extension of the deadline): no penalty will be applied;
• where the piece of work is submitted more than three working days after the original deadline (or any formally agreed extension of the deadline): a grade of Fail will be awarded.

The University policy statement on penalties for late submission can be found at: https://www.reading.ac.uk/cqsd/-/media/project/functions/cqsd/documents/qap/penaltiesforlatesubmission.pdf

You are strongly advised to ensure that coursework is submitted by the relevant deadline. You should note that it is advisable to submit work in an unfinished state rather than to fail to submit any work.

Formative assessment

Formative assessment is any task or activity which creates feedback (or feedforward) for you about your learning, but which does not contribute towards your overall module mark.

Students will receive feedback on their work during the workshop sessions.

Reassessment

Additional costs