Aim
The aim of the course is to provide the students with advanced knowledge and insight in analytical chemistry with emphasis on analytical separation techniques. Common techniques such as gas chromatography (GC) and liquid chromatography (HPLC) are included but also more specialized techniques such as capillary electrophoresis (CE) and flow field fractionation (FFF). Additionally, qualitative mass spectrometry including interpretation of mass spectra, and quantitative gas chromatography - mass spectrometry (GC-MS) for selective detection are considered.

The course also contributes to the development of the ability of the students to independently choose, optimise and perform chemical analyses. The course thus aims to provide the conditions needed for the student to be able to assimilate a coherent overview of the subject, which will underpin his or her ability to create new techniques/methods that will be applicable in new topics arising in the industry.

Another aim of the course is to provide skills in standard laboratory analytical methods and this will be trained by planning and performing analytical separations, mass spectrometric detections and by working up generated data to be compiled in the form of written technical reports, taking into consideration applicable environmental, safety and quality standards.

A literature seminar is aimed at encouraging students to practise their skills in review of relevant reference literature, in good laboratory practice as expressed in validated methods, and in oral and written presentations.

Knowledge and understanding
For a passing grade the student must

• be able to explain advanced theories of gas chromatography especially derivatisation methods prior to analysis, describe how gas chromatography coupled to mass spectrometry (GC-MS) is employed and describe how a detector is chosen taking into consideration the properties of the analytes

• be able to explain advanced theories of liquid chromatography (HPLC), describe different stationary and mobile phases and selective detectors utilised in HPLC, and explain how a detector is chosen taking into consideration the properties of the analytes and the sample matrix

• be able to demonstrate familiarity with the foundations of capillary electrophoresis and be able to explain how capillary electrophoresis is used for the analysis of low molecular analytes and macromolecules respectively

• be able to demonstrate familiarity with the foundations of qualitative mass spectrometric analysis (GC-MS)

• be able to describe different sample preparations techniques such as liquid-liquid extraction and solid-phase extraction

• be able to explain the meaning of concepts such as quality assurance, quality control, good laboratory practice (GLP), and method validation

Skills and abilities
For a passing grade the student must

• be able to optimise chromatographic separations by means of theoretical calculations

• be able to estimate the choice of retention mechanism (HPLC-method) based on the properties of the analytes and sample matrix, and be able to apply this method experimentally

• be able to evaluate the choice of injection technique in gas chromatography

• be able to interpret experimentally generated mass spectra for qualitative analysis

Judgement and approach
For a passing grade the student must

• be able to demonstrate abilities in searching for, studying and evaluating scientifically relevant information and in presenting scientific results and theories both orally and in writing

• be able to compile experimentally generated data into concise, clearly written technical reports

Contents
Experimental work: Quantitative gas chromatography and liquid chromatography and qualitative gas chromatography – mass spectrometry experiments are carried out. These experiments represent common analytical methods that are employed within the food and pharmaceutical industries as well as in environmental analytical chemistry. Examples of applications are determination of theophyllin in human plasma and ascorbic acid in urine with liquid chromatography, and chiral separations of terbutaline enantiomers with capillary electrophoresis.

Lectures: Gas- and liquid chromatography are treated in this course at a more advanced level and with a broader perspective than in the course of Analytical Chemistry for B3/K3. This applies to both the theoretical and experimental parts.

Within gas chromatography (GC), focus will be on capillary GC, temperature programming, the choice of stationary phase, injector and detector, especially selective detectors. Within liquid chromatography (HPLC) focus will be on common types of retention mechanisms. Different column packing materials (stationary phases) in combination with suitable eluents (solvents) and selective detectors are treated, all in relation to the character of the sample to be analyzed. Gradient elution in liquid chromatography is considered and for liquid chromatography of proteins a short orientation is provided. Sample preparation, method validation and good laboratory practice will be presented. Industrial pharmaceutical applications will be performed, with emphasis on product analytical and bioanalytical chemistry. Advanced theoretical treatment of chromatography will develop the ability of students to optimise the separation conditions. Consequently, important parameters such as migration, retention, separation selectivity, zone spreading, resolution, asymmetry, peak capacity and sample capacity are considered in detail. Another separation technique that is introduced in this course is capillary electrophoresis, including fundamental theories and applications. Fundamental mass spectrometry is broadened with qualitative GC-MS that is treated in detail and quantitative GC-MS is introduced. The quality of analytical results is discussed including both sample preparation and final analysis.

Literature
Harris, D C: Quantitative Chemical Analysis. Seventh ed. Freeman 2007. ISBN: 0-7167-7041-5.
Compendia. Div. of Technical Analytical Chemistry.
Laboratory text. Div. of Technical Analytical Chemistry.