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Analytical and Experimental Chemistry

  • Module code: CH5004
  • Year: 2018/9
  • Level: 5
  • Credits: 30
  • Pre-requisites: Introduction to Spectroscopy & Experimental Techniques (CH4003)
  • Co-requisites: None

Summary

This is a core module for BSc Chemistry and MChem students. It takes forward the themes of analysis and practical procedures (with an emphasis on analytical and organic chemistry) that were introduced in previous modules. It incorporates both a more rigorous approach to laboratory work, coupled with developing the research skills required to devise experiments and then objectively assess results, followed by preparing high-quality reports and presentations.

The analytical methodologies and experimental techniques are those used routinely in academia, industry, and other laboratory research - spectroscopy; organic syntheses; molecular modelling; inorganic and physical chemistries; and the uses of applied separation technologies in common use.

The modes of obtaining and evaluating findings, by use of electronic databases (eg. Reaxys®) in addition to conventional printed literature sources. The ability to write coherent, evidence-based, yet succinct reports is a component.

Students will also gain opportunities to develop other important skills, from utilising statistics to planning and presentation techniques, all of which improve employability.

Over 50% of the formal contact teaching time is spent on practical work. Core teaching material is uploaded onto Canvas with lectures explaining key concepts.

Aims

  • To enhance the understanding of both qualitative and quantitative analyses, and the application of statistics to solve analytical problems;
  • To train students to record all pertinent experimental conditions and to develop an investigative approach to the solution of challenges in the laboratory and to encourage a critical approach to the assessment of experimental results.
  • To enable students to evaluate the supporting literature and electronic information sources, and utilise these in support of written and presented findings.

Learning outcomes

On successful completion of the module, students will be able to:

  • discuss the practices of separation science, chemical manipulation, and using these methods to purify a range of compounds.
  • show how the role of validation of procedures is vital to rigorous scientific methods.
  • define the various stages in problem solving, understanding the value of viable experimental results in statistical testing.
  • perform more advanced chemical experiments, in analytical, inorganic, organic, and physical chemistry fields, but with an emphasis on experimental organic chemistry.
  • compile an accurate and critical account of experiments undertaken, typically as an abstract, that integrates previous learning and peer-reviewed reference material.

Curriculum content

  • Overview of analytical methodology, process models, and sample preparation.
  • Chromatography: partition coefficients, retention time, capacity factor, selectivity factor, column efficiency and resolution.
  • Analytical and process validation - accuracy, precision (immediate & intermediate), linearity, specificity (peak resolution, impurities), ruggedness, limits of detection & quantitation, internal standards.
  • High performance liquid chromatography: pumps, columns, mobile phase selection, solvent gradient / isocratic, detectors.
  • Gas-liquid chromatography: sample injection, ovens (temperature ranges & rates of increase), detectors, stationary phases (columns), carrier gases.
  • Partition chromatography, normal and reverse phase. Ion-pair chromatography and chiral stationary phases.
  • Principles and practice of electrophoresis (including gel, electric focusing, immuno, and capillary).
  • Introduction to hyphenated techniques (GC-MS, HPLC-MS, tandem MS-MS).
  • Synthesis, preparation, and characterisation of the structure of a range of compounds using a broad range of techniques
  • Preparing and planning experimental procedures.
  • The relevance of statistics, quality control and quality assurance systems in analytical science.
  • Develop problem solving skills to relate laboratory work to the theoretical topics.
  • Application of computers to information retrieval and literature searches, using both the internet and non web-based databases.
  • Reporting experimental work in an academic/professional style, using both websites and more traditional printed literature sources such as books, journals, professional society magazines, conference summaries, and/or official reports.

Teaching and learning strategy

  • Lectures are mostly concerned with the analytical chemistry syllabus and will be accompanied by problem solving workshops. These will provide students with the experience to interpret analytical data, fully understand reactions, and comprehend the range of methodologies utilised.
  • Students will also be introduced to research methods and skills through lectures and workshops, primarily in the form of literature searching and preparing a critical analysis of a current research topic.
  • Workshop exercises aid students to continue to learn independently and progressively through problem solving after the workshop sessions.
  • The experimental programme is designed to enhance the laboratory skills of students through the use of more advanced techniques which are of relevance to other modules as well as during later employment or academic research.
  • Practical reports will test the students comprehension of key concepts pertaining to the experiment as well testing written communication skills. Independent learning skills will be developed through the module as students will inevitably encounter procedures pertaining to theory not met elsewhere in the course.

Breakdown of Teaching and Learning Hours

Definitive UNISTATS Category Indicative Description Hours
Scheduled learning and teaching lectures tutorials practical sessions 22 11 66
Guided independent study student independent study 201
Total (number of credits x 10) 300

Assessment strategy

Summative assessment is through: reports of experiments in laboratories, incorporating assessment of laboratory data, samples and other experimental findings; an in-course test based largely around practical and workshop components; a written exercise to find and review literature sources; and an end of module examination.

The examination focuses mostly on the lectured content of the module, but also incorporates learning from the practicals and workshops.

A range of formative assessments of relatively short duration provide regular feedback to students, so that they can develop an awareness of their progress, as well as gauge their strengths and weaknesses. On-going discussion with academic staff and workshops assist in the development of strategies for improvement and enhancement.

Mapping of Learning Outcomes to Assessment Strategy (Indicative)

Learning Outcome Assessment Strategy
Discuss the practices of separation science, chemical manipulation and use to purify a range of compounds; exam, coursework, practicals
Show how the role of validation of procedures and use of appropriate data are vital to rigorous scientific methods; exam, coursework, practicals
Define the varied stages in problem solving, appreciating the value of viable experimental results in statistics; exam, coursework, practicals
Perform more advanced analytical and organic chemical experiments; practicals
Compile an accurate and critical account of experiments undertaken, typically as an abstract, that integrates previous learning and peer-reviewed reference material. practicals

Elements of Assessment

Description of Assessment Definitive UNISTATS Categories Percentage
Written examination Written exam 40%
Literature searching with critique, on-line evaluation of data from practical (2 x 10% = 20%) Coursework 20%
In-class pro-forma completion, data and sample submissions (8 x 5% = 40%) Coursework 40%
Total (to equal 100%) 100%

Achieving a pass

It is NOT a requirement that any element of assessment is passed separately in order to achieve an overall pass for the module.

Bibliography recommended reading

Jonathan M. Goodman; Chemical Applications of Molecular Modelling; Royal Society of Chemistry.

Daniel C. Harris; Quantitative Chemical Analysis; W.H. Freeman & Co.

David Lindsay; Scientific Writing = Thinking in Words; CSIRO Publishing.

Christopher S. Lobban and Maria Schefter; Successful Lab Reports: a Manual for Science Students; Cambridge University Press.

Robert E. Maizell; How to Find Chemical Information: A Guide for Practicing Chemists, Educators, and Students; Wiley-Interscience.

Robert M. Silverstein, Francis X. Webster, and David Kiemle; Spectrometric Identification of Organic Compounds; John Wiley and Sons.

Dudley H. Williams & Ian Fleming; Spectroscopic Methods in Organic Chemistry; McGraw Hill.

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