NPLK13003U Advanced Analytical Chemistry - Sampling and Sample Preparation

Volume 2013/2014
Content
Sampling and sample preparatin is a cornerstone in performing sound experiments, and thus essential to any kind of analytical chemistry project: the results obtained will never be better than the samples injected.

The course starts with a throughout treatment of Pierre Gy’s Theory of Sampling (TOS), which tells how to obtain a representative sample without systematic errors and with an acceptable uncertainty.  Based on TOS the practice and tools for taking the samples and reduce the sample mass in a representative way is treated.  All common matrices, soil, water and air, are addressed.

The last part of the course covers the sample preparation techniques for extraction, purification and pre-concentration of samples for injection into modern analytical instruments such as GC and, HPLC. The preparation part includes active and passive sampling for gases (adsorbents, denuders, traps, filtering etc.), liquid, solid and headspace sampling for liquids (LLE, SPE, SPME SBSE SLE etc.) and liquid and headspace sampling from solids (shake, MW, US, PLE, SFE, etc.). The sample preparation part focus on organic analytes only.

The theory is supplemented with computer simulations, laboratory experiments, excursions and expert guest-lectures of selected topics.
Learning Outcome

This course enables the student to plan and perform sampling and sample preparation, including sampling strategy, determination of number of samples and sample size, sample selection, sampling techniques and tools, and methods for sample preparation for organic analytes, extraction, filtering, purification and pre-concentration including advanced methods like SPME, SBSE, PLE, SLE for common instrumental analytical methods.

Knowledge:

Describe the theory and principles for representative sampling according to Gy’s Theory of Sampling. Describe the theory for active and passive sampling. Describe the tools, instruments, and techniques for sample preparation of organic analytes.

Skills:

Plan sampling experiments and analyse the results in terms of sampling variance using Anova and variographic analysis. Predict sampling variance using Gy’s formula for simple matrices. Plan sample preparation for organic analytes, including selection of tools and techniques.

Competences:

Plan and perform sampling pilot experiments and real sampling for chemical analysis. Develop and apply sample preparation methods for instrumental analysis of organic compounds. Evaluate and discuss the scientific literature within sampling and sample preparation.

Literature
Notes and selected articles will be used extensively. Textbook to be announced on Absalon.
The course LKEF10076 Analytical Chemistry or equivalent is a requirement. Knowledge of basic statistics is also recommended.
Lectures, student presentations of curriculum, expert lectures and excursions, theoretical and practical group work, computer simulations.
For further information feel free to contact Bo Svensmark, svensmark@life.ku.dk
  • Category
  • Hours
  • Colloquia
  • 12
  • Exam
  • 20
  • Excursions
  • 10
  • Lectures
  • 26
  • Practical exercises
  • 8
  • Preparation
  • 106
  • Theory exercises
  • 24
  • Total
  • 206
Credit
7,5 ECTS
Type of assessment
Written assignment, 7 days
Oral examination, 30 min. under invigilation
The written exam is a written take-home assignment.
Exam registration requirements
Student presentation of curriculum, participation in laboratory exercises and handing in reports are mandatory. Active participation in a minimum of 75% of these activities is required.
Aid
Only certain aids allowed
All written aids and any calculator which does not allow communication
Marking scale
7-point grading scale
Censorship form
No external censorship
One internal examiner
Re-exam
If 10 or fewer register for the reexamination the examination form will be oral.
Criteria for exam assesment
According to the learning outcome.