Advanced Analytical Chemistry - Sampling and Sample Preparation

Course 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, 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, a field exercise and expert guest-lectures of selected topics.

Education

MSc Programme in Chemistry
MSc Programme in Environmental Science

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 theory, 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 including selection of tools, techniques and how to optimize sample preparation procedure for organic analytes.

Competences:

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

Lectures, student presentations of curriculum, expert lectures and field trip, theoretical and practical group work, computer simulations using excel.

Notes and selected peer-reviewed papers will be used extensively. 

Textbook: "Handbook of Sample Preparation" ed. Janusz Pawliszyn & Heather L. Lord (Available on Rex) 

The course LKEF10076 Analytical Chemistry or equivalent is a requirement. Knowledge of basic statistics is also recommended.

For further information feel free to contact Karina Knudsmark Sjøholm (jessing@plen.ku.dk)

ECTS
7,5 ECTS
Type of assessment
Written assignment, 7 days
Oral examination, 30 min.
The written exam is a written take-home assignment for the sampling part (acounts for one third) and is in the 3-4 week of the course.
The oral exam (acounts for 2 third) is after the sample preparation part of the course. 20 min. preparation time before the exam.
Both part of the exam must be passed.
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
Criteria for exam assessment

According to the learning outcome.

Single subject courses (day)

  • Category
  • Hours
  • Preparation
  • 106
  • Lectures
  • 26
  • Theory exercises
  • 20
  • Practical exercises
  • 12
  • Colloquia
  • 12
  • Excursions
  • 10
  • Exam
  • 20
  • English
  • 206