Advanced Analytical Chemistry - Sampling and Sample Preparation

Course content

Sampling and sample preparation 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 thorough 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.  The practice and tools for taking the samples and reduce the sample mass in a representative way is treated based on ToS.  All common matrices, soil, water and air, are addressed.

The second 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. This part of the course includes: active and passive sampling for gases (adsorbents, traps, filtering etc.), sample preparation for liquid matrices (Liquid/Liquid Extraction – LLE, Solid Phase Extraction – SPE, Solid Phase Micro-Extraction – SPME, Stir-Bar Solid Extraction – SBSE, Supported Liquid Extraction – SLE etc.), for solid matrices (shake, Microwave Assisted Extraction – MAE, Ultrasonication, Pressurised Liquid Extraction – PLE, Supercritical Fluid Extraction – SFE, etc.), and various headspace methods. 

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. Describe, 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 NPLB14027U Analytical Chemistry or equivalent is a requirement. Knowledge of basic statistics is also recommended.

For further information feel free to contact Giorgio Tomasi (gito@plen.ku.dk)

Written
Oral
Individual
ECTS
7,5 ECTS
Type of assessment
Written assignment, 5 days
Oral examination, 30 min.
The written exam accounts for one third, is a take-home assignment on the sampling part. It takes place between the third and the fourth week of the course.
The oral exam, which accounts for two thirds, takes place after the sample preparation part of the course. 20 min. preparation time before the exam.
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