NPLK13003U Advanced Analytical Chemistry - Sampling and Sample Preparation
MSc Programme in Chemistry
MSc Programme in Environmental Science
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.
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.
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.
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.
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.
Notes and selected peer-reviewed papers will be used extensively.
Textbook: "Handbook of Sample Preparation" ed. Janusz Pawliszyn & Heather L. Lord (Available on Rex)
- 7,5 ECTS
- Type of assessment
- Written assignment, 5 daysOral 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.
- 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.
- 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
The same as the ordinary exam.
The two parts of the exam must both be passed individually. If one part is passed at the ordinary exam and the other part is not, reexam will be offered in the part that is not passed at the ordinary exam.
There cannot be any dispensation from the laboratory exercises, and students who do not fulfil the requirement has to follow the course the following study year.
Criteria for exam assesment
According to the learning outcome.
- Theory exercises
- Practical exercises