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Advanced chromatographic methods

Some basic information about the module

Cycle of education: 2022/2023

The name of the faculty organization unit: The faculty Chemistry

The name of the field of study: Chemical Technology

The area of study: technical sciences

The profile of studing:

The level of study: first degree study

Type of study: full time

discipline specialities : Chemical analysis in industry and environment, Chemical and bioprocess engineering, Organic and polymer technology

The degree after graduating from university: Bachelor of Science (BSc)

The name of the module department : Department of Physical Chemistry

The code of the module: 216

The module status: mandatory for the speciality Chemical analysis in industry and environment

The position in the studies teaching programme: sem: 7 / W15 L30 / 4 ECTS / Z

The language of the lecture: Polish

The name of the coordinator: Paweł Błoniarz, PhD, Eng.

office hours of the coordinator: poniedziałki 12.00-14.00 czwartki 12.00-14.00

semester 7: Karol Bester, PhD, Eng. , office hours Monday 12.00-14.00 Thursday12.00-14.00

The aim of studying and bibliography

The main aim of study: Provide knowledge on the modern chromatographic methods, hyphenated techniques, including sample preparation methods used in environmental, pharmaceutical laboratories and food analysis.

The general information about the module: The module is implemented in 7 semester and includes 15 hours of lectures and 30 hours of lab. The module ends with a pass.

Teaching materials: instrukcje do ćwiczeń laboratoryjnych

Bibliography required to complete the module
Bibliography used during lectures
1 Z. Witkiewicz Podstawy chromatografii, wyd.2-gie WNT, Warszawa. 1995
2 J. Namieśnik, J. Łukasiak, Z. Jamrógiewicz Pobieranie próbek środowiskowych do analizy PWN, Warszawa. 1995
3 K. Robards, P. Jackson, P. Haddad Principles and Practice of Modern Chromatographic Methods, 1st Edition Academic Press, London. 1994
4 W. Rödel, G. Wölm Chromatografia gazowa WN PWN, Warszawa . 1992
5 R. Rosset, H. Kołodziejczyk Współczesna chromatografia cieczowa PWN, Warszawa. 2000
Bibliography to self-study
1 Z. Witkiewicz Nowe kierunki w chromatografii WNT, Warszawa . 1988
2 L. R. Snyder, J. J Kirkland, J. L. Gleic Practical HPLC method development, sec. ed. J. Wiley, New York. 1997
3 R.J. Hamilton, P.A. Sewell Wysokosprawna chromatografia cieczowa PWN, Warszawa . 1982

Basic requirements in category knowledge/skills/social competences

Formal requirements: required course credits: instrumental analysis, analytical chemistry, physical chemistry, mathematics, pyisics

Basic requirements in category knowledge: Required basic knowledge of instrumental methods of analysis, physics and mathematics

Basic requirements in category skills: required basic laboratory skills and practical experience in the use of basic equipment and instrumentation

Basic requirements in category social competences: organizational skills, manipulative and observational skills, being able to work in teams

Module outcomes

MEK The student who completed the module Types of classes / teaching methods leading to achieving a given outcome of teaching Methods of verifying every mentioned outcome of teaching Relationships with KEK Relationships with PRK
01 Has knowledge of the chromatographic techniques applied in environmental, food and material analysis. Mastered the separation mechanisms, column chemistry and can apply optimization procedures. Learned the modern techniques for the preparation of samples for chromatographic analysis. lecture, laboratory exercise written test and report for every laboratory exercise, observation of performance, pass a final written test K_W04+++
P6S_WG
02 Acquired knowledge of the modern chromatographic techniques such as two-dimensional chromatography, multicapilary gas chromatography, ultra-fast performance liquid chromatography and chromatographic hyphenated methods. lecture, laboratory exercise written test and report for every laboratory exercise, observation of performance, pass a final written test K_W13+++
P6S_WG
03 He can design and use approprate chromatographic analysis method for the specific analyte or group of analytes and a sample type. laboratory exercise written test and report for every laboratory exercise, observation of performance, K_U11+
P6S_UO
P6S_UW
04 He uses quantitative methods of analysis, including callibration techniques. Acquired the practical knowledge and skills to interpret and evaluate the quality and reliability of the results of analysis. laboratory exercises pass a written test, observation of performance K_U21+
K_K01+
P6S_KK
P6S_KO
P6S_KR
P6S_UW
05 He has the ability to work independly and in the team during the planning of the analytical procedure and analytical problem solving. laboratory exercises observation of performance K_K03+
P6S_KR

Attention: Depending on the epidemic situation, verification of the achieved learning outcomes specified in the study program, in particular credits and examinations at the end of specific classes, can be implemented remotely (real-time meetings).

The syllabus of the module

Sem. TK The content realized in MEK
7 TK01 Sample preparation techniques for chromatographic analysis. Isolation of analytes from the solid, liquid and gaseous samples. Accelerated solvent extraction (ASE). Microwave assisted extraction (MAE). Solid phase microextraction (SPE, SPME). Methods for gas extraction from the liquid phase. The HS (head-space) techniques, dynamic headspace analysis - P & T (purge and trap). W01-W7 MEK01 MEK05
7 TK02 Modern chromatographic techniques: multi-dimensional gas chromatography (GCxGC), multikapilary gas chromatography (MCC-GC), fast and ultra-fast performance liquid chromatography (micro-HPLC, UHPLC). Chromatography columns, separation mechanisms and column packings in various chromatographic techniques. The column quality parameters and their evaluation. Hyphenated chromatographic methods, types, advantages, selection criteria, review of applications. The combination of gas and liquid chromatography with spectroscopic methods (GC-MS, GC-IR, HPLC-MS, HPLC-IR, HPLC-NMR). Their application in the analysis of samples with compex matrix. W08-W12 MEK02 MEK03
7 TK03 New calibration and quantification methods - application for minimizing the effect of the sample matrix. Isotopic dilution method, and interpolation and extrapolation methodologies. W13-W15 MEK03 MEK04
7 TK04 Determination of analytes in complex matrix samples by GC - the evaluation of the matrix interference impact on the accuracy and precision. Determination of flavonoids in natural products by HPLC-UV / VIS. Isolation of components of food samples by solid-phase extraction SPE - evaluation of extraction yield by HPLC. A fragrance profile analysis by GC-MS in combination with a Head Space (HC-GC-MS) - the quantification of a recovery analytes. Analysis of volatile organic compounds (BETEX) in environmental samples - optimization of the chromatographic separation parameters, evaluation of resolution, efficiency, and selectivity under various conditions of temperature and velocity of the mobile phase. Determination of the average molecular weight by gel permeation chromatography GPC. L01-L30 MEK03 MEK05

The student's effort

The type of classes The work before classes The participation in classes The work after classes
Lecture (sem. 7) contact hours: 15.00 hours/sem.
Studying the recommended bibliography: 5.00 hours/sem.
Laboratory (sem. 7) The preparation for a Laboratory: 5.00 hours/sem.
The preparation for a test: 15.00 hours/sem.
contact hours: 30.00 hours/sem.
Finishing/Making the report: 10.00 hours/sem.
Advice (sem. 7) The preparation for Advice: 1.00 hours/sem.
The participation in Advice: 5.00 hours/sem.
Credit (sem. 7) The preparation for a Credit: 15.00 hours/sem.
The written credit: 2.00 hours/sem.

The way of giving the component module grades and the final grade

The type of classes The way of giving the final grade
Lecture Written test - 50% of the maximum number of points (OW) required to pass; the grade is calculated using the following coefficients: 1.0 - for a positive grade obtained in the first term; 0.9 - for the evaluation on the second term and 0.8 - for the third term
Laboratory The condition necessary for completing the laboratory is to obtain a positive assessment for every exercise included in the schedule. The crediting of a given exercise requires a passing grade for a written test checking preparedness for the topic of the exercise (with a weighting of 0.75 to a weighted average) and a passing grade for a report on results of the exercise (with a weighting of 0.25 to a weighted average). The final assessment of the laboratory is counted as the arithmetic mean of all partial grades obtained for every exercise included in the schedule. The final grade for the laboratory is rounded according to WKJK.
The final grade The final mark in the module (K) is calculated according to the formula: K= w 0,5 OW + w 0,5 OL; where: OW, OL denote positive marks for lecture test and laboratory practice, respectively, w - coefficient for delay, w =1.0 when a passing mark is obtained in due time, w=0.9 for a first resit, w=0.8 for a second resit. The final mark is rounded according to WKZJK.

Sample problems

Required during the exam/when receiving the credit
(-)

Realized during classes/laboratories/projects
(-)

Others
(-)

Can a student use any teaching aids during the exam/when receiving the credit : no

The contents of the module are associated with the research profile: yes

1 P. Błoniarz; P. Chmielarz; K. Kisiel; M. Klamut; K. Matyjaszewski; M. Niemiec; A. Pellis; C. Warne; I. Zaborniak Controlled Polymer Synthesis Toward Green Chemistry: Deep Insights into Atom Transfer Radical Polymerization in Biobased Substitutes for Polar Aprotic Solvents 2024
2 P. Błoniarz; P. Chmielarz; M. Flejszar; A. Hochół; K. Spilarewicz; K. Ślusarczyk Replacing organics with water: Macromolecular engineering of non-water miscible poly(meth)acrylates via interfacial and ion-pair catalysis SARA ATRP in miniemulsion 2023
3 P. Błoniarz; P. Chmielarz; K. Surmacz Coffee Beverage: A New Strategy for the Synthesis of Polymethacrylates via ATRP 2022
4 P. Błoniarz; D. Maksym; J. Muzart; T. Pacześniak; A. Pokutsa; A. Zaborovskyi Cyclohexane oxidation: relationships of the process efficiency with electrical conductance, electronic and cyclic voltammetry spectra of the reaction mixture 2021
5 P. Błoniarz; K. Ohkubo; A. Pokutsa; A. Zaborovskyi UV-induced oxygenation of toluene enhanced by Co (acac)2/9-mesityl-10-methylacridinium ion/N-hydroxyphthalimide tandem 2021
6 P. Błoniarz; J. Muzart; T. Pacześniak; A. Pokutsa; S. Tkach; A. Zaborovskyi Sustainable oxidation of cyclohexane and toluene in the presence of affordable catalysts: Impact of the tandem of promoter/oxidant on process efficiency 2020
7 P. Błoniarz; O. Fliunt; Y. Kubaj; T. Pacześniak; A. Pokutsa; A. Zaborovskyi Sustainable oxidation of cyclohexane catayzed by a VO(acac)2 - oxalic acid tandem: the electrochemical motive of the process efficiency 2020
8 P. Błoniarz; P. Chmielarz; T. Pacześniak; K. Rydel-Ciszek; A. Sobkowiak; K. Surmacz; I. Zaborniak Iron-Based Catalytically Active Complexes in Preparation of Functional Materials 2020
9 P. Błoniarz; Y. Kubaj; D. Maksym; J. Muzart; T. Pacześniak; A. Pokutsa; A. Zaborovskyi Versatile and Affordable Approach for Tracking the Oxidative Stress Caused by the Free Radicals: the Chemical Perception 2020