COURSE OBJECTIVES
To introduce students to the basic principles of chemical analysis of materials, from sampling, selection of an appropriate method to interpretation of the results obtained.
PREREQUISITE COURSES
Attended lectures and completed exercises from the course General Chemistry.
COURSE LEARNING OUTCOMES
1. Understand the systematic approach to chemical analysis
2. Create a sampling plan with the aim of obtaining a representative sample
3. Apply chemical laws for the purpose of identification, separation and quantification of analytes in real samples
4. Propose an appropriate method of separation and isolation of analytes from a real sample
5. Critically compare methods of quantitative chemical analysis
6. Identify the causes of errors in chemical analysis
7. Analyze a real sample using an appropriate method of chemical analysis
8. Analyze and interpret the results of chemical analysis using statistical tests.
LEARNING OUTCOMES OF THE STUDY PROGRAM TO WHICH THE LEARNING OUTCOMES OF THIS COURSE CONTRIBUTE
1. explain the scientific foundations important for chemistry and materials engineering, especially in the fields of chemistry, physics, mathematics and chemical engineering
2. define simple problems in the field of chemistry and materials engineering in order to solve them
3. analyze materials using chemical and physical techniques and laboratory equipment and devices
4. theoretically interpret the results of experimental work
5. organize effective work in the laboratory, independently or as part of a multidisciplinary team
6. present the results of their work in written and oral form
COURSE CONTENT BY UNITS OR WEEKS
LECTURES AND SEMINARS
1. The role of analytical chemistry in materials analysis. Fundamentals of the analytical process. Laboratory safety.
Seminar: Safety data sheet and hazard pictograms
2. Sources of errors in chemical analysis. Systematic, random and gross errors. Statistical processing of results. Accuracy. Trueness. Precision.
Seminar: Statistical tests (t, F, Dixon's and Grubbs's)
3. Sample and sampling. Sample representativeness. Sampling planning. Subsampling. Sample preparation for chemical analysis. Water in a solid sample. Decomposition of a solid sample.
Seminar: Examples and tasks - Sampling planning (sampling location, number of samples, sample quantity)
4. Gravimetric methods: Mass measurement. Types of precipitates. Precipitate formation. Factors affecting precipitate formation. Purity of precipitate.
Seminar: Computational tasks - Gravimetric analysis
5. Introduction to titrimetric methods: Volume measurement. Standard solutions. Indicators. Titration curve.
Seminar: Computational tasks - Titrimetric analysis
6. Titrimetric methods: Neutralization titrations. Neutralization titration curves. Selection of indicators.
Seminar: Computational tasks - Neutralization titrations
7. First test.
8. Titrimetric methods: Precipitation titrations. Precipitation titration curve. Selection of indicators. Complexometric titrations. Complexometric titration curve. Selection of indicators.
Seminar: Computational tasks - Precipitation and complexometric titrations
9. Titrimetric methods: Redox titrations. Redox titration curve. Selection of indicators.
Seminar: Computational tasks - Redox titrations
10. Electroanalytical methods: Electrogravimetry. Indicator and reference electrodes. Direct potentiometric measurements. Potentiometric titrations.
Seminar: Computational tasks - Electrogravimetry, direct potentiometric measurements
11. Introduction to spectrometric methods. Lambert-Beer's law. Calibration. Calibration curve.
Seminar: Computational tasks - Application of Lambert-Beer's law and construction of a calibration curve
12. Separation and isolation of analytes. Separation efficiency. Errors. Classification of separation techniques. Masking. Selective precipitation.
Seminar: Tasks - Masking and selective precipitation
13. Separations based on partitioning. Partition coefficient and partition ratio. Liquid-liquid extraction. Extraction of weak acids. Extraction of metal ions.
Seminar: Computational tasks - Extraction
14. Chromatography. Chromatographic system. Classification of chromatographic techniques. Surface chromatography and column chromatography. Chromatogram Chromatographic resolution. Capacity factor. Selectivity and efficiency.
Seminar: Chromatogram analysis and computational tasks (number and height of theoretical sections, resolution factor, selectivity factor)
15. Second test
LABORATORY EXERCISES
1. Measurement of volumetric dishes
2. Acid-base titrations: Standardization of HCl and NaOH
3. Acid-base titrations: Determination of H2C2O4
4. Potentiometric titrations: Determination of CH3COOH
5. Precipitation titrations: Determination of chloride according to Mohr
6. Redox titrations: Standardization of KMnO4, Determination of copper
7. Electrogravimetry: Determination of copper
8. Turbidimetry: Determination of sulfate in water
9. Selective deposition.
10. Chloride determination with an ion-selective electrode
11. Thin-layer chromatography: Separation and qualitative analysis of metal ions in an alloy sample
Analysis of a real sample? Chemical analysis of cement: sample dissolution, preparation of stock solution, determination of SiO2+insoluble content (gravimetry), determination of Fe2O3 and Al2O3 content (spectrophotometry), determination of CaO and MgO content (complexometric titration)
MODES OF INSTRUCTION
classical
lectures, seminars and workshops, exercises
STUDENT OBLIGATIONS
Attendance at lectures, successfully completed laboratory exercises, submitted laboratory exercise papers and passed the final laboratory exercise exam.
MONITORING OF STUDENTS? WORK
Class attendance, Experimental work, Written exam, Oral exam, Continuous assessment, Report
GRADING AND ASSESSMENT DURING CLASS AND ON THE FINAL EXAM
Student work during classes is evaluated through the following activities:
- two (2) preliminary exams
- laboratory exercises, through work in the laboratory (preparation, accuracy of results, reports) and a final preliminary exam from laboratory exercises
- short knowledge tests at the end of individual lectures that also serve to check attendance at lectures
Students who achieve the required minimum number of points (threshold) or more through these activities are exempt from taking the written part of the exam. They take the oral part of the exam during the 1st or 2nd summer exam period.
Students who do not pass the preliminary exams take the written and oral parts of the exam.
Students who have re-enrolled in the course can take the exam without attending lectures again. If they wish to take the preliminary exam, they are required to attend classes.
Evaluation of student work during classes and at the final exam:
Laboratory exercises: continuous monitoring/exame: threshold: 10, max: 20
Short tests: continuous monitoring/exame: threshold: 5, max: 10
1st midterm: continuous monitoring: threshold: 10, max: 20
2nd midterm: continuous monitoring: threshold: 10, max: 20
Oral exam: continuous monitoring/exame: max: 30
Written exam: exame: threshold: 20, max: 40
The total grade is formed based on the points achieved:
50 - 61 - sufficient (2)
62 - 74 - good (3)
75 - 87 - very good (4)
88 - 100 - excellent (5)
MANDATORY LITERATURE
M. Kaštelan-Macan, Analitička kemija, I dio (Gravimetrija), Sveučilište Zagreb, 1991.
Z. Šoljić, M. Kaštelan-Macan, Analitička kemija: Volumetrija, Fakultet kemijskog inženjerstva i tehnologije, Zagreb, 2002.
Z. Šoljić, Laboratorijske osnove kvantitativne kemijske analize, Fakultet kemijskog inženjerstva i tehnologije, 2006.
S. Babić, M. Biošić, A. Badrov, Interna skripta za laboratorijske vježbe, 2021.
QUALITY ASSURANCE METHODS THAT ENSURE THE ACQUISITION OF OUTPUT KNOWLEDGE, SKILLS AND COMPETENCES
Student survey, pass rate analysis
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