Quantitave chemical analysis

Course code: 2.5

Semester: 2^nd

Category: Mandatory (special background course)

Course hours: 2Th +2 L

ECTS units: 5

 

LEARNING OUTCOMES

After completion of the course the students will be able to:

• Apply the methods of analytical Chemistry,
• Conduct safely the basic analytical determinations,
• Solve methodically Classical Chemical Analysis problems,
• Organize an analytical Chemistry laboratory.

 

General Skills

• Search, analyze and synthesize data and information using the necessary technologies
• Autonomous work
• Teamwork
• Respect for the natural environment.

 

Course content

A.Teoretical part

1. Introduction: Purpose and significance of Analytical Chemistry. The Analytical Problem. Chemical Analysis Methods. Interferences. Steps of an analytical method. Bibliography.
2. Reagents, labware and materials: Water and chemical reagents. Labware and materials. Labware calibration and cleaning.
3. Sampling: Sampling methods. Factord affecting the sampling methods. Types of samples. Sample handling.
4. Sample treatment – I: Necessity for treatment. Grinding, Sieving. Heat treatment. Precipitation. Filtration. Centrifugation.
5. Sample treatment – II: Extraction. Wet digestion. Fusion. Cremation. Combustion. Use of microwaves and ultrasounds. Material loss risks in a sample analysis.
6. Errors in measurements and expression of results. Measurement uncertainity. Normal error curve. Incertainity of measurements. Confidence interval. Rejection of measurement values. Scientific expression of the results.
7. Statistical techniques in Chemical Analysis. Random errors. Comparison of two means, limit of Detection, limit of Quantitation, systematic measurements error assesement and control, standard deviations comparison, required number of samples calculation, the least-square method, the X² test and the Friedman test.
8. Gravimetric Analysis: Characteristics of the technique. Types of precipitates. Precipitate formation. Precipitate properties changes. Precipitate contamination. Labware, Instruments and materials. Homogeneous preciritation. Precipitation reagents. Precipitation analysis applications. Evolution methods. Electrigravimetric analysis. Thermogravimetric analysis.
9. Titrimetric Analysis – I: The basics of titrimetric techniques. Categories and types of titrations. Activity and Chemical balance. Instruments, Labware and Materials.
10. Titrimetric Analysis – II: a) Acid-base titrations. The solvant effect. Standard solutions and indicators. Applications. b) Precipitation titrations. The Mohr, Volhard and Fayans methods. Standard solutions and indicators. Applications.
11. Titrimetric Analysis – III: a) Complexometric titrations. Standard solutions and indicators. Applications. b) Oxidation-reduction (redox) titrations. Standard solutions and indicators. Applications.
12. a) Introduction to the spectroscopic techniques of analysis: UV/Vis spectroscopy, IR spectroscopy, Atomic spectroscopy, Mass spectroscopy. b) Introduction to the chromatographic techniques of Analysis: Basic quantities in Chromatographic Analysis. Gas chromatography. Liquid chromatography. Mobile/stationary phases interactions.
13. Quality control, health and safety in the laboratory: Quality systems costs and benefits, inspection and review. The responsibility of the administration and the personnel. Safety in the laboratory. Hazardous substances and devices. Laboratory wastes management.

B.Laboratory part

1. Introduction to acid-base titrimetry: Standard solutions and indicators. Preparation and titration of a standard acid solution.
2. Analysis of a Na₂CO₃ aqueous sample of unknown concentration. Preparation and titration of a standard NaOH solution. Acidity determination in a wine or vinegar sample.
3. Analysis of alcaline mixtures using two separated or two consecutive titrations.
4. Introduction to the precipitation titrations – Chloride determination using the Mohr method.
5. Precipitation titrimetry curves – Chloride determination using the Volhard method.
6. Introduction to the complexometric titrations – Water hardness determination.
7. Complexometric determination of Zn and Al.
8. Introduction to the redox titrations – Preparation and titration of a standard KMnO4 solution.
9. Determination of Fe²⁺ and Η₂Ο₂ using manganiometry.
10. Iodometric determination of OCl^– and Cu²⁺.
11. Introduction to Gravimetric analysis – Fe/Al ratio determination in a sample.
12. Gravimetric detrmination of SO₄^2-.
13. Acid-base potentiometric titrations.

 

Suggested bibliography

1. In greek

A1: Βιβλία από την πλατφόρμα ΕΥΔΟΞΟΣ:

• ChristianG.D. & al (2019) “Αναλυτική Χημεία”, Κωδικός Βιβλίου στον Εύδοξο: 86199898.
• DanielC. & LucyC.A. (2021) “Αναλυτική Χημεία”, Κωδικός Βιβλίου στον Εύδοξο: 94644882.

Α2: Αλλα βιβλία και βοηθήματα:

• Παπακωνσταντίνου Σ.Π. (2017), “Ποσοτική Χημική Ανάλυση_Συμπληρωματικές Σημειώσεις Θεωρείας” (αρχείο pdf διαθέσιμο δωρεάν στους φοιτητές του Τμήματος).
• Γκέργκης Β.Χ. κ.ά (2013) “Ποσοτική Αναλυτική Χημεία – Εργαστηριακές Ασκήσεις”, (αρχείο pdf διαθέσιμο δωρεάν στους φοιτητές του Τμήματος καθώς και σε έντυπη μορφή).

1. In english:

• Harvey D., “Analytical Chemistry 2.1”, Libre text Project 2023, free from: chem.libretexts.org