Instrumental Chemical Analysis – Methods of Chemical Analysis and Characterization

Course Code:

Π1 4030


4th Semester

Specialization Category:

Required ( ΜΕΥ )

Course Hours:




Course Tutors

Yorgos Facorellis

Course Description
Course Theory
A. Spectroscopic methods of analysis:
 Electromagnetic radiation. Basic physical quantities and concepts: intensity, frequency, energy and wavelength. Categories of electromagnetic radiation.
 Absorption in the UV-visible region. Electronic transitions of molecules. Quantity expressions of light absorption: transmittance (T) and absorbance (A). Beer’s Law. Basic instrumentation of UV-visible absorption spectroscopy: the double beam technique; monochromators and detectors. Shapes and forms of absorption spectra.
 Molecular fluorescence. Fluorescence emission and its relationship to absorption in the UV-visible. Requirements for molecular fluorescence. Phosphorescence. Basic instrumentation and recording excitation and emission spectra. Applications of fluorescence.
 Absorption of molecules in the Infra Red. Fourier Transform Infra Red (FTIR) spectroscopy. Vibrations of bonds in molecules. Stretching and bending vibrations. Basic instrumentation in FTIR spectroscopy: Michelson’s interferometer and Fourier transform. Transmittance and reflectance techniques. Advanced sampling techniques: Attenuated Total Reflection (ATR), diamond cell and microscopy-FTIR. Recording spectra from KBr pellets and films. Interpretation of FTIR spectra.
 X-ray Diffractometry (XRD). Sources of monochromatic X-rays. Diffraction phenomena. Bragg’s law. Detection of single phase crystalline materials. Detection of multiphase materials in powdered samples (stone samples and minerals). Sampling: forms and types of samples. Basic instrumentation and geometric conditions for recording of spectra. Using libraries in the interpretation and verification of XRD spectra.
 X-Ray Fluorescence (XRF), Scanning Electron Microscopy (SEM): operating principles, sources of electron beam; focusing lenses. Interaction of electron beam with sample. Elastic scattering of electrons and back-scattered electrons. Non-elastic scattering, secondary electrons, Auger electrons, X-rays, cathodoluminescence. Image formation in electron spectroscopy. Sampling requirements. X-Ray microanalysis in Scanning Electron Microscopy (SEM-EDAX).

 Partition of sample molecules between two phases: mechanism and partition coefficient. Other mechanisms of chromatographic separation: adsorption, ion exchange, size exclusion.
 Instrumental separation techniques: Chromatographic Techniques. Mobile and stationary phase. Categories of chromatographic techniques. Mobile and stationary phases; categorizing chromatographic techniques according to separation mechanisms.
 Planar chromatography. Thin Layer Chromatography (TLC). Specializing and fine-tuning of mobile phase according to samples types.
 Gas chromatography (GC) and High Performance Liquid Chromatography (HPLC). Basic instrumentation: temperature programming in gas chromatography; types of columns and detectors in the two techniques. Chromatographic peaks; expressions for evaluating quality of separation. Chromatographic resolution. Application of each technique according to the type of samples. Quantitative information: integration of peaks. Quantitative criteria: response factors. Techniques combined with mass spectrometry: GC-MS and LC-MS.
 Methods of dating archaeological findings: Dendrochronology.
 Dating with carbon-14 (C14).
 Luminescence dating. Dating with uranium rows and amino acids racemization. Other dating techniques.

Course Practices
The laboratory part of the course will include practices, where students will participate in selected characterization techniques of inorganic and organic art and archaeology materials:

• Sampling-Optical Microscopy
• Special Observation Techniques/Fluorescence Microscopy/ Selective staining
• Crystallography
• TLC,
• GC,
• C14 dating,
• Dendrochronology.
• Reports Evaluation -Test

The Scope of the Course

To present the necessity of materials characterization and methods of dating; to provide the students with decision-making skills for selecting the suitable characterization methodologies among a large number of available techniques.

After the completion of the course students will be able to:
-understand the working principle of the most important characterization and dating techniques.
-propose an appropriate spectroscopic and / or chromatographic technique and a method of selective staining-optical microscopy of cross sections to characterize the materials that make up an object.
-Decision-making and applying an appropriate sampling method or protocol for certain techniques. Interpret basic information resulting from various spectroscopic and separation techniques.
-choose an appropriate archaeological dating method for certain types of materials.
To convey the skills for obtaining and handling samples for various techniques to the students;
-acquire hands-on experience in the use of selected available specific methods and techniques; extracting information out of the results from specific techniques; to interpret the acquired information; to illustrate the possibilities and limitations of the relevant techniques.
-Use basic image processing and data analysis software (ImagePro/Leica Application Suite (LAS) and consult specific databases (ifac.cnr, copa etc)

Language of evaluation: Greek
Students’ evaluation (100%):
The student’s final grade results from 50% of the grade of the theoretical part and 50% of the grade of laboratory practice.
I. Written final exam in theory (50%) which includes:
multiple choice questions, open-ended questions, critical questions, comparison data.
II. Evaluation of students’ performance during the laboratory exercises which includes laboratory written assignments (technical reports) and short written evaluation (50%).

 Alexopoulou A., Sperantza, C., Ioakeimoglou, E., Paterakis, A., Kaminari, A., 2012, Documentation and Conservation of a wooden canopric chest, in Proceedings of the 5th Symposium of the Hellenic Society for Archaeometry Association Editors: N. Zacharias, M. Georgakopoloulou, K. Polykreti, G. Fakorellis, Th. Vakoulis, Kalamata: University of the Peloponnese – Papazisis
 Burns,R.G., 2009, Mineralogical application of crystal field theory 2nd ed, Cambridge Topics in Mineral Physics and Chemistry 5 Cambridge University Press
 Derrick, M. R., Stulik, D. and Landry, J. M. , 1999, Infrared Spectroscopy in Conservation Science, Los Angeles: The Getty Conservation Institute,
 Doménech-Carbó, M.T. and Costa, V. 2009, Electrochemical Methods in Archaeometry, Conservation and Restoration, Berlin, Heidelberg: Springer-Verlag
 Eastaugh, N., Walsh, W., Chaplin, T., Siddhal, R., 2014, Pigment compendium. Optical Microscopy of Historical Pigments, Oxford: Elsevier. Daniel C. Harris, Exploring Chemical Analysis, W. H. Freeman; 4th edition (May 16, 2008)
 FitzHugh ,E.W (ed)., 1997, Artists Pigments. A Handbook of their History and Characteristics 3 National Gallery of Art, Washington &Oxford University Press
 Harris, C.D., 2008, Exploring Chemical Analysis, W. H. Freeman; 4th edition.
 Mazzeo, R., 2017, Analytical Chemistry for Cultural Heritage, Weinheim: Springer
 Rouessac, F. and Rouessac, A., 2007, Chemical Analysis: Modern Instrumentation Methods and Techniques, New York: Wiley, 2 edition
 Rouessac, F. and Rouessac, A. 2007, Chemical Analysis: Modern Instrumentation Methods and Techniques, New York:Wiley, 2 edition
 Skoog, D., J.Holler,J, Nieman,T., 2005, Αρχές της Ενόργανης Ανάλυσης, Aθήνα: Κωσταράκης,
 Stuart, B.H., 2007 Analytical Techniques in Materials Conservation, Chichester: John Wiley & Sons
 Taylor R.E. and Aitken M.J., 1997, Chronometric Dating in Archaeology, Advances in Archaeological and Museum Science, vol. 2, New York and London: Plenum Press.
 Λυριντζής,I., 1994, Αρχαιομετρία. Μέθοδοι χρονολόγησης στην αρχαιολογία, Aθήνα: Καρδαμίτσα.
 Λυριντζής,Ι. 2005, Φυσικές επιστήμες στην αρχαιολογία, Αθήνα: Τυπωθήτω
 Οξενκιουν-Πετροπούλου, Μ., 2020, Φασματομετρικές Μέθοδοι στην Σύγχρονη Ενόργανη Ανάλυση, Αθήνα: Τσότρας

Journal of Archaeological Science
Journal of Cultural Heritage
Journal of Mediterranean Archaeology and Archaeometry