Learning objectives
Let students know the basis of analytical techniques usually employed in petrology and geochemistry in the study of the works of art, which are built, at least in part, with geological stuff. These techniques is shown in both the diagnostic phase of degradation of the stuff and in the restoration works, with the aim to suggest a way to preserve the works of art in a restoration project and to indicate the place where to find suitable raw materials to employ in the restoration works.
Prerequisites
Knowledge of the base concepts of general mineralogy; systematic mineralogy as for silicates and oxides normally occurring in rocks and usually employed in pigments. Knowledge of the employment of the optical transmitted light mineralogy microscope. Basal knowledge on physics, as for electromagnetic waves. Knowledegde of the basis of the inorganic chemistry
Course unit content
<strong>1. Scientific therminology</strong><br />
a. on analyitical methods<br />
b. on sampling techniques<br />
c. on measurements<br />
d. statistics of measurements<br />
<br />
<strong>2. sampling</strong><br />
a. microsampling on works of art<br />
b. sample representativity<br />
c. sampling anisotropic rocks<br />
d. selective sampling<br />
e. subsamples and aliquotes<br />
<br />
<strong>3. samples handling </strong><br />
a. plasters<br />
b. paintings (frescoes, pictures, …)<br />
c. rocks;<br />
d. sample homogeneization<br />
e. subsampling and aliquot drawing<br />
f. introduction to draw samples not representative of the system<br />
<br />
<strong>4. mineral separation</strong><br />
a. aims and results<br />
b. magnetic methods of separation<br />
c. gravimetric separation employing heavy liquids<br />
d. Hand picking<br />
<br />
<strong>5. Analysis of volatile components</strong><br />
a. definition of volatile component in the Earth Sciences<br />
b. loss on ignition (LOI)<br />
c. CHNS method<br />
<strong><br />
6. analysis of elements which occur in different redox state</strong><br />
a. iron, titanium, chromium, sulphur<br />
b. analysis of divalent and trivalent iron through titration<br />
c. analysis of divalent and trivalent iron through Mössbauer spectroscopy<br />
d. high energy methods to in situ analysis of divalent and trivalent iron<br />
<br />
<strong>7. X-rays</strong><br />
X-ray generation<br />
Optical characters of X-ray radiation<br />
X-ray employment in diffractometry<br />
X-ray employment in X-ray fluorescence spectroscopy<br />
<strong><br />
8. X-ray diffraction</strong><br />
Basical on diffraction phenomena<br />
Crystal lattice as diffraction lattice<br />
Model approximations and usefulness<br />
Laue conditions of diffraction<br />
Bragg equation<br />
Diffracted X-ray intensities<br />
Diffraction effects of minerals and their “signature” in their diffraction patterns<br />
Resolution ability for instruments which employ electromagnetic waves<br />
Employment of diffraction in diffractometry s.s., in X-ray fluorescence spectrometry and in electron microanalysis<br />
<strong><br />
9. Diffraction techniques</strong><br />
Aims of a diffractometric analysis<br />
Single crystal methods<br />
Powder methods<br />
Debye-Sherrer and Gandolfi cameras<br />
Powder diffraction on planar sample holders<br />
Outlines on four rings diffractometry<br />
Identification of a single mineral<br />
Identification of minerals in a mixture<br />
Diffraction techniques for clay minerals<br />
Outlines on quantitative diffractometry<br />
<br />
<strong>10. X-ray fluorescence spectrometry</strong><br />
Sample handling<br />
Glass disks and powder pellets<br />
Parameters on the instrument<br />
Net peak calculation<br />
Calibration curves<br />
Analytical limits of the method<br />
<br />
<strong>11. portable X-ray fluorescence spectrometers</strong><br />
main differences between portable and laboratory equipments<br />
analytical limits.<br />
<br />
<strong>12. outlines on other analytical techniques on unmodified samples </strong><br />
a. ICP-MS (Inductively Coupled Plasma and Mass Spectrometry)<br />
b. ICP-OES (Inductively Coupled Plasma and Optical Emission Spectroscopy)<br />
c. LA-ICP-MS (Laser Ablation Inductively Coupled Plasma and Mass Spectrometry)<br />
<br />
<br />
<strong>13. in situ analyses on thin sections</strong><br />
a. Scanning Electron Microscope with micronalysis<br />
<ul>
<li>General running outlines</li>
<li>Sources and detectors</li>
<li>Qualitative chemical microanalysis</li>
<li>Quantitative chemical microanalysis</li>
<li>Averaged chemical analyses, on linescans and on areas</li>
<li>Quantitative chemical analysis maps</li>
</ul>
b. Electron Probe MicroAnalysis<br />
<ul>
<li>General running outlines</li>
<li>Performance differences between electron microprobe and scanning electron microscope</li>
<li>Sources and detectors</li>
<li>Employment of the instrument</li>
</ul>
c. outlines on Laser Ablation Inductively Coupled Plasma and Mass Spectrometer<br />
<br />
<strong>14. Isotope analyses</strong> <br />
e. classic mass spectrometry on radioactive and radiogenic isotopes<br />
f. in situ mass spectrometry (SHRIMP) on radioactive and radiogenic isotopes <br />
g. oxygen isotope analysis on silicates and oxides <br />
h. outlines on the in situ oxygen isotope analyses, on silicates and oxides<br />
<br />
<strong>15. ultraviolet light microscope</strong><br />
a. General running outlines<br />
b. Employment in studying thin sections of rocks, mortar, plaster<br />
<br />
<strong>16. laboratory experiments</strong><br />
a. rock sample handling: thin section and cross section preparation; grinding, milling and homogeneization, aliquot extraction for chemical analyses<br />
b. painting sample handling (frescoes, pictures) : cross section preparation<br />
c. sample preparation for XRF analysis<br />
d. sample preparation for standard X-ray diffractometry<br />
e. sample preparation for clay minerals X-ray diffractometry<br />
f. SEM-EDS analysis on rock samples (qualitative, quantitative, averaged, chemical maps)<br />
g. SEM-EDS analysis on plaster samples (qualitative, quantitative, averaged, chemical maps)<br />
h. SEM-EDS analysis on fresco samples (qualitative, quantitative, averaged, chemical maps)
Full programme
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Bibliography
<strong>Armigliato A. & Valdrè U.</strong> (1982): Microscopia elettronica a scansione e microanalisi – parte I. <em>Università degli Studi di Bologna, 411 pp</em>. <u>Of interest</u>: capp. 1, 2, 3. <br />
<strong>Armigliato A. & Valdrè U.</strong> (1982): Microscopia elettronica a scansione e microanalisi – parte II. <em>Università degli Studi di Bologna, 356 pp</em>. <u>Of interest</u>: capp. 1, 2, 3.<br />
<strong>Bonatti S. & Franzini M.</strong> (1984): alcune indicazioni sul reticolo reciproco. <em>Da: “Cristallografia mineralogica”, Boringhieri, Torino, 361 pp</em>. <u>Of interest</u>: cap. 6.<br />
<strong>Bonissoni G.</strong> (1977): introduzione alla spettrometria dei raggi X di fluorescenza. <em>ETAS Libri, 245 pp</em>. <u>Of interest</u>: capp. 1, 2, 3, 4, 5.<br />
<strong>Currie L.A.</strong> (1995): Nomenclature in evaluation of analytical methods including detection and quantification limits. <em>Pure & Appl. Chem., 67(10): 1699-1723</em>.<br />
<strong>Droop. G.T.R.</strong> (1987): A general equation for estimating Fe3+ concentrations in ferromagnesian silicates and oxides from microprobe analyses, using stoichiometric criteria. <em>Mineralogical Magazine, 51: 431-435</em>.<br />
<strong>Gallone A.</strong> (1990): Analisi fisiche e conservazione. <em>Franco Angeli, 182 pp</em>.<br />
<strong>Horwitz W.</strong> (1990): Nomenclature for sampling in analytical chemistry. <em>Pure & Appl. Chem., 62(6): 1193-1208.</em><br />
<strong>Hutchinson C.S.</strong> (1974): laboratori handbook of petrographic techniques. <em>Wiley, 527 pp</em>. <br />
<strong>Jordan C.F. Jr., Fryer G.E., Hemmen E.H.</strong> (1971): Size analysis of silt and clay by hydrophotmeter. <em>J. Sedim. Petrol., 41(2): 489-496</em>.<br />
<strong>Klein C.</strong> (2008): Mineralogia. Zanichelli, 606 pp. <u>Of interest</u>: cap. 7. AA.VV.: Intensità delle radiazioni X diffratte. A<em>ppunti dalle lezioni (Roma)</em>.<br />
<strong>Lazzarini L. & Laurenzi Tabasso M. </strong>(1986): Il restauro della pietra. <em>CEDAM, 320 pp</em>. <br />
<strong>Matteini M. & Moles</strong> <strong> A.</strong> (1999): La chimica nel restauro – I materiali nell’arte pittorica. <em>Nardini editore, 379 pp.</em><br />
<strong>Potts J.</strong> (1997): A glossary of terms and definitions used in analytical chemistry. <em>Geostandard Newsletters, 21(1): 157-161.</em><br />
<strong>Ricci Lucchi F.</strong> (1980): Sedimentologia – parte I. <em>CLUEB</em>. <u>Of interest</u>: cap. 2.3.1. <br />
<strong>Rigault G</strong>. (1966): Alcune indicazioni sul reticolo reciproco. <em>Da: “Introduzione alla cristallografia”, Livrotto e Bella, Torino</em>.<br />
<strong>Salvioli Mariani E.</strong> (2005): microscopia elettronica a scansione e microanalisi. <em>Appunti dalle lezioni.</em><br />
<strong>Seccaroni C. & Moioli P.</strong> (2002): Fluorescenza X – prontuario per l’analisi XRF portatile applicata a superfici policrome. <em>Nardini editore, 161 pp</em>. <u>Of interest</u>: part I.<br />
<strong>Simmons G.</strong> (1959): The photo-<em>extinction method for the measuremente os silt-sized particles. </em>J. Sedim. Petrol., 29(2): 233-245.
Teaching methods
<strong>TEACHING TECHNIQUES</strong><br />
Outline of the general concepts in the analytical techniques. Description of analytical techniques, highlighting, for each of them, potentials and limits. Laoratory activities in both sample handling and sample analyzing, employing all the laboratories at the present available in the Earth Science Department of the University of Parma. <br />
<strong>EXAMINATION</strong><br />
Oral exam: basis of concepts of analytical techniques; details on a specific analytical technique, and its possible employment in a project of restoration of a wirk of art.
Assessment methods and criteria
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Other information
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