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Identification of Historical Colourants by Mass Spectrometry Volodymyr Pauk

Palacky University in Olomouc Faculty of Science Department of Anlalytical Chemistry. Identification of Historical Colourants by Mass Spectrometry Volodymyr Pauk under the supervision of prof . Lemr. Olomouc 2012. Ref. [1]. Outline 1. Introduction 2. Experimental 3. Results

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Identification of Historical Colourants by Mass Spectrometry Volodymyr Pauk

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  1. Palacky University in Olomouc Faculty of Science Department of Anlalytical Chemistry 18.05.2012 by V.Pauk Identification of Historical Colourants by Mass Spectrometry VolodymyrPauk under the supervision of prof. Lemr Olomouc 2012 Ref. [1]

  2. Outline 1. Introduction 2. Experimental 3. Results 4. Conclusion 18.05.2012 by V.Pauk

  3. Introduction • 1. Identification of colourants: • restoration • evaluation • approximate dating • 2. ‘The Legend’ 18.05.2012 by V.Pauk a b c Partial views of ‘Crucifixion’, St. Šebestian church on St. Hill in Mikulov Ref. [2]

  4. Introduction 3. Prussian Blue vs Indigo 18.05.2012 by V.Pauk Prussian blue Indigo • dark-blue shade • small shaped particles • high tinting strength • highly insoluble in water and organic solvents Synthetic,18th century, Berlin 18th – 19th century Natural, plant origin Antique times – 19th century (replaced by synthetic dye) Fe4[Fe(CN)6]3 Iron (III) hexacyanoferrate (II) Indigotine Ref. [3, 4, 5]

  5. Experimental • Equipment: • Micromass Q-TOF Premier, Z-spray ESI source, negative mode; • Acquity UPLC system; Elma S40H ultrasound bath, 0.45 µm filters. • Sample preparation: • Eq. 1 Fe4[Fe(CN)6]3 + NaOH → Fe(OH)3↓ + Na4[Fe(CN)6] • Eq. 2 • Data acquisition and processing: • m/z 133.95 (Prussian blue), m/z 263.08 (indigotin), • Mass lynx v. 4.0 (Waters Laboratory Informatics) • QC Expert v. 3.2 (TriloByte LTD.) 18.05.2012 by V.Pauk

  6. Results 18.05.2012 by V.Pauk a) and b) FIA mass-chronograms of Prussian blue and indigo; curves I, II, and III respond to 100, 1000 and 5000 ng/mL , respectively; integrated peak areas for 5000 ng/mL are shown; c) MS spectrum of Prussian blue d) MS spectrum of indigo Traces of Prussian blue in samples !!! • LOD: 10 ng/mL, • 47 pg absolute • LOD: 12 ng/mL, • 59 pg absolute Linear calibration up to 5000 ng/mL

  7. Conclusion 18.05.2012 by V.Pauk • Developed method: • successful in analysis of real samples • fast • sensitive • no chromatographic separation • Application: • Fast screening of Prussian blue and indigo in historical and art objects

  8. References • [1] Reproduction of Peter Paul Rubens - La découverte de la pourpre available on http://no.wikipedia.org/wiki/Fil:Peter_Paul_Rubens__La_d%C3%A9couverte_de_la_pourpre.JPG. • [2] Partial photos of the painting of ‘Crucifixion’, St. Šebestian church on St. Hill in Mikulov, Czech Republic, available on http://breclavsky.denik.cz/multimedia/galerie/2328622.html?section=1,1. • [3] Kirby, J.; Saunders, D. Fading and colour change of Prussian blue: methods of manufacture and the influence of extenders. National Gallery Technical Bulletin (London), 2004, 25: 73 – 99. • [4]Bartoll, J. The early use of prussian blue in paintings. 9th International Conference on NDT of Art, Jerusalem Israel, 25–30 May 2008. • [5] Bechtold, T.; Mussac, R. Handbook of natural colorants. Wiley, 2009, 412 p. 18.05.2012 by V.Pauk

  9. 18.05.2012 by V.Pauk • Thank youfor attention

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