Abstract
Accelerated ageing is an often-used tool in conservation research, yet difficult to apply to parchment due to the materials inherent heat sensitivity. The complexity of this organic material makes the analysis of its deterioration especially challenging. An attempt to develop a non-heat ageing protocol for parchment is described in this paper. The work was performed within the scope of a MA-thesis at the State Academy of Art and Design Stuttgart. Samples of a modern new limed goat parchment and pieces of reconstituted parchment made from bovine hide powder were subjected to a combination of light ageing and dynamic ageing at moderate temperatures. All samples were analysed with the goal to observe degradation on as many structural levels as possible: colour measurement via VIS spectrometry and light-microscopic observation of fibre damage were employed to assess visible changes. Shrinkage temperature (Ts) was measured as an indicator for the amount of intact intrafibrillar bonds and the determination of the maximum moisture absorption capacity gave an impression on the parchments overall level of hygroscopy. In addition, PMF (Peptid Mass Fingerprinting) via MALDI/MS TOF was performed on extracts from unaged and light aged goat parchment. The results of the different types of analysis showed significant degradation on different structural levels of the parchment, indicating that accelerated ageing of parchment that uses a combination of light and dynamic ageing may be a viable alternative to the more commonly applied thermal ageing.
Zusammenfassung
Künstliche Alterung von Pergament – Untersuchungen eines photokatalysierten Niedrigtemperatur Ansatzes
Künstliche Alterung ist ein in der restauratorischen Forschung häufig angewandtes Hilfsmittel, das jedoch aufgrund der materialtypischen Hitzempfindlichkeit nur schwer auf Pergament anwendbar ist. Zudem erschwert die Komplexität dieses organischen Schriftträgers die Untersuchung seines Erhaltungszustandes. In dem vorliegenden Beitrag werden die Ergebnisse einer Versuchsreihe zur Entwicklung eines hitzefreien Alterungszyklus für Pergament zusammengefasst, die Thema einer Master-Thesis von der Staatlichen Akademie der Bildenden Künste Stuttgart war. Proben eines neuen, kalkgeäscherten Ziegenpergaments und eines rekonstituierten Pergaments aus Rinder-Hide Powder wurden zunächst Licht- und anschließend bei moderaten Temperaturen dynamisch gealtert. Die Probenauswertung hatte eine möglichst genaue Betrachtung aller Strukturebenen zum Ziel: Farbmessungen mittels VIS- Spektroskopie und eine lichtmikroskopische Faseruntersuchung dienten der Erfassung sichtbarer Veränderungen, während die Messungen der Schrumpfungstemperatur (Ts) und die Bestimmung der maximalen Feuchteabsorptionskapazität Aufschluss über intakte intrafibrillare Bindungskräfte und die Hygroskopie lieferten. Zusätzlich wurde an Extrakten des ungealterten und lichtgealterten Ziegenpergaments eine PMF-Untersuchung mittels MALDI-TOF durchgeführt.
Die Untersuchungsergebnisse zeigten für alle Proben einen fortgeschrittenen Abbau auf verschiedenen Strukturebenen. Eine Kombination von Licht – und dynamischer Alterung stellt eine mögliche Alternative zur üblichen thermischen Alterung dar.
Résumé
Le vieillissement accéléré du parchemin
Le vieillissement accéléré du parchemin est un instrument souvent utilisé en recherche de conservation, cependant difficile à appliquer au parchemin en raison de la sensibilité inhérente de ce matériau à la chaleur. La complexité de ce matériau organique complique particulièrement l´analyse de sa détérioration. Nous décrirons une tentative de développer un protocole de vieillissement pour le parchemin sans chaleur. Ce travail a été réalisé dans le cadre d´un Master à l´Académie des Arts et du Design de Stuttgart. Des échantillons d´un parchemin de chèvre moderne nouvellement chaulé et des morceaux de parchemin reconstitué faits à partir de poudre bovine ont été soumis à une combinaison de vieillissement modéré et dynamique à des températures modérées. Tous les échantillons ont été analysés avec pour objectif d´observer la dégradation à autant de niveaux structurels que possible: spectrométrie pour évaluer le changement de couleur et une observation sous microscope normal des dégâts causés aux fibres ont été utilisées pour évaluer les changements visibles. Un rétrécissement à la température (Ts) a été utilisé comme indicateur de la quantité de liaisons intra-fibrilles intactes et la détermination de la capacité d´absorption maximale d´humidité a servi à déterminer le degré général d´hygroscopie des parchemins. De plus, PMF via MALDI/MS TOF a été réalisé sur des extraits de parchemin de chèvre non vieilli et légèrement vieilli. Les résultats des différents types d´analyses ont montré une dégradation significative des différents niveaux internes du parchemin, indiquant que le vieillissement accéléré du parchemin combinant un vieillissement modéré et dynamique pourrait être une alternative au vieillissement accéléré thermique plus communément utilisé.
About the authors
Marie Kern is a graduate of the education program for Conservation and Restoration of works of art on paper, archive- and library materials at the State Academy of Art and Design in Stuttgart, where she obtained her Masters Degree in 2015. From 2015 to 2017 she has been working as a postgraduate intern at the paper conservation department of the Staatsgalerie Stuttgart and is now employed as a conservator for paper-based artworks at the LWL Museum für Kunst und Kultur in Münster, North Rhine Westfalia. The research presented in this article was the subject of her Master Thesis.
Andrea Pataki-Hundt from 1998 until 2017 she was research assistant at the graduate conservation programme for works of art on paper, archive- and library materials, State Academy of Art and Design Stuttgart, where she also obtained her diploma (1997) and her PhD (2005). In 1998, she was an advanced fellow at the Walters Art Museum Baltimore, supported by DAAD. From 2007 to 2009 she conducted a two-year postdoctoral research programme. In spring 2008 she was a museum guest scholar at the J. Paul Getty Museum, Los Angeles.
Since autumn 2017 she holds a professorship at the Cologne Institute of Conservation Science (CICS) at the conservation programme for documents, works of art on paper, photography, and illuminated manuscripts.
Dr Jan Wouters gained his PhD from the University of Gent, Belgium, in 1978 (chemistry, biochemistry). From 1982, he joined the research laboratory of the Royal Institute for Cultural Heritage (KIK/IRPA) in Belgium. In 1996 he was appointed head of the Laboratory for Materials and Techniques at that institute. He holds an invited professorship at the Intitute for Sustainable Heritage, University College London, UK. He is an active member of the Conservation Committee of the International Council of Museums (ICOM-CC) since 1990. From 2002 through 2008 he was a member of the Directory Board of that Committee and, from 2005 through 2008 he was the President of that Board. He is a co-editor of e-Preservation Science. He is author or co-author of some 180 contributions published in journals, congress proceedings and book chapters.
Daniel P. Kirby after careers as an analytical chemist in semiconductor electronics, pharmaceuticals and academic research, Dan turned his interest to conservation. With over 30 years experience in analytical mass spectrometry, Dan is currently in private practice specializing in applications of mass spectrometry in art, cultural heritage, and wildlife forensics. Recent projects include characterization of pigments and binding media in historic Australian Aboriginal bark paintings and using peptide mass fingerprinting to identify materials in Native Alaska objects, Cross River dance masks, Dr Auxoux’s papier mâché anatomical models, Pre-Columbian Mexican feather shields and coatings on photographic salt prints.
Acknowledgements
This research was originally undertaken as a MA project at the State Academy of Art and Design in Stuttgart and as such, we are grateful to several people and associations which have contributed to this original work. The Förderverein Papierrestaurierung enabled and supported this project for which we are grateful. Mario Röhrle of the State Academy of Art and Design offered his expertise and advice regarding the colour measurement of (semi-) transparent samples and the calculation of colour difference within the CIELab colour space. Dorte V.P. Sommer of the The Royal Danish Academy of Fine Arts kindly shared her experience in the microscopic analysis of parchment fibres. Maria Krämer provided professional feedback, inspiration and support during the project.
Appendix
MALDI-TOF / MA sample preparation according to Kirby et al. 2013:
place samples in 600 μL Eppendorf tubes
60 μL 50 mM ammonium bicarbonate (AMBI), 60 °C, 30 min with intermittent vortexing/agitation
reduce disulfides: 3 μL 20 mM Tris (2-carboxyethyl) phosphine hydrochloride in 50 mM AMBI at 37 °C for 15 min
endcap free sulfhydryls: 3 μL 40 mM iodoacetamide in 50 mM AMBI for 15 min, RT, dark
digest: 8 μL trypsin (0.02 ug/μL in 50 mM AMBI), 37 °C overnight
MALDI analysis
Alpha-cyano-4-hydroxycinnamic acid (αCHCA) matrix prepared as a saturated solution in 40 % (v-v) acetonitrile (ACN) – 0.1 % trifluoroacetic acid (TFA)
samples (4 μL) mixed with matrix (20 μL) in a separate tube and spotted on the MALDI plate
six peptide standards from 904 Da to 3657 Da spotted on the plate as external calibrants
a Waters microMX Laser Desorption-Time of Flight Mass Spectrometer operated in reflector mode used to collect positive ion spectra from 800–3800 Da. Resolution is typically greater than 8000 (mass/Δ mass) allowing baseline resolution of isotopes over the mass range of interest and monoisotopic mass accuracy at least ± 0.1 Da.
mMass freeware for MALDI/TOF spectra:
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