Microanalysis of Parchment

A presentation of cutting-edge sampling techniques and microanalytical, semi-microanalytical, and non-destructive methods for examining historic parchment, focusing on visual, microscopic, chemical, and physical approaches. Drawing on the achievements of the European project ‘Methods in the Microanalysis of Parchment,’ this volume addresses the challenges of studying fragile and invaluable cultural objects while minimizing sampling.

Parchment in the form of manuscripts, scrolls, charters, book covers and substrata for artworks, makes a major contribution to the most valuable objects of European cultural heritage. Large collections exist in varying degrees of preservation in public and private libraries, archives, museums and in diverse religious foundations. The degradation of parchment involves the decay of the intact fibre structure through different stages of alteration to a terminal stage when the fibre structure is close to complete disintegration. In contact with water or storage in moist conditions, the fibres then transform into a gelatinous substance. Objects made of parchment are of a very complex chemical and physical nature and sampling from these precious objects is normally highly restricted. Analysis therefore needs to be based on very accurate microanalytical or non-destructive methods which are able to produce valid results. Microanalysis of Parchment presents sampling techniques and non-destructive, microanalytical and semi-microanalytical methods for the analysis and testing of historic parchment based on visual, microscopical as well as chemical and physical techniques. The contributions in this volume represent the main achievements of the European joint project on parchment ‘Methods in the Microanalysis of Parchment’ sponsored by the European Commission.

ContributorsAcknowledgementsPrefaceRene LarsenIntroductionRene LarsenParchmentMaterialsMicrosampling and microscopical assessment of parchment including microchemical analysis of binding media, dyes and inkA new microsampling technique for parchmentLeopold Puchinger and herbert StachelbergerIntroductionDescription of the microdrilling instrumentDrill sizes and technique of needle sharpeningEvaluation of drill bits and holes left in the parchment - applicationsSummaryReferencesEvaluation of old parchment collagen with the help of transmission electron microscopy (TEM)Leopold Puchinger, Dietmar Leichtfried and Herbert StachelbergerIntroductionMaterials and methodsDiscussion of the results obtained with TEMDiscussion of the results from TEM by comparison with other methodsConclusionsReferences Evaluation of methods for the microanalysis of materials added to parchmentJan Wouters, Johan Claeys, Karijn Lamens and Marina Van BosIntroductionHistorical sources for the composition of miniaturesMaterials and methodsResults and discussionConclusionAcknowledgementsReferencesChar acterization of vegetable gums used as binding media in inks by gas chromatography and multivariable analysisPascale Richardin, Sylvette Bonnassies-Termes and Jean-Christophe DoreIntroductionExperimentalCharacterization by gas chromatography of neutral sugars and uronic acidsAnalysis of vegetable gumsApplication to metallogallic inksConclusionAcknowledgementsReferencesAppendices Sulphur inclusions within parchment and leather exposed to sulphur dioxideDerek J. Bowden and Peter BrimblecombeIntroductionExperimentalResultsDi scussionConclusionsAcknowledgementsEndnotesReferen ces Thermophysical and thermochemical analysis of microsamplesThe hydrothermal stability (shrinkage activity) of parchment measured by the Micro Hot Table Method (MHT)Rene Larsen, Dorte V. Poulsen and Marie VestIntroductionExperimentalSamplesResults
DiscussionConclusionsReferencesThe thermal response of parchment and leather to relative humidity changesDerek Bowden and Peter BrimblecombeIntroductionBackgroundExperimental
Examples and resultsConclusionsEndnotesReferences Characterization of historic and unaged parchments using thermomechanical and thermogravimetric techniquesMarianne Odlyha, Neil Cohen, Gary Foster and Roberto CampanaIntroduction to termomechanical and thermogravimetric techniquesDynamic mechanical thermal analysis (DMTA): stress-strain measurementsDMTA: Measurement of viscoelastic propertiesDMTA: Underwater heating creep measurementsThermogravimetry analysis (TGA)Overall conclusions from thermomechanical and Thermogravimetric measurementsPrincipal conponent analysis (PCA)References Chemical and structural characterization of collagen and palaeogenetics of parchmentAmino acid analysis of new and historical parchmentsRene Larsen, Dorte V. Poulsen, Marie Vest and Arne L. JensenIntroductionExperimentalResultsDiscussi onConclusionReferences13C and 15N solid state nuclear magnetic resonance (NMR) spectroscopy of modern and historic parchmentsMarianne Odlyha, Neil Cohen, Gary Foster, Roberto Campana and Abil AlievIntroductionExperimentalResults (13C NMR spectra)Results: 15N solid state NMR spectraConclusionsReferencesStudy of the chemical breakdown of collagen and parchment by Raman spectroscopyThomas Garp, Kurt Nielsen, and Soghomon BoghosianThe principles and methods of Raman spectroscopyFT-Raman spectroscopic studies of parchementConclusionsReferencesDetection of radicals in collagen and parchment produced by natural and artificial deterioration, electron spin resonance spectroscopy (ESR) and its implications for artificial ageing and test of conservation treatmentsDaniella Bechmann Hansen, Kurt Nielsen and Sen Birk RasmussenThe principles and methods of electron spin resonance spectroscopy (ESR)Results and discussion: ESR spectroscopic study of parchmentConclusionReferencesDetermination of the molecular weight distribution in parchment collagen by steric exclusion chromatographyFrederique Juchauld and Claire ChahineIntroductionMaterials and methodsExperimentCorrelation between the two chromatographic methodsCorrelation with differential scanning calorimetry (DSC) resultsConclusionsReferencesSDS-PAGE and 2D-electrophoresisRene Larsen, Dorte V. Poulsen and Marie VestIntroductionExperimentalResults and discussionConclusionAcknowledgementsEndnotesRefere ncesAnalysis of collagen structure in parchment by small angle x-ray diffractionTimothy J. Wess and Kurt NielsenBackground to collagen structureX-ray diffractionSynchrotron radiationData analysis and parametersModel buildingPrincipal component analysisConclusionPyrolysis capillary gas chromatography (PY-CGC) of historical parchment samplesLeopold Puchinger, Dietmar Leichtfried and Herbert StachelbergerIntroductionMaterials and methodsPyrolysis capillary gas chromatography (PY-CGC)Discussion of the results obtained with PY-CGCDiscussion of the results from TEM and PY-CGC by comparison with other methodsConclusionsReferencesPalaeogenetics of parchmentJoachim BurgerIntroductionGenetic backgroundMethods (from Burger et al. 2000b)Results and discussionFrom which individual animal did this come? DNA profilingConclusionReferencesComplementary and comparative analysisThe use of complementary and comparative analysis in damage assessment of parchmentsRene Larsen, Dorte V. Poulsen, Marianne Odlyha, Kurt Nielsen, Jan Wouters, Leopold Puchinger, Peter Brimblecombe and Derek BowdenIntroductionExperimentalDeterioration characterized by shrinkage phenomenaThe impact of chemical deterioration on the hydrothermal stabilityChemical damage modelling by the prediction of T(S) from chemical dataPCA of thermomechanical, thermogravimetric and solid state NMR dataMacroscopic and microscopic properties vs. measurement dataConclusionsEpilogue: The problem of model building and correlation analysisReferences,

Contributors

Acknowledgements

Preface

René Larsen

Introduction

René Larsen

Parchment

Materials

Microsampling and microscopical assessment of parchment including microchemical analysis of binding media, dyes and ink

A new microsampling technique for parchment

Leopold Puchinger and herbert Stachelberger

Introduction

Description of the microdrilling instrument

Drill sizes and technique of needle sharpening

Evaluation of drill bits and holes left in the parchment - applications

Summary

References

Evaluation of old parchment collagen with the help of transmission electron microscopy (TEM)

Leopold Puchinger, Dietmar Leichtfried and Herbert Stachelberger

Introduction

Materials and methods

Discussion of the results obtained with TEM

Discussion of the results from TEM by comparison with other methods

Conclusions

References

Evaluation of methods for the microanalysis of materials added to parchment

Jan Wouters, Johan Claeys, Karijn Lamens and Marina Van Bos

Introduction

Historical sources for the composition of miniatures

Materials and methods

Results and discussion

Conclusion

Acknowledgements

References

Characterization of vegetable gums used as binding media in inks by gas chromatography and multivariable analysis

Pascale Richardin, Sylvette Bonnassies-Termes and Jean-Christophe Doré

Introduction

Experimental

Characterization by gas chromatography of neutral sugars and uronic acids

Analysis of vegetable gums

Application to metallogallic inks

Conclusion

Acknowledgements

References

Appendices

Sulphur inclusions within parchment and leather exposed to sulphur dioxide

Derek J. Bowden and Peter Brimblecombe

Introduction

Experimental

Results

Discussion

Conclusions

Acknowledgements

Endnotes

References

Thermophysical and thermochemical analysis of microsamples

The hydrothermal stability (shrinkage activity) of parchment measured by the Micro Hot Table Method (MHT)

Rene Larsen, Dorte V. Poulsen and Marie Vest

Introduction

Experimental

Samples

Results

Discussion

Conclusions

References

The thermal response of parchment and leather to relative humidity changes

Derek Bowden and Peter Brimblecombe

Introduction

Background

Experimental

Examples and results

Conclusions

Endnotes

References

Characterization of historic and unaged parchments using thermomechanical and thermogravimetric techniques

Marianne Odlyha, Neil Cohen, Gary Foster and Roberto Campana

Introduction to termomechanical and thermogravimetric techniques

Dynamic mechanical thermal analysis (DMTA): stress-strain measurements

DMTA: Measurement of viscoelastic properties

DMTA: Underwater heating creep measurements

Thermogravimetry analysis (TGA)

Overall conclusions from thermomechanical and Thermogravimetric measurements

Principal conponent analysis (PCA)

References

Chemical and structural characterization of collagen and palaeogenetics of parchment

Amino acid analysis of new and historical parchments

René Larsen, Dorte V. Poulsen, Marie Vest and Arne L. Jensen

Introduction

Experimental

Results

Discussion

Conclusion

References

13C and 15N solid state nuclear magnetic resonance (NMR) spectroscopy of modern and historic parchments

Marianne Odlyha, Neil Cohen, Gary Foster, Roberto Campana and Abil Aliev

Introduction

Experimental

Results (13C NMR spectra)

Results: 15N solid state NMR spectra

Conclusions

References

Study of the chemical breakdown of collagen and parchment by Raman spectroscopy

Thomas Garp, Kurt Nielsen, and Soghomon Boghosian

The principles and methods of Raman spectroscopy

FT-Raman spectroscopic studies of parchement

Conclusions

References

Detection of radicals in collagen and parchment produced by natural and artificial deterioration, electron spin resonance spectroscopy (ESR) and its implications for artificial ageing and test of conservation treatments

Daniella Bechmann Hansen, Kurt Nielsen and Søren Birk Rasmussen

The principles and methods of electron spin resonance spectroscopy (ESR)

Results and discussion: ESR spectroscopic study of parchment

Conclusion

References

Determination of the molecular weight distribution in parchment collagen by steric exclusion chromatography

Frédérique Juchauld and Claire Chahine

Introduction

Materials and methods

Experiment

Correlation between the two chromatographic methods

Correlation with differential scanning calorimetry (DSC) results

Conclusions

References

SDS-PAGE and 2D-electrophoresis

René Larsen, Dorte V. Poulsen and Marie Vest

Introduction

Experimental

Results and discussion

Conclusion

Acknowledgements

Endnotes

References

Analysis of collagen structure in parchment by small angle x-ray diffraction

Timothy J. Wess and Kurt Nielsen

Background to collagen structure

X-ray diffraction

Synchrotron radiation

Data analysis and parameters

Model building

Principal component analysis

Conclusion

Pyrolysis capillary gas chromatography (PY-CGC) of historical parchment samples

Leopold Puchinger, Dietmar Leichtfried and Herbert Stachelberger

Introduction

Materials and methods

Pyrolysis capillary gas chromatography (PY-CGC)

Discussion of the results obtained with PY-CGC

Discussion of the results from TEM and PY-CGC by comparison with other methods

Conclusions

References

Palaeogenetics of parchment

Joachim Burger

Introduction

Genetic background

Methods (from Burger et al. 2000b)

Results and discussion

From which individual animal did this come? DNA profiling

Conclusion

References

Complementary and comparative analysis

The use of complementary and comparative analysis in damage assessment of parchments

René Larsen, Dorte V. Poulsen, Marianne Odlyha, Kurt Nielsen, Jan Wouters, Leopold Puchinger, Peter Brimblecombe and Derek Bowden

Introduction

Experimental

Deterioration characterized by shrinkage phenomena

The impact of chemical deterioration on the hydrothermal stability

Chemical damage modelling by the prediction of T(S) from chemical data

PCA of thermomechanical, thermogravimetric and solid state NMR data

Macroscopic and microscopic properties vs. measurement data

Conclusions

Epilogue: The problem of model building and correlation analysis

References

• Edited by René Larsen