Case study Physicochemical characterization

Case study Physicochemical characterization

Case Study: Physicochemical characterization
of two 19th Century Portuguese Carte-de-Visite
by non-destructive techniques
M . P e r e s 1, L . D i a s 2, J . M i r ã o 2,3, T . F e r r e i r a 2,4, L .
C a r v a l h o 5, F . C o s t a 1, E . J a r d i m 6
1C
entro de Ciências Moleculares e Materiais, Universidade de Lisboa
2L
aboratório HERCULES - Herança Cultural, Estudos e
Salvaguarda, Universidade de Évora
3C
entro de Geofísica de Évora, Universidade de Évora
4C
entro de Química de Évora, Universidade de Évora
5C
entro Física Atómica, Universidade de Lisboa
6C
entro de Filosofia das Ciências, Universidade de Lisboa
[email protected]
2nd International Workshop on Physical and Chemical Analytical Techniques in Cultural Heritage
Lisbon, June 2012
SCIENTIFIC PHOTOGRAPHY:
STUDY OF INSTRUMENTATION AND CHEMICAL-PHYSICAL
PROCESSES DURING THE PERIOD
19TH- EARLY 20TH CENTURIES
2
R E S E A R C H P R O J E C T: P T D C / H I S - H C T/ 1 0 2 4 9 7 / 2 0 0 8
F I N A N C E D BY
3
4
MEMBERS
•
Fernanda Madalena Abreu Costa
•
Maria Estela de Freitas Vera - Cruz Jardim
•
Isabel Marília Viana e Peres
•
Marie Sophie Corcy
•
Pedro Miguel Barcia Ré
•
Rui Jorge Lourenço Santos Agostinho
•
Sara Raquel Dias de Sousa Carvalho
•
António Maria Reis Pereira
5
INTRODUCTION
 Identification of 19th century photographic prints
 Visual and microscopic methods of identification
 Identification of photographs using non contact
and non destructive methods
 Qualitative and quantitative XRF analysis of
photographs
 Scanning Electron Microscopy coupled with a
Energy Dispersion Spectrometry (SEM-EDS)
 Reflectance Fourier-Transform Infrared
Spectroscopy
19 th Century Portuguese Carte-de-Visite
6
Lady portrait (A. Solas)
Man portrait (A. Solas)
7
EARLY PHOTOGRAPHIC
Identification of primary
visual
clues : name
PROCESS
IDENTIFICATION
METHODOLOGY
of photographer, date, exhibition
or
photographic competition labels, logos, etc.
Date: c. 1896
Identification of secondary visual clues:
surface topography; tonality and colour
of the image layer; presence or absence
of fading or deterioration.
(A. Solas, c. 1896)
Glossy surface; brown tonality; no fading and
some deterioration
8
IDENTIFICATION OF 19TH
CENTURY PHOTOGRAPHIC
PRINTS
POSSIBLE STRUCTURE
Protective layer
Binder layer
(image+ toning)
Baryta layer
Paper support
Card
(A. Solas; c.a. 1896)
9
Classification (Reilly; 1986)
One layer
(no binder layer and
no baryta layer)
Two Layers
(no baryta layer)
Three layers
- Salted paper
- Cyanotype
- Platinotype
- Albumen print
- Carbon print
- Gelatin silver (POP)
- Collodion (POP)
- Gelatin silver (DOP)
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MICROSCOPIC
EXAMINATION OF
PHOTOGRAPHS
Stereoscopic Zoom Microscope
NIKON SMZ1500
• Magnification:10x
and 70x
• Illumination: 45º
• Exposure and Gain:
constants for each
magnification
C.C.M.M., Chemistry and Biochemistry Department,
Faculty of Sciences, University of Lisbon
(M. Peres, 2011)
11
MICROSCOPIC ANALYSIS
Mag. 10x (200ms, 1,2x)
Protective layer hide
paper fibers
Mag. 70x (600ms, 1,4x)
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QUANTITATIVE X-RAY FLUORESCENCE
SPECTROSCOPY (XRF)
EDXRF Spectrometer
• X-ray tube (PW 1140; 100 kV, 80 mA)
equipped with a changeable
secondary target, normally made off
molybdenum
• Si (Li) detector, with a 30 mm2 active
area and 8 µm beryllium window
• Energy resolution 135 eV at 5.9 keV
and the acquisition system is a
Nucleus PCA card
• Commercial pulse processor (Oxford).
• The X-ray generator was operated at
50 kV and 20 mA and a typical
acquisition time of 1000 s was used
Centro de Física Atómica, U.L.
(M. Peres 2011)
QUALITATIVE X-RAY FLUORESCENCE SPECTROSCOPY (XRF)
13
Pb
Lβ 1
Pb
Lα1
Pb
L γ1
Pb
L1
S Kα1
Ba
Ba Kβ1
Kα2
Ba
Lβ2,15
Pb
η
Sr
Kα1
Ba
Lγ1 Mn
Kβ1
Ni
Kα2
- No conclusive analysis regarding silver existence
- Significant amount of lead
- Possible presence of baryta layer
Scanning Electron Microscopy coupled with Energy
Dispersive Spectrometry (SEM-EDS)
14
The surface morphology and
homogeneity of uncoated samples were
analysed in a HITACHI S-3700N variable
pressure Scanning Electron Microscope
(SEM-EDS) coupled with a Bruker X-Ray
Energy Dispersive Spectrometer used for
elemental composition estimation.
Acceleration voltage of 20.0 kV and
variable pressure of 50 Pa were used for
chemical analysis.
Backscattered electron imaging mode
was used.
Laboratório HERCULES, Un. Évora
(L. Dias, J. Mirão, T. Ferreira, 2011)
15
SEM-EDS ANALYSIS
• Variable pressure chamber (50 Pa)
• A 20 cm width chamber allows the analysis of
the entire photograph avoiding microsampling
Laboratório HERCULES, Un. Évora
(L. Dias, J. Mirão, T. Ferreira, 2011)
P5
P1
P3
P4
P2
P7
P6
SEM-EDS ANALYSIS
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-Evidence of silver (no gold detected)
-The significant amount of lead is confirmed and points out an enamelled paper
-Overall presence of barium indicates a baryta layer
Fourier-Transform Infrared Spectroscopy
17
• Fourier Transform Infrared Spectrometer
ALPHA FTIR da BRUCKER
OPTIKS , portable spectrometer
• ALPHA model of Brücker with a
reflectance module A241/DV
QuickSnapTM and a video camera
• 64 scans with 4 cm-1 resolution
• Diameter of analysis: 6 mm
• The spectra were obtained in the
reflectance mode and converted to
absorvance mode by the Kramers-Kronig
algorithm.
Laboratório HERCULES, Un. Évora
Fourier-Transform
Infrared Spectroscopy
Comparative spectra analysis of A. Solas
sample (G1) and mate collodion test sample
(E2)
Prova G1
Prova E2 (colódio mate)
% T
18
2853
2922
1287
1643
3500
3000
2500
2000
1500
1004 856
1000
500
Nº de onda / cm-1
The IR spectrum comparison was done using the cellulose
nitrate spectrum in transmittance from Getty Conservation
Institute (DERRICK et al 1999).
MULTI-TECHNIQUE NON-DESTRUCTIVE APPROACH
19
No gold
Collodion
Silver
process
c. 1896
Baryta
layer
ENNAMELED
PAPER
Lead
Woodbury (1896)
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FINAL NOTES
• The microscopic essays using Reilly’s flowchart allowed us to do a first
characterization of the analysed photographic prints.
• Elemental analysis by non-invasive XRF and SEM-EDS provided additional
information about photographic prints (presence of baryta layer, toning with
gold, the presence of sulfur as a degradation agent) and knowledge about
the surface morphology and homogeneity of the prints.
• Reflectance Fourier-Transform Infrared Spectroscopy allowed the
identification of a protein material as well as the chemical nature of the
protective material layer.
• The use of multi-technique non-destructive approach provided information
about the stratigraphic structure of the photographic prints and also allowed
the identification of the major elements present in the samples.
On the overall, the analyses revealed key information about the deterioration
status of the photographic prints that can be critical to its preservation and
restoration, being also useful on the identification of fakes or reproductions
References
21
 CATTANEO, B., CHELAZZI, D., GIORGI, R., SERENA, T., MERLO; C., BAGLIONO, P. (2008), Physico-
chemical characterization and conservation issues of photographs dated between 1890 and
1910, Journal of Cultural Heritage, 9, pp. 277-284.
 ENYEART, J., ANDERSON, A., PERRON. S., ROLLINS, D., & FERNANDO, Q. (1983). Non-destructive
Elemental Analysis of Photographic Paper and Emulsions
Spectroscopy, History of Photography, Vol. 7, Nº. 2, pp. 99 – 113.
by
X-ray
Florescence
 RICCI, C. et al (2007), ATR-FTIR imaging of albumen photographic prints, Journal of Cultural
Heritage, 8: 387-395.
 STULIK, D. & KAPLAN, A. (2010), An example of complex composite materials and processes:
Photography in ARTIOLI, G. (coord), Scientific Methods and Cultural Heritage: An Introduction to
the
Application
of
Materials
Science
to
Archaeometry
and
Conservation
Science, Oxford, University Press, pp. 419-433.
 WOODBURY, W. (1896). Enamel paper. In The Encyclopaedic Dictionary of Photography. W.
Woodbury. New York, The Scovill & Adams Company of New York, p. 192.
22
Acknowledgements:
Acknowledgements
• FCT- Fundação para a Ciência e Tecnologia
• Ministério da Educação de Portugal
• Anabela Boavida, C.C.M.M, Fac. de Ciências da Un. de
Lisboa
• José Carlos Frade, Laboratório de Conservação e
Restauro José de Figueiredo, Instituto dos Museus e da
Conservação.
• Nuno
Borges
de
Photography, Braga
Araújo,
Historian
of