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Michele Derrick; Luiz Souza; Tanya Kieslich; Henry Florsheim; Dusan Stulik
Journal of the American Institute for Conservation, Vol. 33, No. 3. (Autumn - Winter, 1994), pp.
227-245.
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1. I N T R O D U C T I O N
Polyester resins were introduced in the 1940s.
Because of their transparency and ease of
preparation, they were soon used for the
encapsulation of natural history objects (Purves
and Martin 1950). Although it was later
discovered that the long-term
life of the
polyester was not appropriate for museum
objects (Meurgues 1982), polyester resins are
still commonly used by schools, scientists, and
hobbyists for embedding and casting many
objects. Polyester resin is also routinely used as
a medium for embedding multilayer paint cross
sections from art objects (Plesters 1956;
Wolbers and Landrey 1987; Tsang and
JAIC 33 (1994):22745
JAIC 33(1994):227--45
229
TABLE 1
propriate viscosity (Horie 1987). When combined with a methyl ethyl ketone peroxide
catalyst, a crystal clear, uniform, solid block is
produced that is readily polished and easily
microtomed. The resin cures overnight at
room temperature or in a few hours at slightly
elevated temperatures. It shrinks minimally
during curing at room temperature and slightly
more when cured with increased temperatures.
It is cheap, readily available, easily prepared,
and only moderately toxic. These many positive features give polyester resin several advantages over the other embedding resins on
the market (e.g., acrylics, and epoxies) and account for its popularity as an embedding
medium for paint cross sections.
W e the polyester resins typically are used
for paint cross sections in art conservation,
forensic scientists generally use epoxies, acrylics,
and cyanoacrylates. We found that the epoxies
tend to be yellow in color as well as too hard
and brittle to microtome sections at the thicknesses of 1-10 pm required for infixed
analyses. The acrylics were clear and colorless,
but they were very exothermic and shrank significantly upon curing. One acrylic embedding
JAIC 33 (1994):22745
JAIC 33(1994):227-45
3. EMBEDDING P A I N T C R O S S
S E C T I O N S W I T H POLYESTER
RESIN
3.1 PROCEDURE
T o embed a typical paint sample in polyester
media (brands noted in table I), six drops of
catalyst (methyl ethyl ketone ether) are mixed
thoroughly with 10 rnl of liquid polyester/
styrene resin. The transparent resin is initially
light blue in color. It turns yellow when the
catalyst is well mixed and quickly becomes
colorless as the reaction proceeds (Ward's
Natural Science 1990). Excess catalyst will
speed up the curing process but will also make
the final mount more brittle and dif3icult to
microtome. A mold is initially half-filled with
231
3.2 INFILTRATION
The penetration of the liquid embedding
resin into the interior of a paint sample can
occur when there are voids or open spaces in
JAIC 33 (1994):227-45
- p - A A . " , r r - - - - - -
- -
. .
------
_.,-_----.__,
Wax
ipoxies
Acrvlics
Break-awz
mold
Polyestf
m e rubber
.nold
Fig. 1. Example blocks of polyester, epoxy, acrylic, and wax embedding media for paint cross sections
corresponding to table 1. Break-away molds and small, flexible silicone rubber molds are shown.
JAIC 33(1994):227-45
&
-
JAIC 33 (1994):227-45
JAIC 33(1994):227-45
235
cb
Caroplastic
3996.00
3497.00
2998.00
2499.00
2000.00
1761.00
1522.00
1283.00
1044.00
805.00
Wavenumber (CM-1)
Fig. 4. Infiared spectrum of paint cross section sample (top) and Caroplastic brand polyester resin (bottom).
The spectnun for the paint sample contains absorption bands corresponding to the embedding resin (marked
with *). This spectrum shows that the embedding resin has soaked into the paint sample.
CAO42 embedded in
Caroplastic after 39 minutes
Caroplastic
Wavenumber (CM-1)
Fig. 7. Infked spectra of Caroplastic polyester resin (bottom) and paint cross section (top) for which the top
embedding layer of Caroplastic was poured over the sample 39 minutes after the catalyst was added to the resin
solution. Even though the embedding resin was extremely thick when it was placed on the top of the sample,
the resin still infiltrated the paint sample. This infiltration is shown by its infixed spectrum, which contains
absorption bands corresponding to the embedding resin (marked with *).
JAIC 33 (1994):227-45
JAIC 33(1994):227-45
sample bottom
sample top
Fig. 12. Steps used for encapsulating a cross section sample with a banier material inside a polyester
embedding resin
=
Fig. 13. Photomicrograph of embedded paint cross
section (Catas Altas sample CA039) that was barrier
coated with Rhoplex thickened with Cab-O-Sil
prior to embedding in polyester resin. The acrylic
layer prevented the infiltration of the resin, as
indicated by the opaque white appearance of the
ground layer. 37x
JAIC 33 (1994):227-45
TABLE 2
JAIC 33(1994):227-45
quired to shrink the material are not recommended for sample preparation; in a few attempts, the samples could not be prepared
without bubbles being trapped inside the plastic. The presence of bubbles keeps the sample
fiom being held uniformly and makes
microtoming difEcult.
The next-test used a SpUtter coater to coat
samples with greater than a 5-nm-thick layer of
gold. Several samples of two types (plaster and
paint facsimile with glue ground) were prepared
by this method. The results were inconsistent
within sample type; some were infiltrated by
the polyester, and some were not. It appeared
that the smoothness and lack of crevices in the
sample were important for success, since complete coating of all surfaces is necessary to keep
out the polyester. Additionally, carell handling of the sample after coating was required,
because, in some cases, a small portion of the
h g d e coating would attach to the forceps and
come off the sample. Figures 10 and 11 show
photomicrographs of an unstained and FITCstained paint cross section of a sputter-coated
sample that experienced resin infiltration.
Completely sealing samples in an aluminum
foil sandwich with crimped edges was also tried.
This method was extremely time-consuming
and resulted in an opaque, difticult-to-position
sample. Resin infiltration with this method was
inconsistent, and thus it is not recommended.
Several conservation treatments for papers
and painting relinings use nonpenetrating gellike solutions such as methyl cellulose (Baker
1984), acrylic dispersions thickened with
toluene (Keyser 1981; Mehra 1984), and acrylic
dispersions thickened with fimed silica (Byme
1984). Some of these methods were tested for
encapsulating the samples and found successfkl.
Many other thixotropic, quick-drymg solutions
may also work in the same manner. Of the gels
tested, the cellulose ether (Klucel G) film dissolved in the polyester resin. The toluenethickened acrylic (Rhoplex AC-33) was found
to retain toluene, resulting in a pliable film that
239
Caroplastlc
3996
3497
2998
tended to stretch during microtoming. However, when the toluene-thickened gel was allowed to dry thoroughly (a day or more), a
tough, clear film was formed over the sample.
The acrylic (Rhoplex AC-33) thickened with
fumed silica produced a tough 6lm around the
sample that dried quickly. Both of these last
two gels, when dry,kept the polyester resin
fiom infiltrating.
Mixtures of l , 3 , and 10 wt?? of Cab-O-Sil
(coated fbmed silica) in Rhoplex AC-33
produced semiclear filmsthat dried in less than
2 hours. Approximately 3 wt?? of Cab-O-Sil in
the acrylic emulsion was optimum; however,
since the mixture thickens with time, it is best
to judge it by its consistency. The consistency
should be very viscous, that is, greater than that
of honey but less than that of butter. It should
be gel-like but should flow enough to seal at
the points where the solution meets itself It is
better to have the consistency slightly too thin
than too thick. If the mixture is too viscous, it
2499
2000
1761
1522
Wavenumber (CM-1)
1283
1044
805
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4. DISCUSSION
Preventing infiltration of the embedding resin
into a sample will allow it to maintain its original
physical and optical characteristics. This may or
may not be desirable depending on the type of
sample and the type of analyses to be done.
In the case of a porous, powdery sample the
advantages of resin impregnation during embedding are that it will produce a solid, consolidated sample that may be highly polished to
a flat, smooth surface. These qualities are usell
for photomicrography, pigment identification,
and SEM/EDS analysis. If needed, the sample
should microtome well into intact thin sections.
However, interpretation of any staining or infiared analysis would be difficult due to the
presence of the resin within the sample. One
viable option would be to perform i d a r e d
analysis on particles fiom a corresponding nonembedded portion of the sample.
Conversely, ifthis sample were not infiltrated with resin, the resultant embedment
would contain a fragile and poorly cohesive
sample. Some particles may fall out of the
sample during polishing, and microtoming the
sample will be difficult and time consuming.
The advantage of an unadulterated sample is
that any analysis method used for examining the
sample is doing just that, examining the sample
and not any added component. Resin infiltration may particularly afFect the results of
photomicrography, fluorescence, staining,
colorirnetxy, or idared microspectroscopy.
The examination and detection of glazes and
other thin, organic layers may be very susceptible to resin infiltration.
5. C O N C L U S I O N S
In a comparison of several types of polymers,
polyester resins met the requirements for an
ideal embedding media for most paint cross
sections much better than did epoxies or acrylics.
Polyester resins set rapidly without heat, are
clear, polish readily, and microtome easily.
However, embedding resins, such as
polyester, can dissolve some waxes, colorants,
and resins. In addition, during the embedding
process, porous, low-binder paints are
penetrated by most types of polymer solutions,
including polyester. Infiltration can occur with
matte or porous paints that are often found in
wall paintings, polychrome sculptures, ethnographic objects, and with glue gessos. This infiltration is visually detected by examining the
cross section for poorly defined edges, darkening or discoloration, and blotchy stain results.
Infiltration may be codinned by the analysis of
the sample with infrared microspectroscopy,
where the presence of the embedding resin in
the sample will produce a spectrum containing
absorption bands characteristic of the resin.
It is important to recognize that infiltration
can and has occurred in embedded paint cross
sections. Infiltration has advantages and disadvantages, because it consolidates and supports
the sample but can also hinder the analysis of
the sample's components. Thus, potential infiltration should be considered when samples
are examined, and a decision should be made
whether it is necessary to prevent the infiltration based on the type of sample and the type of
analyses.
In the cases where embedding without infiltration is chosen as the best option, several
barrier methods have been tested for coating
the sample with materials before embedding the
sample in polyester resin. A method using
Rhoplex AC-33 thickened with fumed silica
worked best, forming a uniform coating around
the sample that, when dry, did not allow the
polyester resin to infiltrate into the sample.
Many other types of high viscosity or
thixotropic materials would probably work as
well for precoating the sample.
6. EXPERIMENTAL
6.1 SAMPLES
Five types of samples were embedded in this
study. The first type was a concentration series
consisting of known mixtures of glue and
gypsum to test the effects of binder
concentration (figs. 5, 6). The second set of
samples was obtained fiom a facsimile painting
that had a glue-calcium carbonate ground layer
with a glue content of 15 wt?/o. This set was
used to evaluate the various kinds of embedding
media shown in table 1. This set of samples
along with samples of plaster (no binder) also
were used to test all of the barrier methods
shown in table 2. The fourth set of samples
consisted of small portions obtained fiom a
larger sample (CA042) that had f d e n off a
polychrome sculpture from the church of Catas
Altas, Minas Gerais, Brazil (figs. 2, 3).
Quantitative analysis of the protein content of
the sculpture sample by gas chromatography
showed that it contained 12% by weight of glue
in gypsum (Schilling 1994). After the
acrylic-silica barrier layer was found to work on
the test samples, it was then tried on pomons of
another polychromy sample (CA039) from the
church. This last set of samples, shown in
figures 13 and 14, contain a gesso sottile layer
(analyzed glue content of 5%) on the bottom
and a gesso grosso layer in the middle (analyzed
JAIC 33 (1994):227-45
6.2 MICROTOMING
An R M C Model 7000 microtome configured with a glass knife was used to produce
5 pm thin sections of the embedded samples.
Tungsten knives may also be used to prepare
thin sections in this range; stainless knives usually are used to produce thicker sections (20 pm)
and diamond knives for thinner sections (1
pm), Glass knives are made by scoring and
breaking a 1 in. square of glass to give 2 triangular pieces, each with a sharp edge. This procedure produces a 45' angle on the blade. This
angle may be increased for cutting harder
materials and decreased for softer materials
(Malis and Steele 1990).
Small samples are easier to microtome.
Larger samples may be cut into a pie shape and
positioned in a mold so that the point is cut
first. An embedded sample should have all excess medium trimmed fibm the embedment,
leaving only a facet with a few mm of medium
outside of the sample at the cutting surface.
Too large a cutting surface can cause the section
to curl and the sample to debond from the
medium.
Orientation of the sample to the knife edge
can affect the quality of the section. In this
description, a multilayer sample is considered as
a series of parallel lines that can be placed either
vertically or horizontally in a rotatable vise of a
microtome with a horizontal knife edge. For
most samples, the initial cut is best made with
the sample rotated 10' from vertical with the
most important layer closest to the knife. Exact
vertical orientation of the layers can increase
section curling and particle loss, while direct
horizontal orientation can result in the compression of the sample. Depending on the sample
and how it behaves during cutting, the orientation may need to be changed. In all cases, the
sample and the knife should be fastened securely and checked often for tightness.
The optimum thickness of a sample for infrared transmission analysis is 1-10 pm (Derrick
et al. 1991). Sections over 15 ym can absorb
JAIC 33(1994):227-45
IR radiation too strongly. Cutting thick sections can also result in particle loss, chattering of
the knife, and damaged knife edges. Whenever
a problem occurs, it can ofien be solved by slicing thinner sections (1 pn) and then returning
to slice a thicker section (5-10 pm). AU cuts
should be smooth and slow, using a motorized
microtome, if available, set at speeds of 0.1-3.0
rnm/sec.
Vibrations, drafts, temperature, and humidity
can all adversely d e c t microtorning results, as
can variations due to lighting, hand temperature, and human breath. When problems
occur, all factors should be considered and
modified when possible.
As the section is being cut, it should be encouraged to cling to the knife. With a small,
stifTartist's brush (size 2 or 3) the initial cut
edge of the section can be held to the knife surface without touching the sample region. Static
charges should keep the section on the knife.
Afier the section is cut, it can also easily and
delicately be picked up fiom the glass surface
using the brush. For infrared analysis, our sections were taken directly from the microtome,
placed on a BaFz window, and transferred to
the sample stage of the inbred microspectrophotometer.
6.3 INFRARED
MICROSPECTROSCOPY
A Spectra-Tech IRpS organic microprobe
was used for the infrared analysis of the thin sections of each sample. It is equipped with a narrow-band, cryogenically cooled mercury cadmium telluride (MCT) detector. The spectra
are the sum of 200 scans collected fiom 4000800 cm-1 at a resolution of 4 cm-1. The IRpS
is continually purged with dry, CO2-fiee air.
Once microtomed, the thin section slices
were placed on a BaFz window and transferred
to the sample stage of the infiared microspectrophotometer for analysis. An incandescent light
is used to locate and focus on the sample. A
small rectangular region of the sample, typically
243
JAIC 33 (1994):227-45
SUPPLIERS
JAIC 33(1994):227-45
245
MICHELE R. DERRICK graduated &om Oklahoma State University in 1979 with an M.S. in
analytical chemistry. In 1983 she joined the scientific
program of the Getty Conservation Institute, where
she is currently an associate scientist. Her research involves the development of new methods for the characterization and identification of organic materials in
cultural objects primarily using &red spectroscopy
and pyrolysis gas chromatography. Address: Getty
Conservation Institute, 4503 Glencoe Ave., Marina
del Rey, Calif. 90292.
LUIZ A. C. SOUZA received his B.S. (1986) and
M.Sc. (1991) in chemistry fiom the Federal University of Minas Gerais. The experimental work for his
M.Sc. was done at the Institut Royal du Patrimoine
Artistique, Brussels (1987-88). Since 1989 he has
been teaching and researching at the CECOR Center for Conservation and Restoriation of Movable
Cultural Properties of the Federal University of
Minas Gerais, Bradl. He is currently a research fellow at the Getty C o n ~ e ~ a d oInstitute.
n
Address:
CECOR, Escola de Belas Artes, Universidade
Federal de h4inas Gerais, Av. Antonio Carlos, 6627,
Belo Horizonte 31270, MG, Brazil.
TANYA L. KIESLICH received her B.S. fiom
Loyola Maryrnount University in 1992 with a major
in chemistry and a minor in art history. As part of
her undergraduate research, she used i k e d
microspectroscopy for the analysis of paint samples.
She is currently attending the Courtauld Institute of
Art for a postgraduate diploma in the conservation of
easel paintings. Address: Courtauld Institute of Art,
Dept. of Conservation and Technology, Somerset
House, Strand, London WC2R ORN, England.
DUSAN C. STULIK graduated &om Charles
University in Prague, Czechoslovakia, with B.S. and
M.S. degrees in chemistry. He subsequently obtained a Ph.D. in physics &om the Czechoslovakia
Academy of Sciences. He is currently acting head of
the scientific program at the Getty Conservation Institute. His current research is in the application of
modem scientific methods in conservation science.
Address: same as for Denick.
Received for review November 1, 1993. Revised
manuscript received May 4,1994. Accepted for publicationJune 15, 1994.
JAIC 33 (1994):22745
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References
Furniture Finish Layer Identification by Infrared Linear Mapping Microspectroscopy
Michele R. Derrick; Dusan C. Stulik; James M. Landry; Steven P. Bouffard
Journal of the American Institute for Conservation, Vol. 31, No. 2. (Summer, 1992), pp. 225-236.
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