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TREATMENT OF PAINTINGS
Michael C. Duffy
ABSTRACT—A series of simple tests studied the properties of five acrylic emulsion
adhesives: Plextol B500, Rhoplex AC 33 and AC 234, and Lascaux 360 HV and 498
HV. Properties such as peel strength, yellowing, and solubility were investigated to
assess the practicality of these products' use in the treatment of paintings with regard
to their aging characteristics.
1 INTRODUCTION
This study focused on the practical reliability of five polymer dispersions used
frequently in paintings conservation: Plextol B500, Rhoplex AC 33 and AC 234, and
Lascaux 360 HV and 498 HV. These adhesives were chosen because they are readily
available to the conservator. Properties of peel strength (reversibility), color change,
and swelling of dried films (solubility) were examined. Both aged and unaged samples
were tested and examined for flexibility. Consideration of these data provided
information about the long-term stability of these products.
2 LITERATURE REVIEW
THE PRIMARY SOURCE FOR INFORMATION on acrylic polymers and their
properties remains Robert Feller's “Polymer Emulsions,” first published in 1966 and
included as an appendix in the pioneering On Picture Varnishes and Their
Solvents (1985). This study includes fundamental information on polymer emulsions,
such as manufacturing methods, drying phenomena, and film formation. Physical
properties such as minimum film forming temperature (MFT) and glass transition
temperature (Tg) are also noted for some acrylic copolymer emulsions. Feller's study
is essential reading before undertaking further research into acrylic dispersions.
Not until 1984 were comprehensive test results of these materials published in the
conservation literature. Howells et al. examined the aging properties of 14 different
dispersions and considered weight change, color change, solubility, tensile mechanical
properties, response to heat, and pH changes.6 They found that the most significant
changes occurred with thermal aging as opposed to natural, sunlight, and fluorescent
aging. DeWitte's study demonstrated that certain dispersion additives sometimes
influence the physical properties of a synthetic resin.7 These articles are useful
precedents because they begin to examine the long-term stability of these materials
being used by conservators today. In addition, Falvey8 and Barclay9 have published
case studies in which the application of acrylic dispersion adhesives has been useful in
treating difficult problems.
3 SAMPLE PREPARATION
EACH OF THE FIVE ACRYLIC DISPERSIONS were prepared as follows:
The undiluted adhesives were cast onto sheets of silicone release mylar using a doctor
knife. This tool spreads an even film of uniform thickness (0.015″). When dry, these
cast films could be peeled off for testing or left on the mylar carrier. The Plextol B500
had to be mixed with toluene (toluene 1:10 Plextol) to facilitate spreading; otherwise it
beaded up on the mylar surface (for consistency, all samples were prepared using
toluene “thickened” Plextol). The Plextol AC 33 and 489 HV dried down to a hard,
clear film overnight, while the AC 234 and 360 HV remained tacky and soft. Samples
not subjected to accelerated aging were kept under room conditions (approximately
68° F and 50% RH).
The adhesives were applied to sheets of polyester sailcloth as described in section 3.2
and allowed to dry for 48 hours under room conditions. Toluene was sprayed
repeatedly onto the adhesive surface to swell and reactivate the tack. Approximately
500 ml of toluene was required to reactivate five 9″ × 7″ samples. While the samples
were still tacky, a second piece of sailcloth was applied to the surface. The samples
were then placed under vacuum for one hour at 1″ Hg to simulate lining conditions.
After “lining” the samples were cut into 1″ × 7″ strips.
4 PROCEDURE
4.1 Aging of samples
A Scott CRE/500 peel strength tester was used to determine peel strengths for all
samples.13 The machine was equipped with interchangeable load cells of 5 or 500
pounds. Where possible the 5-pound load cell was used. Calibrating the machine with
a 500-gram weight made it possible to get an accurate estimate of the samples' peel
strengths. The weight was hung from the clamp, and a reading was recorded on the
same chart paper being used for the sample. All strengths were recorded in grams per
linear inch. To get a measurement, the loose ends of the strips were clamped into the
opposing jaws of the tester. Turning the tester on caused the clamps to move away
from each other and the sample to be peeled apart. A recording device was used to
chart the peel strengths so they could be graphically compared.
Samples of both aged and unaged cast films were cut into sections weighing
approximately 0.5 grams each. These were weighed into glass vials using an analytical
balance. Three solvents were tested for their effect on the adhesives: distilled water,
toluene, and isopropanol. About 5 ml of the chosen solvent was added to the vials and
left under room conditions for 24 hours. Excess solvent was decanted off, and the
samples were left to dry for another 48 hours in the fume hood. The samples were
weighed again. Percent swelling was calculated with the formula:15
5 RESULTS
AFTER MORE THAN 100 HOURS IN THE CHAMBER, the cast films showed
slight yellowing. The polyester fabric of the lining samples was yellowed as well, but
the adhesive sandwiched in between remained clear. Since light and thermal aging
were occurring simultaneously, it is hard to say which was the cause of yellowing. It
may be significant, however, that the adhesives exposed to light and heat did discolor
while those exposed to heat only did not. Lengthier exposure would have certainly
caused more significant differences in discoloration among the samples. No
measurable differences in flexibility could be discerned between the aged and unaged
samples. All were extremely flexible before and after aging took place.
Some significant trends emerge from the peel strength test data. Average values for the
peel strengths of each sample type were calculated from the Scott Tester charts (see
table 1). Representative charts from each sample type were chosen for evaluation.
Random high and low points were chosen, and an overall average value was attained.
Some peel tests gave uneven results, probably because of bubble inclusions in the
dried dispersion or unevenness in application that were not apparent during sample
preparation. The slightly ribbed texture of the sailcloth fabric was also a factor
contributing to variable adhesion. For practical considerations, peel strengths of under
100 grams were considered failures.
Differences in peel strengths after aging were most apparent with the Rhoplex films.
Aged samples of both wet laminate and reactivated samples had higher peel strengths
than unaged samples. This result may indicate a degree of polymer cross-linking that
occurred after exposure to heat and light. Moreover, the excessive heat of the chamber,
sometimes exceeding the Tg of the samples, may have caused a more tenacious bond.
The solvent reactivated samples of AC 33 failed across the board, although the aged
samples had slightly higher peel strengths. When used as a wet laminate, the AC 33
held more tenaciously, giving peel strengths of about 450 grams in the unaged samples
and about 1,545 grams in the aged samples. AC 234 had slightly higher peel strengths
in the wet laminate samples but failed in the reactivated category. AC 234 wet
laminate samples had much higher (+1020) values than their unaged counterparts.
Aging also caused higher peel strengths in the 498 HV samples. There was about a
1,000 g higher average peel strength for the aged wet samples for this adhesive.
Reactivated unaged samples came close to failing, while the aged reactivated samples
had slightly higher peel strengths (about +100 g). This adhesive performed much like
the Rhoplexes in peel tests.
The most consistent peel strength values were given by the 360 HV, with very high
peel strengths in all categories. There was very little change in values between aged
and unaged samples or even between wet and reactivated samples. This result may be
explained by the fact that the 360 HV remains tacky when dry and bonds readily to
most surfaces. Even the reactivated lining samples formed tenacious bonds with values
two to four times higher than those of the other adhesives.
Plextol also gave similar values in the aged and unaged categories, differing only by
300 g or so. The reactivated samples, however, failed in both the aged and unaged
trials. Of the five adhesives, the Plextol B500 performed the most consistently
between aged and unaged samples without the high bonding of the 360 HV.
To compare changes in color, the L*a*b* system of the Minolta Chroma Meter was
used. Chroma (b*) values were chosen for statistical analysis because increases in this
number correspond to an increase in yellowing of the sample. Six measurements were
taken, and their averages and standard deviations were calculated (see table 2).
Confidence levels were established for comparison of selected groups of data. The
degree of freedom equaled 10 for the two sets of six samples.
Of the five samples tested, Plextol had the most discoloration, with a difference of
3.04 units between aged and unaged samples. Lascaux 360 HV had the least
discoloration, with only a 1.11 difference in Chroma values. Comparison of these two
values using the T-Test established that they differed in discoloration significantly,
measurable at the 99.9% confidence level. Other discoloration values could not be
distinguished from each other at that level of confidence. Comparison of the Rhoplex
AC 33 and AC 234 values yielded a less than 50% confidence level. It should be noted
that although these are measurable differences, the degree of yellowing appeared to
the eye to be about the same for all adhesive samples—the Plextol was not noticeably
more discolored than the others. Aged and unaged samples could easily be
distinguished, however.
With the addition of water the film samples swelled slightly, turning white and
opaque. Swelling in the unaged samples of 360 HV and 498 HV was significantly
greater (16% and 10% respectively) than for the aged samples (0.4% and 0.6%),
suggesting that aged films are much less permeable to moisture than young films (see
table 3). Swelling with water alone would not reverse a polymer film.
Swelling Values
Percent swelling of the films in isopropanol was also very small. The samples became
semi-opaque with the addition of this solvent. The greatest amount of swelling
occurred in the aged and unaged 360 HV samples at around 7.5%. Unaged 498 HV
swelled to about 5%, while values for all the others were under 3%. What
was surprising was that, on average, greater swelling occurred in distilled water than
in isopropanol.
The addition of toluene to the films caused them to swell completely and dissolve into
a clear gel. For the most part, unaged samples swelled at a higher percentage than aged
films. The least swelling occurred in Plextol and AC 33 films, while swelling of the
AC 234, 360 HV, and 498 HV was especially high—in the 30%–50% range.
6 DISCUSSION
Of the five adhesives tested, the Plextol B500 appears to be the most resistant to peel
strength changes over time. Unfortunately, it also sustained the most discoloration of
any of the adhesives. Since the adhesive would be hidden from light in a lining,
yellowing may not be a factor under consideration. Accepting a material's negative
properties to gain the advantage of its positive properties is a compromise frequently
made in conservation. Certainly the discoloration of any of these materials is
inevitable and must be considered vis-ll
7 CONCLUSIONS
WITH THESE RESULTS, it appears that Plextol B500 or Lascaux 498 HV would be
the most suitable for lining paintings where high adhesive strength is required. Where
a lighter bond is needed—perhaps for paper objects or fine fabrics such as silks—the
Rhoplexes would be more appropriate. The very high peel strength of the 360 HV
would seem to limit its application alone, but it should prove useful in combination
with 498 HV to improve tack. Of the solvents tested, toluene was the best choice for
swelling these films.
ACKNOWLEDGEMENTS
NOTES
4. J. Volkmer et al. “An Examination of Lining Materials and Methods for Special
Problems in Painting Conservation,” AIC Bulletin 15, no., 2 (1975): 103–5.
5. A. Ketnath, “Acrylic Resins for the Conservation of Paintings,” Meddeleser an
Konservering 2, nos. 7, 8 (1976): 223–35.
10. The sailcloth was chosen because it is nonabsorbent and would not react with the
adhesives being tested. It is a woven fabric that has been cross-linked with melamine
formaldehyde for high stiffness.
11. Samuel Hudson and Lowell Perkins were of great assistance in modifying the
aging chamber, which was originally designed by Marion Mecklenberg.
13. The Scott Tester was made available by Dr. J. Weaver, chairman of the University
of Delaware Textiles Department.
15. S. Blackshaw and S. Ward, “Simple Materials for Use in Conservation,” In Resins
in Conservation (Edinburgh: SSCR, 1983). 2-1 to 2–15.
ADDITIONAL LITERATURE
Feller, R. L., N.Stolow and E.Jones. On Picture Varnishes and Their Solvents. revised
and enlarged. Washington, D.C.: National Gallery of Art, 1985.
Phenix, A., and G.Hedley. “Lining without Heat or Moisture.” In ICOM Preprints,
84.2.38ff. Copenhagen, 1984.
Snedecor, G.Statistical Methods. Ames, Iowa: Iowa State University Press, 1967.
Wake, W.Adhesion and the Formulation of Adhesives, New York: Applied Science
Publishers, 1976.