Maney Publishing

A Study of Acrylic Dispersions Used in the Treatment of Paintings

Author(s): Michael C. Duffy
Source: Journal of the American Institute for Conservation, Vol. 28, No. 2 (Autumn, 1989),
pp. 67-77
Published by: Maney Publishing on behalf of The American Institute for Conservation of Historic &
Artistic Works
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 A STUDY OF ACRYLIC DISPERSIONS USED IN THE
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
ACRYLICAND OTHERPOLYMERDISPERSIONShave been used as adhesives and in
paint media for more than 20 years. These synthetic polymers have found sporadic
use in the conservation field as well, specifically for consolidating fragile materials
and lining paintings. Properties such as permanence, stability, and reversibility,
important to the conservator, are not always important in industry; yet often these
materials have been adapted for use in conservation without extensive testing.
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 infor-
mation about the long-term stability of these products.
In a recent paintings conservation refresher course sponsored by the FAIC, these
materials were demonstrated to have advantages in their low toxicity, ease of short-
term reversibility, and compatibility with other materials. Disadvantages included
the risk of moisture reactivity when used as a wet laminate, some application difficul-
ties with large fabrics, changing of product formulation without notice, and, most
important, the lack of comparative testing.'

2. LITERATURE REVIEW
THE PRIMARYSOURCE FOR INFORMATION on acrylic polymers and their properties
remains Robert Feller's "PolymerEmulsions," 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 manufactur-

* Solomon R. Guggenheim Museum, 1071 Fifth Avenue, New York, N.Y. 10128
This research was carried out when the author was at the H. F. duPont
Winterthur Museum, Winterthur, Del.

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68 Michael C. Duffy

ing 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.
A review of recent conservation literature in AATA revealed the first mention of
polymer dispersions used as lining adhesives in an article by Mehra published in
1972.2 Mehra's study on the use of Plextol B500 as a lining adhesive included data
on peel strength and sheer strength. In articles published in 1974 and 1975 Mehra
described the use of Plextol B500 in conjunction with a low pressure cold-lining table
he had developed.3 Other practical applications of polymer dispersion adhesives
were addressed by Volkmer et al.4 Accelerated aging of acrylic dispersion Plextol
D360 was done in 1976 by Ketnath, but apparently no test results were reported.5
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 mechani-
cal properties, response to heat, and pH changes.6 They found that the most sig-
nificant 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.
There is much useful information published outside the conservation literature.
Excellent information on polymer dispersions can be obtained from Martens' Emul-
sion and Water-Soluble Paints and Coatings. For information on adhesives and
adhesive theory, Wake's Adhesion and the Formulation of Adhesives and Shield's
Adhesives Handbook are indispensable. The most current information on advance-
ments in industry can be found in journals such as Colloid and Polymer Science.

3. SAMPLE PREPARATION
EACH OF THE FIVEACRYLICDISPERSIONSwere prepared as follows:

3.1 Cast Films

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 condi-
tions (approximately 68' F and 50% RH).

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 A Study of Acrylic Dispersions Used in the 69
Treatment of Paintings

3.2 Wet Laminate Lining Mockups

The five adhesives were applied onto 9" x 7" pieces of polyester sailcloth'0 fabric
using a squeegee to achieve a film of uniform thickness (approximately 1/16"). Pieces
of the same size polyester sailcloth were placed in contact with these samples to
simulate a wet laminate lining. These samples were then placed on the vacuum table
in a mylar envelope at 1" Hg pressure for one hour to assure even adhesion. The
mockups were allowed to air dry under room conditions over a 48-hour period and
then cut into 1"x 7" strips in preparation for peel strength testing.

3.3 Reactivated Lining Mockups

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" x 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"x 7" strips.

4. PROCEDURE
4.1 Aging of samples
HALF OF THE PREPARED LININGSAMPLES-both wet and reactivated-plus the
cast films were placed into an aging chamber.11 Both thermal and light aging
occurred during the samples' exposure. The chamber was a Plexiglas box fitted with
a General Electric 275 Watt Sunlamp Bulb regulated by a rheostat. A small fan kept
air circulating in the chamber, and a Heathkit Relative Humidity Indicator monitored
humidity inside the chamber.12 An attempt was made to regulate the humidity inside
the chamber with a saturated solution of sodium iodide salts. Even so, the humidity
fluctuated significantly, mostly in the 36%-400/%range. Temperature averaged 46'-
58' C (115'-136' F). Light falling on the tray holding the samples was about 500
footcandles. Over a one-month period the samples received 124.25 hours of ex-
posure, equaling approximately 62,125 footcandle-hours. Even in this relatively
short period the samples showed noticeable yellowing in both the clear films and the
lining mockups. Control samples were kept under room conditions while the others
were aging.

4.2 Peel Strength Testing (ASTMD-903-49)

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

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70 Michael C. Duffy

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.

4.3 Measuring Change in Color

Yellowing was measured using a Minolta Chroma Meter CR-100.14 Data were
collected from the aged and unaged samples of each type of adhesive and compared
after statistical analysis.

4.4 Swelling of Cast Films

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 analyti-
cal 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
W2 - W1 x 100
Wi
Wi = weight of the sample before addition of solvent
W2 = weight of the sample after decanting solvent and drying.

5. RESULTS
5.1 Aging 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.

5.2 Peel Strengths

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 evalua-
tion. 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

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 A Study of Acrylic Dispersions Used in the 71
Treatment of Paintings

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 be-
tween aged and unaged samples without the high bonding of the 360 HV.

5.3 Color Change

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 dis-
coloration, 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 ap-
peared to the eye to be about the same for all adhesive samples--the Plextol was not

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72 Michael C.
Duffy

Table 1
Peel Strength Values
(in grams/linear inches)
Plextol B500 Aged Wet 2113
React 198*
Unaged Wet 2450
React 170*
Rhoplex AC 33 Aged Wet 1545
React 153*
Unaged Wet 450.
React less than 100
RhoplexAC 234 Aged Wet 1625
React 340
Unaged Wet 605
React 113*
Lascaux 360 HV Aged Wet 4675
React 4975
Unaged Wet 5513
React 4568
Lascaux 498 HV Aged Wet 1508
React 283
Unaged Wet 540
React 178
* with values less than 100 (failure)

noticeably more discolored than the others. Aged and unaged samples could easily
be distinguished, however.

5.4 Percent Swelling

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.
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 swell-
ing 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

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 A Study of Acrylic Dispersions Used in the 73
Treatment of Paintings

Table 2
Chroma (b*)Values
(in L*a*b*units)
Plextol Aged 4.13 s.d.= 0.75
Unaged 1.0 0.14
Difference 3.04
Rhoplex AC 33 Aged 2.94 0.34
Unaged 1.30 0.08
Difference 1.64
Rhoplex AC 234 Aged 2.52 0.14
Unaged 0.78 0.11
Difference 1.74
Lascaux 360 HV Aged 2.32 0.28
Unaged 121 0.05
Difference 1.11
Lascaux 498 HV Aged 3.07 0.12
Unaged 1.11 0.04
Difference 1.96
T-Tests tcalc ConfidenceLevel
Plextol vs. 360 HV 5.07 99.9%
Plextol vs. AC 33 3.50 99.5%
498 HV vs. AC 234 1.83 90%
AC 234 vs. AC 33 0.50 less than 50%

Table 3
Swelling Values
(in percent-byweight)
Water Isopropanol Toluene
Plextol Aged 2.6% 2.3% 9.3%
Unaged 1.8 2.0 12.1
Rhoplex AC 33 Aged 3.1 0.8 6.6
Unaged 4.4 2.7 14.5
Rhoplex AC 234 Aged 3.9 1.0 30.3
Unaged 2.5 1.2 40.8
Lascaux 360 HV Aged 0.4 7.5 46.3
Unaged 16.1 7.6 52.5
Lascaux 498 HV Aged 0.6 2.6 45.6
Unaged 10.6 4.8 43.8

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74 Michael C. Duffy

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
MATERIALSUSED IN CONSERVATIONshould be stable over an extended period of
time. This does not seem to be the case for the polymer dispersions tested. Dis-
coloration (the formation of conjugated double bonds) occurred in measurable
amounts in all samples after a relatively short exposure to aging conditions. Changes
in peel strengths related to the aging of films indicate increased difficulty of revers-
ibility in the Rhoplexes and 498 HV. While the precise peel strength desirable would
depend on a number of factors not examined here extreme highs and lows were
judged to be undesirable. The extremely high peel strength value for HV 360 makes
its reversibility a harsh undertaking for a fragile art object. Conversely, reactivated
samples with low peel strengths do not have the adhesive strength to keep a fabric
securely adhered to another and so threaten delamination. Changes in technique of
reactivating the adhesive may be required if it is to be used in the lining procedure.
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 discolora-
tion 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
13mbined adhesives could be tested to determine if a mixture of two adhesives
would yield more favorable properties than either one used alone. Comparison of peel
strength vs. sheer strength values would further enhance understanding of these
materials. There are many avenues for further study of the use of these materials in
the conservation field.

7. CONCLUSIONS
WITHTHESE 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.
Unfortunately, the long-term reliability of these materials appears questionable,
considering the short aging exposure, resulting discoloration, and increased peel
strengths. Further testing with longer-term exposure and interim testing are war-
ranted to determine if an actual trend toward irreversibility with aging exists. In the

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 A Study of Acrylic Dispersions Used in the 75
Treatment of Paintings

meantime, the results put forth here should be considered when these adhesives are
applied to works of art.

ACKNOWLEDGMENTS
THANKSARE DUE TO LOWELLPERKINSAND JANET SCHRENKof the Winterthur
Museum Program in Art Conservation at the University of Delaware, who served as
advisers on this research project. At the University of Delaware, Jeremiah Weaver
generously provided assistance in gathering and interpreting peel strength data.
Samuel Hudson from DuPont's textile division also provided assistance and en-
couragement for the project.

NOTES
1. See FAIC, Williamstown Painting Refresher Notes (Washington, D.C.: FAIC,
1983).
2. V. R. Mehra. "Comparative Study of Conventional Relining Methods and
Materials and Research Towards Their Improvement." Interim Report ICOMCommittee
for Conservation, 3rd Triennial Meeting (Madrid, 1972). 21/72/4. 28pp.
3. V.R. Mehra, "Nap-bond and Cold Lining on a Low Pressure Table," Maltechnik
Restauro 81, no 2 (1974): 87-95; and "Further Developments in Cold-Lining (Nap-
Bond System) In ICOMCommitteefor Conservation (Venice, 1975), 75/11/5, 1-26.
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.
6. R. Howells et al., "Polymer Dispersions Artificially Aged, " in Adhesives and
Consolidants, London: IIC, 1984, 36-43.
7. E. DeWitte et al., "Influence of the Modification of Dispersions on Film Proper-
ties," In Adhesives and Consolidants, London: IIC, 1984, 32-35.
8. D. Falvey, "Practical Cold Lining Developments, " ICOMCommitteefor Conserva-
tion, 7th Triennial Meeting (Copenhagen, 1984) 84/2/12-15 ff.
9. M. H. Barclay, 'The Final Report on a Stabilizing Treatment for an Unusually
Large and Heavy Contemporary Oil Painting on Canvas." ICOMCommitteefor Conser-
vation, 7th Triennial Meeting (Copenhagen, 1984). 84/2/3.ff.
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.
S11.Samuel Hudson and Lowell Perkins were of great assistance in modifying the
aging chamber, which was originally designed by Marion Mecklenberg.
12. Heath Co., Benton Harbor, Mich. 49022.
13. The Scott Tester was made available by Dr. J. Weaver, chairman of the Univer-
sity of Delaware Textiles Department.

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76 Michael C. Duffy

14. Minolta Corporation, Ramsay, N.J. 07446.

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
Berger, G. 'The Procedure of Developing an Adhesive for Paintings: The Impor-
tance of Valid Tests," In Adhesives and Consolidants, 13-17. Paris: IIC 1984.
- . 'Testing Adhesives for the Consolidation of Paintings." Studies in Conserva-
tion 17 (1972): 173-194.
Bjarnhof, M. "Removal of Damp Blotches by the Aid of a Low Pressure Table," In
ICOMPreprints, 84.2.10ff. Copenhagen, 1984.
Boissonnas, P., and W. Percival-Prescott. "Some Alternatives to Lining," ICOM
Committeefor Conservation, 7th Triennial Meeting. 84/2/35-44. Copenhagen, 1984.
Bradley, S. "Strength Testing of Adhesives and Consolidants for Conservation
Purposes," In Adhesives and Consolidants, 22-25. London: IIC, 1984.
Crafts Council. Adhesives and Coatings. London: Crafts Council, 1983.
Down, J. "Adhesive Testing at the Canadian Conservation Institute" In Adhesives
and Consolidants, 18-21. Paris: IIC, 1984.
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.
Martens, C.R. Emulsion and Water-soluble Paints and Coatings, Rheinhold Publish-
ing Corp. 1964.
Phenix, A., and G. Hedley. "Liningwithout Heat or Moisture." In ICOMPreprints,
84.2.38ff. Copenhagen, 1984.
Sander, I. "The Use of Synthetic Resins in Picture Conservation," In Resins in
Conservation, Edinburgh: SSCR, 1983.
Sheilds, J. Adhesives Handbook. Cleveland: CRC Press, c. 1970.
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.

SUPPLIERS
Plextol B500............................. Roehm GmbH
Postfach 4242
61 Darmstadt
West Germany

Rhoplex AC 33 ...................... Roehm & Haas

Rhoplex AC 234 ...................... Independence Mall West
Philadelphia, Pa. 19105
USA

JAIC 28 (1989): 67-77

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 A Study of Acrylic Dispersions Used in the 77
Treatment of Paintings

Lascaux 360 HV........................ Lascaux Farbenfabrik

Lascaux 498 HV....................... Department Restauro
CH-8306 Bruetisellen
Switzerland

Sailcloth................................. Bainbridge-Aquabatten
252 Revere Street
Canton, MA 02021

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