216 

A Preliminary Evaluation of the Surfaces

of Acrylic Emulsion Paint Films and the
Effects of Wet-Cleaning Treatment by
Atomic Force Microscopy (AFM)
Elli Kampasakali, Bronwyn Ormsby,  Antonino Cosentino, Costanza Miliani and
Tom Learner

The surfaces of acrylic emulsion (dispersion) paint films were investigated by atomic force microscopy (AFM), with supporting
chemical information provided via infrared spectroscopy.The morphological and chemical features of the surfaces of a series of
recently cast reference paint films were explored, including characterization of changes induced by exposure to water and mineral
spirits. A portable in situ AFM system was also used to document the surfaces of acrylic emulsion paintings in Tate’s collection.
The complete and partial removal of migrated surfactant was successfully imaged alongside features arising from mechanical action.
Differences in paint surfaces and migrated surfactant layers were observed in relation to pigment type, paint brand and exposure to
accelerated ageing, in addition to applied wet surface cleaning treatments.The findings contribute to further understanding of the
subtle changes occurring at acrylic emulsion paint film surfaces and are relevant to current debates on the removal/disturbance of
original surface surfactant from these films through conservation treatment.

INTRODUCTION
The potential for changes to the bulk film and surface
properties of acrylic emulsion paint films resulting from
surface cleaning treatments is of natural concern to
conservators [1]. Recent research has demonstrated that
use of aqueous and other polar solvent-based surface
cleaning treatments risk the at least partial removal of
surfactant from the surface of emulsion films [2–5] and
the extraction of water-soluble materials from bulk
paint films with longer exposures [5, 6]. Polyethoxylate
(PEO)-type non-ionic surfactants such as the Triton®
series, incorporated into polymer latex and emulsion
paint formulations as emulsifiers and dispersing agents
[7], have been identified within and on the surface of
acrylic emulsion paint films and painting surfaces [3,
4, 6, 8-11]. Other water-soluble components, such as
oligomers, wetting agents, de-foamers and salts may also
be affected by such cleaning agents.
PEO-based surfactants tend to exude to the surface
as small rounded crystals or patches, and/or form
Received August 2009
coherent thin films across paint surfaces [2, 4, 8]. While
the removal of surface surfactant has not proven to be
particularly detrimental to bulk film physical properties
[2, 12], the presence of these materials influences other
physical properties such as surface gloss, soiling and
resoiling rates, surface roughness [5], paint swelling,
pigment removal during cleaning [13], as well as water
penetration and transport [14]. Factors influencing the
migration, exudation, phase separation, and desorption
of surfactant from latex paint films are a continuing topic
of discussion within the coatings industry and have been
reviewed elsewhere [15].
Atomic force microscopy (AFM) is one of the
most frequently employed imaging techniques for soft
polymeric materials and has thus far been the most
successful method for characterizing subtle changes
occurring at the surfaces of acrylic emulsion paint films
that are not visible to the naked eye, nor visible using
other imaging techniques. AFM is a scanning probe
technique used for high-resolution surface investigation
at the micrometre and nanometre scale. It essentially
involves scanning a probe tip situated on the end of
a flexible cantilever across the sample surface and

© The International Institute for Conservation of Historic and Artistic Works 2011 DOI: 10.1179/204705811X13110713013317
 a preliminary evaluation of the surfaces of acrylic emulsion paint films  217
measuring the attractive or repulsive forces between the
tip and the sample.
As AFM is capable of acquiring images with little
or no sample preparation, it has been used to elucidate
surface structure in many fields of technology, including
biomolecules [16–18], nanoparticles [19, 20] and
polymer composites [21–24], and has more recently
been applied to the study of paint films. Biggs and co-
workers used AFM to determine the rates of physical
degradation (e.g. ablation of the resin layer, loss of
pigment particles and surface roughening) of pigmented
polyester/melamine surfaces after ultraviolet (UV) light
exposure to predict long-term changes in gloss and
colour [25]. Kirsch et al. [26] investigated the impact on
latex paint films of abrasion caused by three different
scrubbing techniques (brush, scratch pad, ball point pen).
The images obtained demonstrated that the surfaces of
highly filled latex paints were dominated by pigment,
exhibiting a porous structure, and that after the scrub
tests the paint surfaces were dominated by the polymer
component. In another study, Tiarks and co-workers
used AFM to explore the effect of polymer binders and
dispersing agents on the distribution of titanium dioxide
(TiO2) pigments in dried acrylic paint films, where a
relationship between film formation conditions and the
clustering behaviour of TiO2 pigment was demonstrated
[27].
AFM has also been successfully used to explore
the distribution and formation of surfactant layers
on unpigmented acrylic latex film surfaces [28, 29]
and the effects of wet-surface cleaning treatments
on the surfaces of pigmented acrylic emulsion paint
films have recently been investigated. Ploeger et al.
[5] noted morphological changes on naphthol red,
bone black and ultramarine blue test paint films after
1 hour immersions in aqueous systems. Changes in
surface roughness noted were attributed to pigment
particle size differences, different polymer binder
compositions and the amounts of surface surfactant
present. Chiantore et al. [30] and Scalarone et al. [31]
studied the appearance of water-rinsed and thermally
aged unpigmented acrylic emulsion polymer films,
where differences were attributed to coalescence of
the polymer and migration of surfactant to the paint
surface. Ormsby and co-workers also used AFM for
preliminary investigations into the surfaces of titanium
white artists’ acrylic emulsion paint films, noting that
migrated surfactant layers appeared to swell prior to
removal through swabbing with aqueous systems and
that the amounts of migrated surfactant present varied
with paint brand [2, 32].
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EXPERIMENTAL
This study involved the use of two different AFM
systems – one bench-top and one portable – to explore
the effects of simplified cleaning treatments on the
surfaces of test paint films cast from two contemporary
paint brands and of three acrylic emulsion-based works
of art from Tate’s collection (further described in Table
1). Issues such as the presence and removal/disturbance
of the surface surfactant layer, surface roughness and
changes to surface topography were explored by means
of atomic force microscopy in order to characterize
changes arising from surface cleaning treatments. To
assist the interpretation of the AFM images, chemical
information was collected from paint surfaces using
Fourier transform infrared – attenuated total reflectance
spectroscopy (FTIR-ATR) and portable mid-infrared
reflectance spectroscopy, details of which have been
published elsewhere [3].
The group of test paint samples and areas on each
of the Tate paintings were imaged and subjected to a
1 minute swab rolling treatment with either deionized
water or low boiling range aliphatic hydrocarbon
(petroleum spirit, boiling point 60–80°C, Analar,VWR/
BDH product No.101794H) as described in Table 2.
The treated test samples were then re-imaged using
the bench-top AFM system after one week’s drying in
ambient dark conditions; the painting surfaces were re-
examined in situ with the portable system as soon as the
cleaned areas were blotted and appeared dry. A selection
of Talens titanium white paint films were also light-aged
at 15000 lux for 16 weeks under Philips TLD 58W/840
daylight tubes with the UV component filtered by
acrylic sheet (Perspex®). Assuming reciprocity, this is
equivalent to ~50 years exposure under normal museum
conditions. Details of the subsequent conservation
treatments carried out on each of the works of art have
been published elsewhere [33].
The bench-top AFM system was operated in tapping
mode, in which the probe tip lightly touches the sample at
regular intervals while maintaining a constant oscillation
amplitude. When the tip interacts with the paint surface
the oscillation amplitude decreases; this decrease is sensed
and the tip is then raised away from the sample to regain
the previous amplitude [34]. The tip-sample interaction
is monitored by reflecting a laser off the cantilever into
a split photodiode detector. By detecting the difference
in the photodetector output voltages, changes in the
oscillation amplitude are determined [35]. In this way,
through control electronics, the tip can be rastered across
the sample to generate topographical images. One of the
218  E. KAMPASAKALI, B. ORMSBY, A. COSEnTINO, C. MILIANI AND T. LEARNER

Table 1  List of samples and works of art analysed by atomic force microscopy and FTIR-ATR spectroscopy and description of paint constituents

Paint or artist and Paint description Pigments identified Extenders identi- Paint medium PEO-based Relative amount of
title (colour) fied surfactant detected surfactant on surface
on surface?

Talens Titanium white PW6 Chalk EA/MMA Yes1 Major

Rembrandt Colours
(2003) Titanium white PW6 Chalk No1 None
(light aged)
Azo yellow lemon PY3 Chalk Yes1 Moderate

Phthalocyanine PG7 Chalk Yes1 Major

green
Burnt umber PR101 + PBk11 Chalk Yes1 Major

Gesso PW6 Chalk, kaolin Yes1 Major

Liquitex Titanium white PW6 – BA/MMA No1 None

High Viscosity
Colours
(2003)

Warhol, Dark pink back- PR207, Ti white CaSO4 EA/MMA No1,2 None
Portrait of Brooke ground
Hayward Green background Unidentified green, – EA/MMA No1,2 None
(1973) Ti white
T12600 Yellow background Cadmium yellow, BaSO4 EA/MMA No1,2 None
Ti white

Liberman, Black Mars black – EA/MMA Yes2 Moderate

Andromeda (1962)
T00650

Hoyland, Umber Burnt umber BaSO4, Chalk EA/MMA Yes2 Major

25.4.69
(1969)
T01129

Note: Surfactant detected with (1) FTIR-ATR and/or (2) portable mid-IR reflectance spectroscopy [3, 9].

unintended benefits of vibrating the probe tip is that the
lateral forces that may be acting on the probe during
scanning are released, hence when the probe is away from
the surface there are no horizontal forces acting on it
[36]. This enables tapping mode to image soft, fragile and
adhesive surfaces (such as paint films) without damaging
them. The images included are topographical or ‘height’
images, as the corresponding phase images did not offer
additional useful information. Images were limited to a
10 × 10 µm field of view due to constraints imposed
by shared use of the instrument and by the relative
roughness of the paint samples.
The in situ images of the painting surfaces were col­
lected using a portable AFM in dynamic force mode.
Here the cantilever never touches the surface but
is oscillated at its resonance frequency, very close to
the sample surface. Changes in the amplitude of the
oscillation caused by the sample surface topography are
compensated by a feedback loop that approaches or
retracts the probe with a piezoelectric z-scanner until
the non-perturbed reference signal is recovered. The
compensating feedback signal is directly related to the
height of the sample surface features. The in situ images
are shown in phase contrast mode in which, in addition

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 a preliminary evaluation of the surfaces of acrylic emulsion paint films  219

Table 2  Details of paint samples examined by AFM (not all shown) and treatments applied

Paint brand/ Paint colour or painting AFM system       Free-film tests Primed canvas substrate tests
artist title

Talens Titanium white Bench control water pet. spirit control water swabbed; spirit swabbed
+ light aged swabbed swabbed

Azo yellow Bench control water pet. spirit – – –

swabbed swabbed

Phthalocyanine green Bench control water pet. spirit control water swabbed; spirit swabbed
swabbed swabbed

Burnt umber Bench control water pet. spirit – – –

swabbed swabbed

Gesso Bench control water pet. spirit control water swabbed; spirit swabbed
swabbed swabbed

Liquitex Titanium white Bench control water pet. spirit control water swabbed; spirit swabbed
swabbed swabbed

Warhol Portrait of Brooke Bench – Background colour sample from yellow canvas
Hayward (removed from reverse foldover edge)
(1973)
– Background colour from green canvas
– Background colour from pink canvas (control,
water cleaned)
Liberman Andromeda Portable – Black paint – control (untreated)
(1962) Black paint – water swabbed
Black paint – petroleum spirit swabbed

Hoyland 25.4.69 Portable – Umber paint – control (untreated)

(1969) Umber paint – water swabbed
Umber paint – petroleum spirit swabbed

to the vibration amplitude, the phase shift between the
cantilever vibration and a reference signal is also measured,
which changes when the resonance characteristic of the
cantilever shifts with tip-sample interaction. This mode
is therefore sensitive both to fine topographical features
and to differences in the stiffness of surface materials,
facilitating more detailed and contrasted images than
seen with the topographical images produced by the
bench-top system. This stand-alone design allowed the
portable AFM head to be placed directly onto painting
surfaces; under controlled conditions (sufficient isolation
and minimal vibration etc.) high-precision measurements
could be obtained. When not in a controlled, research
quality environment (such as a conservation studio) this
technique is hindered by environmental vibrational noise.
Further details of experimental procedures including
paint sample preparation and instrument specifications
are listed in the Appendix.
REFERENCE PAINT SAMPLES
Talens titanium white and gesso
The control (untreated) Talens titanium white free-
film sample image (Figure 1a) shows smooth, large
aggregates formed by the relatively abundant surfactant
layer on this paint film as documented by FTIR-ATR
analysis (Figure 1c) where the main absorbance bands
of the PEO-based surfactant are located at ~2890 (not
shown), 1343, 1110 and 964 cm−1 [9]. These aggregates
were described as ‘hills’ by Hellgren et al. [37] in an
AFM study of formulations based on polymerizable
and conventional surfactants. The absence of these
bands in the FTIR-ATR spectrum obtained from the
sample treated by 1 minute of water-swabbing (Figure
1f) confirmed that this treatment removed all detectable
surfactant.

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220  E. KAMPASAKALI, B. ORMSBY, A. COSEnTINO, C. MILIANI AND T. LEARNER

(a) (d) (g)

(b) (e) (h)

(c) (f) (i)

Figure 1  AFM amplitude images (10 × 10 μm), roughness profiles and FTIR-ATR spectra of Talens titanium white free-film samples: (a, b and c) the
control; (d, e and f) water-cleaned; and (g, h and i) petroleum spirit-cleaned. The asterisk in the FTIR-ATR spectra indicates the characteristic peaks of PEO-
based surfactant.

The AFM image of the water-swabbed film (Figure
1d) revealed rough particulate aggregates and smooth
areas attributable to the pigment particles and polymer
surface respectively, rendered more visible by the
removal of the surfactant layer. A similar observation
was made by Ploeger et al. [5] where exposed particles
were visible on the surface of water-immersed acrylic
paint films. The petroleum spirit-swabbed sample
(Figure 1g) had smaller features, however they appeared
similar to the surfactant ‘hills’ seen on the control
(Figure 1a). The FTIR-ATR spectrum of this sample
(Figure 1i) confirmed that the surfactant layer remained
after treatment, hence the AFM image illustrates the
disruption of the surfactant layer through mechanical
action. These observations were also reflected in the
corresponding AFM roughness profiles in which the
control sample (Figure 1b) was characterized by the
higher, broad features of the surfactant aggregates. The
water-swabbed sample (Figure 1e) had a flatter profile,
and the petroleum spirits-swabbed sample (Figure 1h)
had a reduced profile, intermediate between the control
and water-swabbed sample. Samples of Talens gesso paint
also tested (not shown) produced similar AFM images
due to their similar constituents.
As documented in a recent review of scientific
research into acrylic paints [15], exposure to accelerated
light ageing tends to result in the disappearance of
migrated surfactant layers from the surface of these
paint films. Recent research has also shown that the
migration process resumes when light-aged samples

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 a preliminary evaluation of the surfaces of acrylic emulsion paint films  221

(a) (c) (e)

(b) (d) (f)

Figure 2  AFM amplitude images (10 × 10 μm) and FTIR-ATR spectra of Talens titanium white light-aged free-film samples: (a and b) the control; (c and d)
water-cleaned; and (e and f) petroleum spirit-cleaned.

are further left to naturally age in dark conditions
[9]. One study, however, indicated that surfactant
remained on the surface after light ageing, with
differences attributed to the ageing regimes used and
increased paint film thickness [38]. The photo-oxidative
degradation of non-ionic surfactants is known to occur
[39, 40]; and understanding this process with respect to
artists’ acrylic emulsion paints is the subject of ongoing
research.
In this study, the FTIR-ATR spectra for the light-
aged Talens titanium white films (Figures 2b, d and f)
once again confirmed the absence of surface surfactant
after light exposure. The corresponding AFM images
present useful information on the potential effects of
wet-cleaning acrylic emulsion films with no detectable
surfactant layer. Here, raised particulate agglomerates
were visible on the surface of the surfactant-lean control
sample (Figure 2a), and the petroleum spirit swabbing
treatment appears to have led to a slight surface rough­
en­ing (Figure 2e). The water-swabbed sample (Figure
2c) appeared smoother than the control due to the
removal of particulate surface dirt, and/or the possible
swelling of the polymer film during treatment, also
observed by Kirsch et al. [26].
The Talens titanium white and gesso paint films cast
onto canvas substrates (not shown) produced similar
images to the free-film samples, and FTIR-ATR analysis
confirmed the presence of surfactant on the control
and petroleum spirits-cleaned samples. The water-
swabbed samples were once again characterized by small
particulate aggregates and more visible/smoothed acrylic
polymer areas after the removal of the surfactant layer.
Liquitex titanium white
The FTIR-ATR spectrum of the Liquitex titanium
white free-film sample (Figure 3b) was dominated
by contributions from acrylic polymer and TiO 2
pigment, confirming that no surfactant was present. The
corresponding AFM images (Figure 3a and 3c) were
dominated by paint surface features rather than the larger
‘hills’ common to surfactant-rich samples. This supports
previous FTIR-ATR findings where greater amounts
of surface surfactant were detected on the Talens ethyl

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222  E. KAMPASAKALI, B. ORMSBY, A. COSEnTINO, C. MILIANI AND T. LEARNER
(a)
(b)
Figure 3  AFM amplitude images (10 × 10 μm) and FTIR-ATR spectra of Liquitex titanium white free-film samples (a and b) the control; and (c and d)
water-cleaned.
acrylate/methyl methacrylate [p(EA/MMA)]-based
paints, and none/trace amounts were detected on the
Liquitex butyl acrylate/methyl methacrylate [p(nBA/
MMA)]-based paints [2, 4, 9]. Recent research has also
shown that the abundance of surface surfactant can be
affected by the film substrate [41]. The AFM image of
the water-swabbed sample (Figure 3c) indicated once
again that the surface appeared more polymer-rich
after treatment. This was also observed for the Liquitex
titanium white canvas samples (not shown) which
suggests that films without substantial surfactant layers
may be more vulnerable to swelling during aqueous
treatment.
Talens burnt umber, azo yellow and
phthalocyanine green
As expected, the FTIR-ATR analysis of three other
Talens free-film control samples (burnt umber: Figure 4;
S t u dies i n co n servatio n 5 6 ( 2 0 1 1 ) pa g es 2 1 6 – 2 3 0
(c)
(d)
azo yellow: Figure 5; phthalocyanine green – not
shown) confirmed the presence of high levels of surface
surfactant on these films. The AFM image of the Talens
burnt umber control (Figure 4a) is characterized by a
smooth, relatively flat surface with some loose soiling
that was subsequently removed during cleaning. This
surfactant layer was less ‘hilly’ than the Talens titanium
white control, which may reflect the relative smoothness
of the paint surface and/or differences in the surfactant
migration process. The image of the petroleum spirits-
swabbed sample (Figure 4e) reflects the underlying
paint film contours to a greater extent than the control
(Figure 4a). The slight reduction in the height of the
~1110 cm−1 band for this sample (Figure 4f) suggests
that although some surfactant was removed, substantial
amounts remain on the surface.
The surfactant layer was also only partially reduced
by the water-swabbing treatment (Figures 4c and 4d).
Possible reasons for this include: subtle differences in
 a preliminary evaluation of the surfaces of acrylic emulsion paint films  223

(a) (c) (e)

(b) (d) (f)

Figure 4  AFM amplitude images (10 × 10 μm) and FTIR-ATR spectra of Talens burnt umber free-film samples: (a and b) the control; (c and d) water-
cleaned; and (e and f) petroleum spirit-cleaned. The asterisk in the FTIR-ATR spectra corresponds to the characteristic band of a PEO-based surfactant.

the amounts of surfactant present; inconsistent cleaning
technique; and/or surfactant solubility issues. PEO-based
surfactants are employed as emulsion stabilizers because
of their multiple affinities with the polymer phase, water
phase and added pigments. Further research is required
to investigate whether this type of surfactant has a higher
affinity for particular pigment surfaces and/or whether
the water-solubility of the surfactant changes after
photo-degradation and/or pigment-catalysed reactions
[15].
The AFM image of the azo yellow control sample
(Figure 5a) shows fine features that were not visible
on any of the other films imaged. These features may
simply be fine surface dirt particulates rendered more
visible by the relatively smooth surface of this paint
film, loose (unbound) pigment particles, or perhaps
artefacts of the surfactant exudation process. These
features were partially reduced by the water (Figure
5c) and petroleum spirit swabbing treatments (Figure
5e) and it was noted that pigment transferred onto
the swabs with both cleaning systems. After treatment,
the corresponding roughness profiles (not shown)
changed from plots consisting of small sharp peaks to
curves more typical of surfactant-free paint surfaces. In
addition, no pigment aggregates were visible on these
samples, presumably due to the smaller pigment particle
sizes used.
The difference in the height of the ~1110 cm −1
band in the FTIR-ATR spectra (Figures 5b and 5f)
suggests an increase in surface surfactant abundance after
swabbing with petroleum spirits. This was not noted
for other samples, and it is unlikely that surfactant had
been transported from within the bulk paint film, due
to the low solubility of these surfactants in aliphatic
hydrocarbon solvents. This phenomenon could be due
to the uneven exudation of surfactant across the paint
film and/or the pooling of surfactant during cleaning.
Another interesting feature of the FTIR-ATR data for
this sample was that the water-swabbed film (Figure 5d)
featured a broad band around 3300 cm−1 (not shown)
which also appears to a lesser extent on both the Talens
titanium white and burnt umber films. This absorbance
band suggests that water had been retained within the
films for at least 3 days after treatment.

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224  E. KAMPASAKALI, B. ORMSBY, A. COSEnTINO, C. MILIANI AND T. LEARNER
(a) (c)
(b) (d)
Figure 5  AFM amplitude images (10 × 10 μm) and FTIR-ATR spectra of Talens azo yellow free-film samples: (a and b) the control; (c and d) water-cleaned;
and (e and f) petroleum spirit-cleaned. The asterisk in the FTIR-ATR spectra indicates the characteristic peaks of PEO-based surfactant.
The Talens phthalocyanine green free-film and
canvas samples (not shown) produced similar images to
the umber and azo yellow films, namely: the partial/
complete removal of surfactant after water swabbing with
a corresponding increase in roughness and topographical
detail; a disrupted surface on the petroleum spirits-
cleaned sample; and the removal of loose particulates
where present. The phthalocyanine green canvas sample
was also devoid of the pigment clusters seen in the
titanium white, gesso and umber films, once again
reflecting differences in pigment particle size and
dispersion for the synthetic organic pigmented paints.
WORKS OF ART
Andy Warhol, Portrait of Brooke Hayward, 1973
(Tate T12600)
Small samples of painted canvas were removed from
the Portrait of Brooke Hayward by Andy Warhol. This
mixed media work consists of four equally sized
canvases painted with different acrylic colours, forming
the background for Warhol’s subsequently applied
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(e)
(f)
black alkyd-based screen prints. In this case 0.5 ×
0.5 cm samples of painted canvas were removed with
permission from the reverse fold-over edges of each of
the yellow, pink and green canvases. The paint media of
the coloured layers was identified as p(EA/MMA); the
pigments included cadmium yellow, chromium green
and a synthetic organic quinacridone-based red pigment
(PR 207) [3, 9]. Titanium white was also identified in
all samples, and barium sulphate (BaSO4) and calcium
sulphate (CaSO4) extenders were found in the yellow
and pink samples respectively. FTIR-ATR analysis of
the surface of these samples confirmed that no surfactant
was present [3].
The bench-top AFM images of all three painted
canvas samples (Figures 6a, b and c) show the rough
particulate aggregates also noted on the light-aged
titanium white test samples (Figure 2). As was the case
for the Talens azo yellow and phthalocyanine green
films, the pink canvas sample differed with respect to
the density of the particulate aggregates due to the
predominantly synthetic organic pigment present. After
water-swabbing (Figure 6d) the protruding aggregates
may be slightly less pronounced.
 a preliminary evaluation of the surfaces of acrylic emulsion paint films  225

(a) (c)

(b) (d)

Figure 6  Warhol’s Portrait of Brooke Hayward samples AFM amplitude images (10 × 10 μm): (a) green canvas; (b) yellow canvas; (c) pink canvas; and (d)
water-cleaned pink canvas

Alexander Liberman, Andromeda, 1962
(Tate T00650)
A portable AFM instrument was used in situ to image 20
× 20 μm areas of the surface of Alexander Liberman’s
circular acrylic emulsion-based painting, Andromeda.
Areas of the black paint (identified as Mars black by
SEM-EDX analysis) were imaged to record changes
occurring after water and petroleum spirit swabbing
treatments (Figure 7). Infrared spectroscopy of the
painting surface with a portable mid-IR reflectance
instrument (details published elsewhere) confirmed the
presence of migrated surfactant on the paint surface,
as well as its removal with water and partial removal
with petroleum spirits [3, 9]. Although the AFM phase
contrast images appear different to the topographical
images obtained from the bench-top system, the
untreated paint surface (Figure 7a) was shown to have
similar large surfactant-like ‘hilly’ features which were
subsequently removed via water swabbing (Figure 7b)
to reveal smaller features typical of the paint surface. The
petroleum spirit-swabbed sample (Figure 7c) presents
a combination of the larger features typical of surface
surfactant and the finer features of the polymer surface,
which concurs with the IR data.
John Hoyland, 25.4.69, 1969 (Tate T01129)
John Hoyland’s acrylic emulsion painting 25.4.69 was
also imaged using the portable AFM system. Figure 8a,
taken from a palette knife applied burnt umber passage,

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(a) (b) (c)

Figure 7  Portable AFM images (20 × 20 μm) of black area of Alexander Liberman’s Andromeda: (a) untreated control; (b) water-cleaned; and (c)
petroleum spirit-cleaned. The banding patterns are vibration-derived artefacts of the in situ test set-up.

(a) (b)

Figure 8  Portable AFM images (20 × 20 μm) of umber of John Hoyland’s 25.4.69: (a) untreated control; and (b) petroleum spirit-cleaned. Again, the
banding patterns are vibration-derived artefacts of the in situ test set-up.

depicts the large features characteristic of high levels
of migrated surface surfactant. As was the case for the
Mars black area of the Liberman painting, the use of
petroleum spirits (Figure 8b) resulted in the partial
removal of surfactant; revealing the finer features of the
underlying paint film.
CONCLUSIONS
It is important to characterize the subtle nature of
the surfaces of acrylic emulsion paint films so that
the risks associated with conservation procedures
and access (i.e. display) are known and minimized.
Atomic force microscopy in combination with infrared
spectroscopic analytical techniques have successfully
characterized the surface of artists’ acrylic emulsion
paint films, including documenting changes occurring
after accelerated ageing and wet-surface cleaning
treatment. Differences in the character of the surfaces
of untreated control test paint films cast from different
paint brands and pigment types were observed using a
bench-top AFM system, and a portable AFM system
facilitated the in situ imaging of changes to the sub-
micron morphology of the surface of acrylic emulsion
paintings. In all cases, interpretation of the AFM images
was supported by infrared spectroscopy data, with an
emphasis on monitoring the levels of detectable surface
surfactant.
Where present in reasonable quantities, migrated
surface surfactant layers appear as large, smooth, round
‘hill-like’ structures. The removal/partial removal of
surfactant through surface cleaning treatment was
success­fully imaged by AFM, as was the disappearance of
surfactant after light ageing.

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 a preliminary evaluation of the surfaces of acrylic emulsion paint films  227
The removal of substantial surfactant layers through
aqueous cleaning resulted in the enhanced visibility
of the pigment/extender clusters present in the paint
films. Surfactant remained present on all petroleum
spirits-swabbed samples after treatment, although partial
removal often resulted from mechanical action, causing
surface disturbance. Where surfactant was not present,
the petroleum spirits-swabbed samples also appeared
roughened, a phenomenon that warrants further
investigation. Some topographical differences were also
observed between paints made with different pigments;
for example the synthetic organic pigmented films
(azo yellow, phthalocyanine green and quinacridone
red PR207) tended to have smoother, medium-rich
surfaces, with smaller particulate features reflecting
differences in pigment particle size, distribution and
concentration.
Where migrated surfactant was either not present
or present in low quantities, the paint surface appeared
more polymer-rich after aqueous treatment; which
requires further exploration to determine whether this
results from surface polymer swelling. Fine deposited dirt
particulates visible on the smoother paint surfaces were
also removed through aqueous cleaning.
The migrated surfactant layer on the Talens titanium
white films appeared to be more completely removed
by aqueous cleaning than from the other paints
tested, including the Talens burnt umber sample. This
response may be a function of the amounts of surfactant
present, inconsistent cleaning technique, or may
indicate a surface–surfactant interaction or surfactant
solubility changes that also warrant further investigation.
Nonetheless, partial surfactant removal after one
swabbing treatment is consistent with the repeated
applications often required when removing substantial
soiling layers from works of art [13, 33].
APPENDIX
Paint samples
Paint films were applied onto Teflon-coated stainless
steel plates and 10 ounce pre-acrylic primed cotton
canvas sections using a Sheen Instruments adjustable film
caster to give a dry film thickness of 110 ± 20 µm. By
the time of imaging, the test samples had approximately
5 years natural ageing in dark conditions. The paintings
from Tate’s collection are listed in Table 1 together with
details of the pigment and medium composition of each
paint passage.
S t u dies i n co n servatio n 5 6 ( 2 0 1 1 ) pa g es 2 1 6 – 2 3 0
Bench-top AFM
Images were obtained using a Veeco MultiMode
scanning probe microscope with a ‘J’ scanner and
NanoScope IV controller in tapping mode with silicon
probes. All scans were collected over a 10 × 10 μm area.
The most informative images were derived from the raw
amplitude and 3D data plots, while the phase images
were the most difficult to interpret, particularly for the
rougher samples, due to artefacts. Data processing using
n-Surf 1.0 beta software enabled improvement of the
height images. Since it is almost impossible for an AFM
stage to return and scan the same spot, several areas from
each sample were scanned and representative images
captured. Imaging the Warhol canvas samples proved
more difficult due to the rough surface imparted by the
canvas substrate as well as a light layer of soiling.
In some instances (as in Figures 1b, e and h) surface
roughness profiles were extracted from the AFM images.
The surface profilometry plots were generated from the
AFM image by selecting three pairs of points opposite
sides of the image, each pair of points defining the ends
of three straight lines across the image. The histograms
representing the relative heights of each pixel along each
of these three lines constitute the roughness profiles
shown in Figure 1.
Portable AFM
Images were collected with a Nanosurf easyScan DFM.
Scans were made using a POINTPROBE Silicon SPM-
Sensor, Al-coating cantilever (Nanoworld). The scans
were treated and analysed with SPIP software (Image
Metrology). Scans have been reported in 3D visualization
in grey scale, where the darker colours correspond with
deeper regions and bright colours with higher regions.
In situ measurements were collected by positioning the
painting in a supported horizontal position on the floor
to minimize vibrational noise, and the AFM scan head
(weight 350 g) placed carefully onto the painting surface.
In the absence of more sophisticated vibration damping
methods in the instrumental set-up, the AFM images
obtained from these tests included vibration-derived
artefacts, which are visible as banding patterns (see
Figures 7 and 8).
FTIR-ATR
ATR spectra were obtained on a Nicolet Avatar 360
spectrometer using a germanium ATR crystal (200
scans at 4 cm−1 resolution). At around 2000 cm−1 the
228  E. KAMPASAKALI, B. ORMSBY, A. COSEnTINO, C. MILIANI AND T. LEARNER
germanium crystal has a penetration depth of around 0.66
μm. All data were processed using Omnic 6.2 software.
ACKNOWLEDGEMENTS
The authors would like to thank: AXA Art Insurance;
The Getty Conservation Institute, Los Angeles; Dr
Bamber Blackman and Sian Fogden of Imperial College,
London; Dr Mark Underhill and Dr Joyce Townsend of
Tate, London. Access to portable AFM instrumentation
was facilitated through the transnational access facility
MOLAB group of the 6th Framework Programme
(Contract Eu-ARTECH FP6, RII3-CT-2004-506171).
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AUTHORS
Elli Kampasakali was the AXA art research fellow
at Tate (2007–2009), assessing the effects of surface
cleaning treatments on acrylic emulsion paints for the
Tate AXA Art Modern Paints Project (TAAMPP).
Address: c/o Conservation Science, Tate Britain, Millbank,
London, SW1P 4RG, UK. Email: elinamoz@yahoo.com
Bronwyn A. Ormsby is senior conservation scientist
at Tate, responsible for the analysis of modern and
contemporary art materials and conservation treatment
research. Address: Conservation Science, Tate Britain,
Millbank, London, SW1P 4RG, UK. Email: bronwyn.
ormsby@tate.org.uk
Antonino Cosentino is currently a visiting scholar
at CISA3 (Center of Interdisciplinary Science for
Art, Architecture and Archaeology), University of
California San Diego. Address: University of California
San Diego, 9500 Gilman Dr. # 0436, Atkinson Hall, 5th
Floor, La Jolla, California, CA 92093-0436, USA. Email:
acosentino@ucsd.edu
Costanza Miliani is a research scientist at the Istituto
di Scienze e Tecnologie Molecolari del CNR (CNR-
ISTM) in Perugia and scientist responsible for the
MOLAB a mobile European facility for the non-invasive
in situ study of works of art. Address: CNR-ISTM,
230  E. KAMPASAKALI, B. ORMSBY, A. COSEnTINO, C. MILIANI AND T. LEARNER

c/o Dipartimento di Chimica, Via Elce di Sotto, 8, 06123
Perugia, Italy. Email: miliani@thch.unipg.it
T homas J.S. L earner is senior scientist and head
of Modern and Contemporary Art Research at the
Getty Conservation Institute, overseeing research into
improving methods of analysis of modern paints and
examining their behaviour in response to ageing and
cleaning treatment. Address: Getty Conservation Institute,
1200 Getty Center Drive, Suite 700, Los Angeles, California,
CA 90049, USA. Email: tlearner@getty.edu

Résumé — Les surfaces des films de peinture émulsion acrylique (dispersion) ont été examinées par microscopie à force atomique
(AFM), en tenant compte des informations chimiques obtenues par spectroscopie infrarouge. Les caractéristiques morphologiques
et chimiques des surfaces d’une série de films de peinture moderne de référence ont été étudiées, y compris la caractérisation des
changements causés par l’exposition à l’eau et au minéral spirit. Un système in situ AFM portable a été aussi utilisé pour
documenter les surfaces des peintures émulsions acryliques de la collection de Tate en comparaison des films de référence récemment
préparés. Le retrait complet et partiel des agents tensioactifs qui ont migré a été imagé avec succès ainsi que les caractéristiques
provenant de l’action mécanique. Des différences dans les surfaces des peintures et les couches de tensioactifs ont été observé en
fonction du type de pigment, de la marque de peinture et de l’exposition au vieillissement accéléré, en plus des opérations de
nettoyage aqueux appliquées aux surfaces. Les résultats contribuent à mieux comprendre les changements subtils des surfaces des
peintures émulsions acryliques et sont en rapport avec les débats actuels sur le retrait des tensioactifs d’origine de ces films lors des
traitements de conservation.

Zusammenfassung — Die Oberflächen von Malschichten aus Acrylemulsionen (Dispersionen) wurden mit
Rasterkraftmikroskopie (AFM) untersucht. Diese Untersuchungen wurden durch chemische Analysen mit Hilfe der
Infrarotspektroskopie flankiert. Die morphologischen und chemischen Eigenschaften der Oberflächen einer Referenzserie von
modernen Malschichten wurden untersucht, einschließlich der Charakterisierung der Veränderung, die diese durch Einwirkung
von Wasser und Benzine erfahren. Ein tragbares in situ AFM – System wurde auch dazu verwendet, die Oberflächen von
Acrylmalschichten in der Sammlung der Tate als Vergleich zu unlängst hergestellten Probefilmen zu charakterisieren. Die
vollständige und teilweise Entfernung migrierter Tenside konnte ebenso erfolgreich sichtbar gemacht werden wie die Effekte der
mit der Reinigung einhergehenden mechanischen Beanspruchung. Es konnten Unterschiede der Oberflächen und der migrierten
Tensidschichten in Abhängigkeit von der Pigmentierung, der Herstellerfirma, der Dauer der künstlichen Alterung und darüber
hinaus auch der Art der feuchten Reinigung ausgemacht werden. Die Befunde tragen zu einem tieferen Verständnis der in
Acrylmalschichten auftretenden subtilen Veränderungen bei und sind daher relevant für die Debatte über die Entfernung /
Störung der originalen Oberflächentenside auf diesen Filmen durch Konservierungsmaßnahmen.

Resumen — En este artículo se presenta el estudio de las superficies de diferentes películas pictóricas a base de emulsión acrílica
mediante microscopía de fuerza atómica (AFM), con el respaldo de la información química obtenida por medio de espectroscopía
infrarroja. Para ello se estudiaron las características morfológicas y químicas de las superficies de una serie de películas de pintura
moderna de referencia, incluyendo la caracterización de los cambios que éstas experimentaron tras ser expuestos a la acción del
agua y de hidrocarburos (mineral spirits). Así mismo, se utilizó un sistema AFM portátil in situ para documentar las superficies
de las pinturas a base de emulsión acrílica de la colección de la Tate con el fin de poder compararlas con las películas de referencia
recientemente elaboradas. En esta investigación se han podido obtener imágenes de la eliminación total y parcial del surfactante
migrado junto con los efectos derivados de la acción mecánica. Igualmente se han detectado diferencias en las superficies pictóricas y
en las capas de surfactante migradas en base al tipo de pigmento, la marca de pintura y la exposición al envejecimiento acelerado,
así como a los efectos del tratamiento de limpieza en húmedo de dichas superficies. Los resultados obtenidos contribuyen a una
mejor comprensión de los sutiles cambios que experimentan las superficies pictóricas de las emulsiones acrílicas y son relevantes en
los debates actuales que plantean la eliminación/alteración por medio de un tratamiento de conservación del surfactante original
presente en la superficie de estas películas.

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