SUMMARY Conservators of old silk paintings often need to use

A traditional Chinese repair silks to replace missing areas; they usually prefer to use silk
that has comparable mechanical properties to the silk in the original
method for weakening painting. It is possible to change the properties of modern silk and
a method that is already in use in China involves soaking silk in
silk for use in the a 0.1 M potassium permanganate solution, typically for one hour.
The technique was investigated using specially woven Chinese
conservation of silk silks that the British Museum was able to procure thanks to the
Shanghai Museum. The silks were artificially aged with potassium
paintings permanganate and the tensile strength of the resulting material was
measured. Three methods for removing manganese residues were
assessed using scanning electron microscopy with energy dispersive
Vincent Daniels, Marei Hacke, Jin Xian X-ray spectrometry to test for residual metal; acidified hydrogen
Qiu and Valentina Marabini peroxide was the best of the reagents tested. Painted and unpainted
samples of weakened silk were subjected to accelerated ageing
and showed small colour changes lightening for light ageing and
yellowing for heat ageing with the changes occurring predominantly
in the early stages of ageing. The painted samples showed smaller
colour changes. A simulation of a mounted painting in scroll format
was produced so that repairs could be made with the weakened
silk. The artificially weakened silk proved to be a satisfactory repair
material both technically and aesthetically.

Introduction
Chinese paintings are produced in many set formats and are
mostly painted on paper or silk. The supports for paintings
can be very sophisticated when a crucial balance between
strength and flexibility is required, for example in traditionally
made hanging scrolls or hand scrolls. Silk, although initially a
relatively strong textile fibre, becomes weaker over time and
eventually this deterioration manifests in paintings as tears,
cracks and lacunae, Figure 1. The missing areas are often
filled with silk repairs as part of a combined conservation and
remounting process. The experience of traditionally trained
scroll conservators has shown that a silk infill must be of a
comparable or weaker strength to the surrounding painted
silk substrate, and that performing a repair with a silk that is
too strong will result in the relevant section, instead of being
reinforced, becoming weaker and fragmented by adverse
mechanical forces in the area of the join. Finding appropri-
ate materials for silk repair can, as described below, be a very
challenging task.
In China there has been a longstanding tradition of
producing copies of great masterpieces. These copies,
if contemporary with the originals, would have aged in a
similar fashion. Conservators in China have traditionally
used old silk from non-image areas of discarded, damaged
copies to repair original paintings that are in danger of
further breaking or tearing or which already show missing
areas. Many conservators in China have a stock of old silk
off-cuts to use in their repairs, but this material is not readily
available to conservators outside China, including those at
the British Museum, and even in China such resources are
slowly being depleted. Additionally, modern conservation
ethics do not look favourably on this practice as it attaches
current perceptions of importance and value to the paintings
used to provide repair silk. In consequence, there is a need
to investigate and use reliable, accessible and cost-effective
methods to artificially age modern silk to match the strength
of naturally aged silks.

41
Figure 1. Detail of a sixteenth-century painting Portrait of an Official in front of the Forbidden City (1881,1210.0.87), claimed to be by Zhu
Bang, showing poorly executed old repairs (predating its acquisition by the British Museum) that are discoloured and in need of replacement
Old silk prepared for painting is already coated with a thin
sizing layer of animal glue mixed with alum, and both the silk
and coating darken on ageing. When the colour of silk repairs
is adjusted to that of the painting it is advantageous if the
repair silk is slightly lighter than the original to facilitate colour
matching. It is also important to match the weave type of the
repair silk to that of the painting. In 1982 the British Museum
obtained 28 specially woven silks with weave types typically
encountered on old paintings. The silks were produced at the
request of Mr Feng Yao Geng, former head of conservation
at the Shanghai Museum, and the stock was shared by the
Shanghai Museum with its partner museums in China, the
UK and the USA.
The conservation process for repairs using old silk
The conservation of Chinese paintings on silk begins with
finding a suitable repair silk for any missing areas. This repair
silk must match the original substrate in a number of respects:
warp and weft alignment; weave type; thickness of threads;
and spacing between threads. The initial hue of the silk is also
considered. This selection process is traditionally undertaken
by the scroll mounter on the basis of observation using simple
magnifiers, touch, and training and experience. To prepare old
silk for use as a repair material it is washed, dried by stretch-
ing on a wooden or lacquered surface, brushed with jiao shui
(a cow skin glue) if needed and finally coloured by brushing
42 | Vincent Daniels, Marei Hacke, Jin Xian Qiu and Valentina Marabini
on natural pigments in a jiao shui binder until the desired hue
is reached.
Traditionally in China, if an old repair silk remains too
strong or too dark for the painting to be treated, potassium
permanganate solution is used to weaken it further and also to
lighten its colour. The degree of weakening increases with the
duration of the silks immersion in potassium permanganate,
which is followed by immersion in oxalic acid (an oxidation-
reduction process). Scroll mounters at the Shanghai Museum
are instructed in the long-established use of potassium
permanganate for bleaching and weakening silk for use in
scroll repair. No published accounts of these treatments on silk
appear to exist and it was at the instigation of the conservators
at the British Museum responsible for Chinese paintings who
are led by a master mounter previously trained at the Shanghai
Museum (JXQ) that the research reported here was initiated.
Chinese paintings, normally in the form of hanging or
hand scrolls, are surrounded by decorative silk mounts and
lined with several layers of paper. A Chinese silk painting with
missing substrate areas can only be repaired as part of a full
remount, Figure 2. The repair technique requires the removal
of the backing and lining paper layers from the painting to
allow access to the back of the painted silk. After disassembling
the painting from its surrounding silk mount, it is first wetted
and washed from the front and, depending on the degree of
water-soluble discolouration in the silk, this process is repeated
Figure 2. Hanging scroll painting of Plum Blossom (1952,1108,0.9) in the style of Chen Jiru (15881639: Ming Dynasty) before
and after conservation in 2012. The repairs using naturally aged repair silk were executed as part of the remounting process

A traditional Chinese method for weakening silk for use in the conservation of silk paintings | 43
Figure 3. Detail of the model silk scroll being repaired from the verso: (a) cutting the repair silk to shape; (b) applying wheat starch paste
to the edge of the missing area; (c) paring down the edge of the silk repair patch; and (d) drying the repair
several times. The painting is then faced with tung oil paper,
a specially treated paper that releases easily when wet. This is
adhered to the recto (front) of the painting with a thin layer
of wheat starch paste, which at the British Museum is mixed
with funori (hai cai in Chinese), a type of seaweed known for its
stability and good working properties that is commonly used
in Japanese paintings conservation [1]. This facing layer is
further secured with two or more layers of Chinese xuan paper
adhered with wheat starch paste so that the painting can be
inverted and then firmly secured onto a table with its backing
exposed. Whilst this layered assemblage is still wet and the
adhesives softened, the previous linings, which usually com-
prise three to five layers, are carefully removed with tweezers
until the verso (back) of the paintings silk substrate is exposed.
Once dry, the repair process can begin, Figure 3.
From the back of the painting, the area of loss can be assessed,
dry-cleaned, and a slightly larger piece of the selected repair silk
than is strictly necessary is positioned so the orientation of the
weave corresponds to that of the original. Diluted wheat starch
paste is applied generously along the perimeter of the loss and
the repair silk is cut with scissors to the correct shape and size
overlapping the loss by 34 mm. Extra paste is applied with a
thin brush to strengthen the repair locally (the entire verso will
later be covered in paste during the application of the new lining
papers). No pressing is required and the repairs are left to dry in
air from the rear, since the painting is still secured to the table
through the tung oil paper and xuan paper facings. When fully
dried, the overlapping edges of the repairs are pared down with
great care and precision using a thin blade, taking the utmost
care not to damage the original silk at the join.
Tears in a painting are treated differently; a strip of thin,
natural, undyed silk of an open weave is secured to the back
of the tear with dilute wheat starch paste applied with a
thin brush, Figure 4. Later in the conservation process, after
44 | Vincent Daniels, Marei Hacke, Jin Xian Qiu and Valentina Marabini
the painting has been completely relined and the facings
removed, the recto is again revealed. At this stage, while the
painting is stretched on a drying board, additional toning of
the silk repairs can be undertaken using traditional Chinese
natural pigments.
Silk
The vast majority of cultivated silk is reeled from the cocoons
of the domesticated silkworm Bombyx mori. The posterior
glands of the larvae simultaneously produce two continu-
ous filaments made of a protein called fibroin. The filaments
are approximately triangular in cross-section and are bound
together by the proteinaceous gum sericin, which is often
removed by degumming in a hot alkaline solution to separate
the silk into fine and lustrous fibres.
Degradational changes in old silk fibres can be attributed
to both hydrolytic and oxidative reactions, which lead to a
reduction of elongation and losses in tensile strength and elas-
ticity, i.e. embrittlement [2]. Silk is vulnerable to degradation
by light exposure, in particular ultraviolet (UV) light. Such
photo-oxidation leads to the yellowing and weakening of silk.
Initial degradative breakdown is thought to be due to the
cleaving of hydrogen bonds, which is followed by oxidation of
side chain amino acids, in particular tyrosine, and the eventual
scission of the polypeptide chain at the CN position and
at the tyrosine residues [3]. The oxidative degradation of
the amino acids tyrosine and tryptophan is believed to cause
yellowing in silk [3].
Dark storage and display under low light levels with UV
filtration are now standard practices for the preservation of
silk in museum collections. Recent investigations suggest that
high ambient relative humidity (RH) levels also promote the
degradation of silk and recommend drier conditions, in the
range 3050% RH [4].
Use of potassium permanganate in conservation
Potassium permanganate is a powerful oxidizing agent that
is routinely used in chemical synthesis and analysis. As an
oxidant it becomes more effective with increasing concentra-
tion and/or temperature. It is generally used in acid conditions
to avoid the formation of black manganese dioxide, which is
precipitated when oxidation is carried out in neutral or alka-
line conditions.
In the conservation of pictorial art on paper and silk,
bleaches are sometimes used for the removal of stains of
an organic nature. There are several oxidizing bleaches in
use, including neutral potassium permanganate solution.
Plenderleith and Werner described the technique as a last
resort, as it is definitely deleterious to the paper; at the same
time it rarely fails [5]. They recommended the use of a 0.5%
(0.0316 M) solution brushed onto the paper and left for five
minutes, after which the paper is treated with a 2% solution
of oxalic acid. One of the disadvantages of potassium per-
manganate as a conservation treatment is the extremely strong
purple colour of the solution and the intense black deposit of
manganese dioxide formed in the paper during the first stage
Figure 4. Detail of verso of the Plum Blossom painting seen in Figure
of the treatment, which makes it impossible to see how the
2, showing tears that have been repaired with open-weave silk
bleaching of stains is progressing. In the above method, the before relining. Scale bar shows 5 mm divisions
black colour is discharged by the oxalic acid, but other reagents
can be used to reduce the black water-insoluble manganese
dioxide (containing Mn4+) to the pale pink and water-soluble light (1064 nm) for very short periods could weaken silk to
manganese sulphate (containing Mn2+), including sodium produce the desired results. Although laser treatment caused
metabisulphite. The final stage of the process is thorough the fibres to tear and frayed holes of a few millimetres diameter
washing of the paper to eliminate all traces of manganese to develop in the textile, no weakening of the individual fibres
compounds that might otherwise cause accelerated deteriora- was evident, and the technique was judged unsuccessful [10].
tion of the paper; manganese is a transition metal of variable Nilson et al. experimented with thermal and UV ageing,
oxidation state that can act as a catalyst for oxidation [6]. storage in solutions with various pHs and exposure to environ-
The effect of residual manganese has been seen in previously ments with different RHs. They compared the results with
permanganate-bleached prints when, in subsequent oxidative naturally aged silk using spectroscopic and chromatographic
bleaching (with chlorine dioxide), they turn brown. techniques and tensile testing [11]. They concluded that
thermal ageing at 125C produced artificially aged silk most
Artificial weakening of silk: previous work similar to naturally aged silk, although they did not comment
Approaches for the production of artificially weakened silk for on the hue of the product.
conservation purposes were examined in the British Museum
in 1993 [7]. Repair silks weakened by treatment with gamma Experimental and results
rays and electron beams are used in Japan for the conserva- Further details are given in the experimental appendix.
tion of silk paintings [8, 9]. However, silk aged in this way
was not readily available in the UK. Accordingly, other more Potassium permanganate treatment
accessible methods were tested to determine whether a com- Weakening in potassium permanganate was performed by
parable product could be made. The methods tried were of immersing the silk in an aqueous solution. In the 1993 study,
two main types: (a) those that introduced energy into the silk the use of a 0.02 M solution led to inadequate weakening so
to accelerate degradation, e.g. exposure to UV or visible light in these experiments two more concentrated solutions (0.1 M
(photodegradation) and storage at temperatures between 100 and 0.05 M) were made by dissolving potassium permanga-
and 150C (thermal degradation); and (b) chemical degrada- nate in deionized water (15.804 and 7.902 g.L1 respectively)
tion by acid, alkali or oxidizing agents, e.g. sulphuric acid, [7]. After the test silk had been immersed in the solution for
hydrochloric acid, nitric acid, sodium hydroxide and potassium one hour, it was removed and washed in water. The silk, now
permanganate. Of all the methods tested only the product of coloured black with manganese dioxide, was next immersed
heat ageing was acceptably weak and brittle, but the initially in a reducing agent and then removed when the black colour
colourless silk became yellow. As the unwanted colour could had been completely discharged (after c.60 seconds). The silk
only partially be bleached out with alkaline hydrogen peroxide, was then washed in water and left in a bath of water for 30
the product was not considered suitable for use due to these minutes before air drying.
potential difficulties with colour matching. The reaction between oxalic acid and potassium perman-
More recently, the availability in the British Museum of a ganate is well known to chemists, as oxalic acid is used to
laser used for conservation cleaning purposes prompted an determine the strength of potassium permanganate solution
investigation of whether exposure to high levels of infrared by titration [12]. However, the reaction is slow at room

A traditional Chinese method for weakening silk for use in the conservation of silk paintings | 45
 Figure 5. EDX spectra of silk that has been treated with 0.05 M potassium permanganate and reduced with acidified hydrogen
peroxide, sodium metabisulphite or sodium dithionite to remove the precipitated manganese dioxide; see the manganese
peak at 5.9 keV
temperature and needs to be heated to 70C to proceed at a
convenient rate, thus it was decided that three other reducing
agents that reacted more rapidly at ambient temperature
would be tested, namely:
1. 10 volume hydrogen peroxide containing 1% volume/
volume sulphuric acid;
2. 1% sodium dithionite (a fresh solution was used as the
reagent reacts with oxygen);
3. 2% sodium metabisulphite.
All three reducing agents were visually effective at discharging
the black colour.
Determination of residual manganese
Silk has an affinity for metal cations, which is the basis for
the use of metal-containing mordants when dyeing silk with
natural dyes. Metal complexes may form by interaction with
the nitrogen, oxygen or sulphur atoms in the main or side
chains of the protein [13]. Shimizu showed that the metal
cations were adsorbed onto the silk and formed ionic bonds
with terminal carboxylic groups and that, with increasing pH,
terminal amino groups also became adsorption sites [14].
The retention of manganese ions by the silk is thus a
strong possibility and could, if it occurred, lead to unwanted
oxidative damage in the longer term. The preferred reducing
agent was, therefore, the reagent that left the smallest residual
manganese content. The silk was analysed for manganese
in a variable pressure scanning electron microscope using
energy dispersive X-ray microanalysis (VP-SEM-EDX).
The black silk containing manganese dioxide was analysed
as well as the samples that had been treated with the three
reducing agents. An EDX spectrum for the permanganate-
treated silk displayed a strong manganese signal, while any
residual manganese was undetectable in the spectrum for
the silk after the acid peroxide treatment had been applied.
The spectra for the silk samples treated with dithionite and
metabisulphite had manganese peaks above the background
46 | Vincent Daniels, Marei Hacke, Jin Xian Qiu and Valentina Marabini
level, Figure 5. As a result, the acid peroxide treatment was
chosen as the most successful reducing agent and applied in
subsequent experiments.
Tensile tests
The averaged results from tensile strength measurements with
an Instron 4411 tensile tester are shown in Table 1 and details
of the procedure are given in the experimental appendix. It
can be seen that increasing exposure time decreases the tensile
strength, and that the stronger the permanganate solution the
greater the extent of degradation. Treatment in a 0.1 M per-
manganate solution at 40C for 60 minutes produced silk with
a tensile strength of 1.83 N. Using higher temperatures would
be expected to produce weaker silk more rapidly but, as the
desired weakness can be obtained by treatment at or near
room temperature, there seems little advantage in elevating
the temperature.
VP-SEM examination showed that the permanganate
treatment caused the fibres to become brittle and a few broken
fibres could be seen as evidence of this, Figure 6.
Colour reversion tests
A subsequent visible colour change of silk infills would be
detrimental to the appearance of the conserved silk scroll
paintings. It was also important, therefore, to establish
whether the treated silk would discolour over time and accel-
erated ageing tests were used to predict the effects of ageing.
Generally, the most accurate tests use elevated temperatures
or illumination to increase the rate of the chemical reactions
that occur during ageing, but some approaches to accelerated
ageing also simulate the influence of other factors responsi-
ble for degradation, such as altered levels of humidity or air
pollutants. Details of the two methods applied in these experi-
ments (light ageing and combined heat and humidity ageing)
are given in the experimental appendix.
During conservation treatments, silks for the repair of
paintings are coloured by surface application of pigments
 Figure 6. SEM image of unreduced, potassium permanganate-treated, degummed silk. The broken
fibres are indicative of the weakened nature of the silk
suspended in a solution of animal glue, known in Japan as
nikawa and in China as jiao shui. Accordingly, colour change
on ageing was measured not only on the treated silk but also
on treated silk that had been sized and painted to match the
type of old silk that might need to be repaired.
The control samples and the samples that were exposed
to accelerated ageing for eight weeks are shown together
in Figure 7 and their reflectance spectra are presented in
Figures 8 and 9. It is evident that heat and humidity ageing
led to a greater colour change than light ageing under the
conditions used. Generally, light ageing caused bleaching
(an increase in reflectance) while heat and humidity ageing
caused darkening and yellowing (an overall decrease in
reflectance and greater absorption in the blue region of the
visible spectrum, at 400500 nm). The colour change for the
pigmented samples was generally less severe than the colour
change for the non-pigmented samples, indicating that the
pigments used are relatively stable or are capable of masking
the bleaching, darkening and yellowing effects of accelerated
ageing to some extent. For the non-pigmented samples it
was apparent that the chemically weakened silk changed to
a greater extent than the untreated silk. This colour change
is greatest at the beginning of the ageing period and then
decreases during the course of the light ageing experiment
until the spectra are nearly unchanged between measure-
ments, Figure 8. An anomaly during heat and humidity
ageing (explained in the experimental appendix) led to a
lower rate of deterioration during the first two weeks, but
it can nevertheless be seen that the colour change after four
weeks is significant and that while colour changes are still
occurring after six and eight weeks, the rate of change is
not as great. No statistically significant colour change was
detected for any of the control samples during the eight-
week period in ambient dark conditions. The weakened
A traditional Chinese method for weakening silk for use in the conservation of silk paintings | 47
undyed control sample was measured again after 14 and
39 weeks and no change was detected within the limits of
experimental error.
Evaluation of the new repair silk
To evaluate the working properties of this artificially aged
silk a test model was produced. A piece of new plain-weave
silk was cut into two parts: one part to represent an old silk
painting substrate and the other to act as the repair silk. Both
parts of the new silk were first washed in boiling water then
weakened by the permanganate method. When dry, the silk
to be used for repairs was placed on a table surface where
it was sized by brushing with a jiao shui and alum solution
(jiao fan shui). In this case a solution of 1% jiao shui and 0.1%
alum (hydrated aluminium potassium sulphate) was used. This
solution was applied a number of times until the silk became
waterproof; the weave of the silk was then aligned for drying
and stretching. The resulting silk was more rigid, allowing it
to be handled more easily during the repair process. The silk
was finally coloured by brush with natural pigments dispersed
in water with a jiao shui binder and left to dry on the table with
the threads aligned.
The piece of silk representing the original painting was
lined with xuan paper using wheat starch paste to resemble
a lined painting. When dry, the lined silk was brushed once
with a jiao shui and alum solution and left to dry stretched on
a table surface with the weave aligned. The silk representing
the painting was coloured with natural Chinese pigments
and dried as above. Many holes were deliberately made in
the silk to represent damage and to provide opportunities to
practise repairs.
The lined silk was then treated as if it were a painting;
it was washed, faced, had its lining removed, as detailed
above, and was repaired in places with the prepared silk. By
Table 1. Tensile test results for weakened silk samples
with standard deviations in square brackets
Sample
Silk as supplied
Degummed silk
Treated with 0.05 M KMnO4 for 30 minutes
Treated with 0.05 M KMnO4 for 60 minutes
Treated with 0.05 M KMnO4 for 90 minutes
Treated with 0.1 M KMnO4 for 30 minutes
Treated with 0.1 M KMnO4 for 60 minutes
Treated with 0.1 M KMnO4 for 90 minutes
practising the silk repair technique normally applied on scrolls
using specially produced models, the handling properties of
the artificially weakened silk were tested and differences in
Tensile test
results (N) surface texture and touch were compared with that of old
83.1 [5.4] silk. The working properties of the newly weakened silk were
75.7 [12.3]
found to be very similar to those of naturally aged silks and,
aesthetically, the results were also considered successful by
20.0 [1.9]
the conservators of Chinese silk paintings at the British
5.1 [1.4]
Museum (JXQ and VM). Although old silk repair patches
2.6 [0.1]
can be coloured without the need for sizing, the artificially
6.2 [2.2]
weakened silk requires sizing. Both naturally old silk and
2.5 (0.8) artificially weakened silk fibres are darker at the surface, and
2.0 (0.4) the lighter interior is revealed if the silk is pared down at the

Figure 7. Silk samples after eight weeks of natural and accelerated ageing

48 | Vincent Daniels, Marei Hacke, Jin Xian Qiu and Valentina Marabini
Figure 8. Reflectance spectra showing colour changes for untreated and weakened uncoloured
silk samples

Figure 9. Reflectance spectra showing colour changes for untreated and weakened pigmented
silk samples

A traditional Chinese method for weakening silk for use in the conservation of silk paintings | 49
overlap of the repair patch and the object. The difference in
hue is slightly greater for the permanganate-treated silk but
is hardly noticeable, especially as the paring is performed on
the back of the painting.
Conclusions
Chemically weakened silk was prepared by oxidizing it in
potassium permanganate solution. During the process manga-
nese dioxide is formed in the silk. Three methods were tested
for removing these manganese-containing residues from the
silk and a method that used acidified hydrogen peroxide was
most successful. Elemental analysis in the VP-SEM showed
no detectable manganese in the final product.
The weakened silk was tested for its colour stability during
light or heat ageing. Results showed that the chemically weak-
ened silk was more prone to discolouration than the untreated
silk; discolouration took the form of bleaching during light
ageing and darkening/yellowing during thermal ageing.
However, once coloured by the application of pigment, the
difference in discolouration between the chemically weakened
and untreated samples was less obvious, indicating that the
pigments are relatively stable and to some extent mask the
discolouration of the silk itself. The colour changes shown by
the freshly prepared samples were greatest at the beginning
of the ageing periods and then decreased until they became
very small. The change of hue may be caused by chemical
changes occurring in compounds formed during the oxidation.
Rather than prepare a fresh piece of chemically weakened silk
for each treatment, a better alternative would be to prepare
and store batches of silk in the studio to ensure that exposure
to studio lighting naturally ages the repair silks before they are
needed for treatment.
Conservation assessment showed the working properties of
weakened silk to be very similar to those of genuinely old silk.
To facilitate colour matching with pigments in jiao shui solution,
sizing with jiao shui and alum was needed.
Experimental appendix
Silk textile
The silk used for the experiments was specially made in
China for use in scroll repair. It was the product of a col-
laboration between the Shenyang Palace Museum, Nanjing
Museum, Beijing Palace Museum and Shanghai Museum.
In this project 28 different types of silk textile were manu-
factured. Outside China, the British Museum and the Freer
Gallery of Art in Washington DC also received lengths of
this silk. Only one type of silk was used in this experimental
work: a plain weave with a weight of 42 g.m2 that is suitable
for use in silk painting.
Degumming
To determine whether or not the silk was gummed it was ana-
lysed using a method described by Carboni [15]; the method
removes the sericin and leaves behind the fibroin. A weighed
sample was soaked overnight in 0.5% sodium hydroxide then
washed in cold water on the following day. The sample was
next boiled twice in distilled water for 30 minutes, dried and
reweighed. A mass loss of 22.8% was obtained, which is con-
sistent with the mass loss expected for gummed silk (2025%).
50 | Vincent Daniels, Marei Hacke, Jin Xian Qiu and Valentina Marabini
This compared to a mass loss of only 2.8% when the silk was
not treated with alkali but only boiled in distilled water. The
results indicated that the silk was gummed.
VP-SEM-EDX
VP-SEM-EDX was carried out using a Hitachi S3700N vari-
able pressure SEM and the backscatter electron detector. The
chamber pressure was 30 Pa and the samples were analysed at
a working distance of 10 mm. The accelerating voltage was
20 kV. EDX spectra were collected for 200 s live time.
Tensile tests
Strips of silk were cut with scissors so that the warp was par-
allel to the long direction of the strip. The strips were tested
for tensile strength on an Instron 4411 with a 100 N load
cell. The distance between the jaws of the grips was 50 mm
and the extension rate was 20 mm per minute. Because of
the large variations in strength between the differently treated
experimental samples it was sufficient to test only three repeat
samples of each type of silk.
Producing samples for colour reversion tests
It was decided to permanganate-treat the silk as purchased,
rather than after a separate degumming step, as it was
thought unlikely that most users would use this extra step. In
addition, it was considered prudent to test the colour rever-
sion on weakened silk that may have retained some of its
gum, as this was expected to exacerbate the effect of colour
reversion, i.e. colour reversion of degummed silk should be
smaller than the colour reversion of silk with its gum, pro-
vided the degumming process does not adversely affect the
stability on ageing. Samples of the silk were treated at room
temperature for one hour in 0.1 M potassium permanga-
nate solution (7.9 g KMnO4 dissolved in 500 mL deionized
water overnight). The silk, coloured black with manganese
dioxide, was then immersed for a few minutes in 10 volume
hydrogen peroxide containing 1% sulphuric acid until the
textile turned white. The silk was then washed in a stream
of deionized water and soaked for two days in a deionized
water bath before drying.
Colouring silk for colour reversion tests
Three dilute applications of paint were made to the silk using
each of the following traditional materials bound in jiao shui:
Chinese carbon black ink; indigo; gamboge resin; and iron
oxide red.
Accelerated ageing for colour reversion tests
A set of the four samples (untreated, untreated coloured,
weakened and weakened coloured) was exposed to an arti-
ficial daylight spectrum in a light box equipped with Osram
Lumilux Delux L 18 W/930 fluorescent lamps emitting
approximately 16000 lux and virtually no UV (1 W.lumen1).
The total exposure time of eight weeks is equivalent to 21.5
Mlux hours, which equates to approximately 150 years of
display conditions, assuming 50 lux, eight hours per day, seven
days per week.
Another set of the four samples was suspended in a desic-
cator over a small amount of water so that the RH around
the samples would be elevated. The desiccator was placed in
an oven at 60C for eight weeks. Unfortunately a leak in the
desiccator seal led to evaporation of the water at some point
during the first two weeks of ageing. This was corrected for
subsequent ageing periods and the desiccator seal remained
intact between weeks two and eight. Equating accelerated
ageing time to real time for heat ageing depends on too many
variables and was not attempted here.
Colour measurements for colour reversion tests
Colour measurements before and after accelerated ageing were
performed using a Minolta CM-2600d spectrophotometer and
SpectraMagic 3.7.0.OG software. The instrumental settings
were as follows: SAV (small aperture), UV energy included,
specular component excluded, 10 observer and D65 illumi-
nant. The results reported here are averages of measurements
from five random locations, avoiding areas with obvious stains
or uneven discolouration.
Health and safety and other practical considerations
The process for preparing artificially weakened silk is moder-
ately safe, but hydrogen peroxide and potassium permanganate
are both strong oxidizing agents and appropriate protective
measures must be taken, particularly with the undiluted rea-
gents. While 10 volume hydrogen peroxide and potassium
permanganate solutions are used in the silk weakening method
described, 100 volume hydrogen peroxide and solid potas-
sium permanganate are the forms usually purchased; these
must not be mixed as the ensuing reaction is hazardous. The
effervescence of oxygen produced when hydrogen peroxide
makes contact with the blackened silk may produce a spray
of fine droplets of acidified hydrogen peroxide; this part of
the process should be carried out in a fume cupboard so that
the spray is not inhaled and does not make contact with other
oxidizable material.
Potassium permanganate solutions are prepared by dis-
solving potassium permanganate crystals in water. However,
dissolution can be slow and care must be taken if solutions of
the calculated strength are to be prepared as the intense purple
of the resulting solution makes it difficult to see undissolved
crystals. On storage, the solution stains glassware brown but
this can be removed by washing with the acidified hydrogen
peroxide solution described above.
Acknowledgements
The authors wish to acknowledge with thanks Mr Quxing Yu (Direc-
tor) and Mr Feng Yao Geng (Head of Conservation) of the Shanghai
Museum for enabling the British Museum to obtain the Chinese repair
silks that are the subject of this paper. They also thank Carol Peacock
for help with writing this article and Michelle Hercules for performing
the laser tests. Finally, helpful discussions with Joanna Kosek and Keisuke
Sugiyama are gratefully acknowledged.
A traditional Chinese method for weakening silk for use in the conservation of silk paintings | 51
Authors
Vincent Daniels (vdaniels@thebritishmuseum.ac.uk) is an emeritus
researcher, Marei Hacke (mhacke@thebritishmuseum.ac.uk) a
scientist, and Jin Xian Qiu and Valentina Marabini (vmarabini@
thebritishmuseum.ac.uk) are conservators, all in the Department of
Conservation and Scientific Research at the British Museum.
References
1. Michel, F., Funori and JunFunori: two related consolidants with
surprising properties, in Adhesives and consolidants for conservation: research
and applications, www.cci-icc.gc.ca/symposium/2011/index-eng.aspx
(accessed 6 May 2013).
2. Kuruppillai, R.V., Hersh, S.P. and Tucker, P.A., Degradation of silk
by heat and light, in Historic textile and paper materials, ed. H.L. Needles
and S.H. Zeronian, American Chemical Society, Washington DC
(1986) 111127.
3. Robson, R.M., Silk: composition, structure, and properties, in
Handbook of fibre chemistry, ed. E.M. Pearce, Marcel Dekker Inc., New
York (1998) 415464.
4. Luxford, N., Silk durability and degradation, in Understanding and
improving the durability of textiles, ed. P.A. Annis, Woodhead Publishing,
Cambridge (2012) 205232.
5. Plenderleith, H.J. and Werner, A.E., The conservation of antiquities and
works of art, Oxford University Press, Oxford (1971).
6. Daniels, V., Aging of paper and pigments containing iron and copper:
a review, in The broad spectrum: studies in the materials, techniques, and
conservation of color on paper, ed. H.K. Stratis and B. Salvesen, Archetype
Publications, London (2002) 116121.
7. Daniels, V., Production of artificially aged silk for conservation,
Department of Conservation and Scientific Research report 1993/15, British
Museum (1993) (unpublished).
8. Keisuke Sugiyama, conservator of pictorial art, British Museum,
personal communication (March 2013).
9. Kawanobe, W., The role of science in the restoration of Japanese
painting, in Restoration of Japanese paintings, 33rd International Symposium
on the Conservation and Restoration of Cultural Properties, ed M. Kato and
K. Yamaguchi, Tokyo Bunkazai Kenkyujo, Tokyo (2011) E-31E-38.
10. Daniels, V., Hacke, M., Marabini, V. and Kosek, J., Production of
aged silk for conservation purposes, Department of Conservation and
Scientific Research Project 7483, British Museum (2010) (unpublished).
11. Nilson, J., Vilplana, F., Karisson, S., Bjurman, J. and Iverson, T., The
validation of artificial aging methods for silk textiles using markers for
chemical and physical properties of seventeenth-century silk, Studies
in Conservation 55 (2010) 5565.
12. Jeffery, G.H., Bassett, J., Mendham, J. and Denny, R.C., Vogels
textbook of quantitative chemical analysis, 5th edn, Longmans Scientific
and Technical, Harlow (1989) 66.
13. Hojo, N. and Shirai, H., Metal complexes of silk protein, in Structure
of silk yarn. Part B: Chemical structure and processing of silk yarn, ed. N. Hojo
and D. Mahadevappa, Science Publishers, Enfield NH (2000) 135157.
14. Shimizu, F., Adsorption behaviour of metal ions on silk and their
effect on the photo-degradation of the silk, in Structure of silk yarn.
Part B: Chemical structure and processing of silk yarn, ed. N. Hojo and D.
Mahadevappa, Science Publishers, Enfield NH (2000) 159172.
15. Carboni, P., Tests on the raw silk, in Silk, translated by K. Walter,
Chapman and Hall, London (1952) 111159.