1. NOVEMBER 2010
MAGAZINE OF THE ROYAL AUSTRALIAN CHEMICAL INSTITUTE INC.
Ancient culture at the Australian Synchrotron
Women and the research culture
Travels with a titrator

2. Most of us will admit to having been buried in our
work at some time. But if you were a servant to
the ancient Egyptian nobility, circa 3000 BCE, you
might literally have been buried alive with your master
or mistress when they died. The aim was to ensure that
pharaohs and other members of the nobility would not
have to do any menial work in the afterlife, something
many of us still aspire to.
History is unclear on how long the practice lasted,
but it may have been phased out as a matter of
commonsense. After all, why waste a perfectly good
servant? Much better to paint their likenesses on the
tomb walls, or build a servant to take care of you.
The small statuettes found in tombs dating from
later periods of ancient Egypt circa 2000–340 BCE
ultimately performed this function, working as personal
slaves or undertaking manual labour on behalf of the
deceased. Called shabti, the figurines were initially
intended to provide a home for the dead person’s ka or
life-force.
Made from clay, limestone, wood or Egyptian faience
(sometimes known as synthetic turquoise), shabtis were
often equipped with farming or fishing implements and
exquisitely glazed or painted. At their peak, shabtis were
found in all but the poorest of graves. One tomb is
recorded as having one for every day of the year – with
20 NOVEMBER 2010
Something old, something new
Ancient culture at the Australian Synchrotron
NANCY MILLS
Ancient Egyptian artefacts have long been a subject of fascination. We can’t ask their
long!dead creators how they were made, but the Australian Synchrotron is the next
best thing, providing new insights into the chemistry of ancient cultural items.
Intended to serve as
personal slaves in the
afterlife, these Egyptian
shabti were made from
a quartz!based ceramic
material called faience.
Image credit:
Nancy Mills.

3. ten overseer shabtis to keep order. Not surprisingly, the
little figurines now feature in distinguished museum
collections around the world.
Something borrowed, something blue
Several faience shabti recently found their way into the
hands of La Trobe University archaeologist Mark Eccle-
ston, on loan from the Ian Potter Museum of Art at the
University of Melbourne. Mark is using the Australian
Synchrotron as part of an ongoing investigation into the
production of Egyptian faience, a quartz-based ceramic
material with a vitrified blue-green surface glaze. Called
tjehenet (‘that which is brilliant or scintillating’) by the
Egyptians (Nicholson 2009), the material was dubbed
‘faience’ by early European travellers, who saw similari-
ties with a type of late-mediaeval, tin-glazed pottery
from Faenza in northern Italy.
Described as ‘the first high-tech ceramic’ (Nicholson
2009), faience is essentially a reconstituted stone that
was independently discovered in Egypt, the Near East,
the Aegean and some parts of Europe. The main ingre-
dients are silica (SiO2), lime (CaO) and an alkali such as
natron, a naturally occurring salt consisting of sodium
carbonate and sodium bicarbonate that was used in the
mummification process. During firing, the lime and
soda in the faience mixture react with the silica to form
a small amount of glass that binds the silica grains.
The faience mixture was moulded or shaped by
hand, but the material was thixotropic (subject to
changes in viscosity) and details were often lost from
the final product. Adding natron or plant ash as alkali
binders made the faience easier to work with. The
colour of the faience varied according to the ingredients
and the methods used to work the material.
Mark’s interest in faience is related to his ongoing
investigation of the use of metals in ancient Egypt
during the New Kingdom (from around 1500 to
1100 BCE), primarily copper and copper alloys such as
bronze. The characteristic blue-green colours of faience
were created by adding copper, but whether this was
added to the mix as copper metal or an alloy such as
bronze, or derived from oxides or other minerals is not
known. Manganese, possibly as the oxide, was used to
add black details such as hieroglyphs.
An important trade item, Egyptian faience was
mainly used for small objects such as amulets, rings and
beads. It was often mass-produced in factories, but some
items were apparently made in large domestic bread
ovens. Mark believes this may mean that women made a
bigger contribution to local industries such as faience
and metals than previously thought.
The metal-working and faience industries were
sometimes located together, and Mark would like to
know how the production facilities were organised and
what raw materials they used. As well as illuminating
our knowledge of faience production, identifying the
raw materials would provide insights into the micro-
economic behaviour of individuals and groups involved
in making and trading faience, raw materials trading and
distribution in the wider economy and the organisation
of trade activities within wider city life. Knowing which
forms of copper and other raw materials were used in
the production process would tell us something about
how these materials might have been acquired by the
people who made the faience. For example, were the raw
materials readily obtained or was state input needed for
access to ‘special’ or ‘controlled’ materials?
Mark demonstrated the production of faience in a
replica 1300 BCE wood-fired bread oven (Eccleston
2008) during the 2008 excavation season at Amarna, an
archaeological site on the east bank of the Nile River
about 300 kilometres south of Cairo. Occupied for just
two or three decades, Amarna is a unique time capsule
of life at around 1350 BCE.
He made the faience from a mixture of powdered
quartz, ball clay, gum Arabic, soda ash, crushed lime-
21NOVEMBER 2010
Egyptian faience made in 2008 to an ancient recipe.
Image credit: Mark Eccleston.

4. 22 NOVEMBER 2010
stone and copper oxide. The faience items were placed
on a bed of quartz pebbles and pottery sherds, and the
oven was held above 800°C for an hour before being
allowed to cool naturally. The firing process weakened
the quartz pebbles so much that they could easily be
crushed to a fine powder and used as raw material for
further batches of faience.
In collaboration with La Trobe University physicist
Peter Kappen, Mark is now putting a series of blue-
green faience-glazed objects to the test at synchrotrons
in Australia and Germany.
Mark and Peter are using the X-ray absorption spec-
troscopy (XAS) and powder diffraction beamlines at
the Australian Synchrotron with additional XAS
studies at HASYLAB (the Hamburg synchrotron radia-
tion laboratory) in Germany. They have also used the
Australian facility’s macromolecular crystallography
beamline to examine faience beads.
The XAS work helped identify the chemical form of
the copper present in the glaze, while the powder
diffraction work showed that the material did not
contain any copper minerals. This raises interesting
questions about the change in structure of the copper
within the glaze as it is fired, and highlights the need for
combining the results of various techniques to under-
stand how faience may have been made. Further experi-
ments are planned using laboratory-made faience
prepared according to known recipes in order to create a
database that will enable researchers to ‘reverse engineer’
the production process and determine the raw materials
used in antiquity.
Overall, the synchrotron results have improved the
collaborators’ knowledge of the structure of faience and
enabled them to ask more-probing questions. The next
phase of the research will involve much closer examina-
tion of the atomic near-range order and structure of
copper within the faience matrix and of the possibility
that the copper is distributed through the amorphous
glassy phase of the glaze as nanoparticles. Mark expects
that the results will help him identify raw materials
likely to have been used to colour the objects. The pair
has also demonstrated the value of synchrotrons for
examining whole objects, which is a very useful result
for further work with museum collections.
Old ...
Less than a century after
celebrated Australian
artist Arthur Streeton
painted his own portrait
at the height of his career,
a new collaboration
between art and science
has revealed details of a
hidden Streeton self-
portrait, also painted in
the early 1920s. David
Thurrowgood from the
National Gallery of
Victoria and Deborah
Lau from CSIRO used the Australian Synchrotron’s
X-ray fluorescence microprobe (XFM) beamline to
examine the Streeton work, with permission from the
artist’s grandson.
Synchrotron techniques are ideal for examining
works of art because they are non-destructive and can
rapidly provide detailed chemical information. The
XFM beamline can scan an entire canvas section by
section, analysing the chemical composition of different
components and ‘fingerprinting’ the elements present in
different pigments.
The collaborative investigation will encourage
increased use of synchrotron techniques for studying
artists’ materials and methods, assisting restoration
work, and potentially providing new evidence in cases
where an artist’s identity is unclear.
Other Australian Synchrotron techniques used to
study works of art include infrared microspectroscopy
and X-ray powder diffraction.
... older ...
The infrared microscopy beamline at the Australian
Synchrotron is being used to help clarify the chemistry
of historic and cultural materials from the 19th and
20th centuries as well as much older materials from
Aboriginal rock art and Mayan paints and plasters.
Alana Treasure from the University of Canberra and
the Australian War Memorial is studying the mecha-
nisms by which corrosive iron gall inks degrade parch-
ment supports from the 19th and 20th centuries. The
work complements international studies of ink degrada-

5. tion on paper (cellulose) supports. Knowledge of these
mechanisms is assisting the development of conserva-
tion treatments to preserve documents and artworks
threatened by iron gall ink corrosion degradation in
collections worldwide, including the National Archives
of Australia. The degradation process is followed by
looking at changes in the amide group in the parchment
collagen.
Researchers from the University of Melbourne and
the Centre for Cultural Materials Conservation in
Melbourne have used the infrared microscopy beamline
to examine paint cross-sections from a late 19th century
commercial building, the Provincial Hotel in the
Melbourne suburb of Fitzroy (Sloggett et al. 2010). The
beamline’s five-micrometre spatial resolution enabled
the researchers to successfully analyse major and minor
components in the highly stratified paint cross-sections,
revealing details of all changes to the decorative facade
of the building and reflecting the history of paint tech-
nology from the 1880s to the 1950s. The group is also
involved in an international collaborative study of the
stability and ageing of 20th century paintings from
South East Asia and Northern Australia.
Researchers from Queensland University of Tech-
nology recently brought paint and stucco samples from
a Classic Maya site in Honduras to the infrared
microscopy beamline. They are keen to gain a better
understanding of plaster and painting techniques used
in the Maya culture, particularly the chemistry of some
pigments unique to Maya buildings. The group also
brought samples from an Aboriginal rock art site in
north Queensland, where the art is typically less than
20 micrometres thick, with the aim of better under-
standing the materials used by these people.
… oldest
Solar wind and stardust samples collected by NASA
spacecraft, including the Genesis mission, are probably
the oldest samples brought to the Australian Synchro-
tron so far. Back on an earthly plane, the oldest terres-
trial (okay, the oldest marine) object brought to the
Australian Synchrotron is a 380-million-year-old fossil.
The fossil in question is a small bone from a placo-
derm, an extinct armoured fish that was the first verte-
brate animal to possess jaws, pelvic and pectoral fins.
The Kimberley region of Western Australia is renowned
for its exceptionally well-preserved fossils. In early 2009,
another West Australian placoderm fossil caused
considerable scientific excitement when an international
research team realised it was evidence for sexual repro-
duction (aka internal fertilisation) – and for live births
around 200 million years earlier than had previously
been believed (Long et al. 2008). A fossil from New
South Wales, also a placoderm, has provided some of
the first definite fossil evidence of a forerunner to the
human eye (Young 2008).
The current keeper of the placoderm fossil brought
to the Australian Synchrotron is Catherine Boisvert
from the Australian Regenerative Medicine Institute, a
palaeontologist interested in all aspects of morpholog-
ical evolution. Working with Kate Trinajstic from
Curtin University of Technology, Catherine is looking
at pelvic evolution in the first jawed vertebrates.
Catherine brought the fossil to the Australian Synchro-
tron so that imaging and medical beamline staff could
test the capabilities of the computed tomography
component of the beamline. She plans to come back
again when the beamline’s phase contrast capabilities
are available later this year.
The synchrotron enabled the internal structure of
the bone to be seen without destroying the specimen.
This is essential when dealing with rare fossil materials.
Synchrotron computed tomography provides higher-
resolution images than laboratory-based X-ray sources.
23NOVEMBER 2010
The fossil remains of an extinct armoured fish are extending
our knowledge of evolution. Image credit: John Long (Long
1995).
Continued page 27

6. pyrotechnics; barium is used for green. As early as
1863 Lamy reported on the toxicity of thallium
(Lamy 1863).
Spectrum analysis was a very hot topic in the early
1860s. In March 1861, Roscoe presented a lecture to
the Royal Institution of Great Britain entitled ‘On
Bunsen and Kirchoff ’s spectrum observations’ (Roscoe
1861). In 1862, to the same Institution, Roscoe gave a
course of three lectures on the use of spectrum
analysis (Roscoe 1862). In 1861, William A. Miller,
Professor of Chemistry at King’s College London,
presented a lecture ‘The new method of spectrum
analysis’ to the British Association for the Advance-
ment of Science (Miller 1861). About six months
later, Miller presented a similar lecture before the
Pharmaceutical Society of Great Britain (Miller
1862). William Allen Miller (1817–70) (Clerke and
McConnell 2004) was an older brother of Francis
Bowyer Miller (1828–87) (Martin 2005), inventor of
the chlorine method (Miller process) for refining gold
that was featured in Part 5 of this series (August issue,
pp. 12–16).
Early Australian interest in spectrum
analysis
Given the tyranny of distance, and the youth of the
Australian Colonies, it is interesting that spectrum
analysis became the subject of three Australian papers
in the 1860s – two were read before the Royal Society
of Tasmania, and one was presented to the Philosoph-
ical Society of Queensland. These papers, and the
men responsible for them, will be dealt with in Part 7
of this series.
David J. Collins FRACI CChem <david.collins@sci.monash.edu.au> is an
Honorary Senior Research Fellow, School of Chemistry, Monash Univer!
sity, and Honorary Senior Fellow, School of Philosophy, Anthropology
and Social Enquiry, University of Melbourne.
* This chronicle is based on early entries in an electronic database,
‘Chemistry in Australia pre!1900’, recently completed by the author and
containing 1098 records. It highlights some of the earliest reports of
chemical studies communicated to scientific societies, and/or published
in scientific journals by chemists working in Australia. A list of publica!
tions referred to in this chronicle can be found at
www.raci.org.au/chemaust and further information on the database
can be obtained from the author.
† The complete 1860–1869 bibliography is available at
www.raci.org/chemaust, together with the additional references
(shown here in italics).
27NOVEMBER 2010
Phase-contrast X-ray imaging allows much greater
contrast from weakly absorbing materials such as soft
tissue than is possible by conventional methods.
Catherine is keen to continue collaborating with
beamline staff to develop soft tissue computed tomog-
raphy scanning methods for sharks and other fish to
gain high resolution 3D anatomical data.
REFERENCES
Eccleston M. 2008, Egyptian Archaeology 32, 33–5.
Long J.A. 1995, The rise of fishes: 500 million years of evolution. University
of New South Wales Press, Sydney; also John Hopkins University Press,
Baltimore, USA. 1995. 230pp. ISBN 0868400785.
Long J.A., Trinajstic K.M., Young G.C., Senden T. 2008, Nature 453, 651–3.
Nicholson P.T. 2009, Faience technology. In Willeke Wendrich (ed.), UCLA ency-
clopedia of egyptology, Los Angeles.
<http://escholarship.org/uc/item/9cs9x41z>
Sloggett R., Kyi C., Tse N., Tobin M.J., Puskar L., Best S.P. 2010, Vibrational Spec-
troscopy 53(1), 77–82.
Young G.C. 2008, Biology Letters 23(4), 110–14.
As a young teenager, Nancy Mills <nancy.mills@synchrotron.org.au>
wanted to be an archaeologist. She eventually chose chemistry, but man!
aged to combine the two when she worked with materials conservation
staff and maritime archaeologists at the WA Museum.
Continued from page 23
Coming up in December
• A natural offshore asset and its
challenges for chemistry
• Convicts, chemistry and
spectroscopes
• Climate change: short answers to
big questions
• RACI 2010 award winners