Journal of Archaeological Science 39 (2012) 2877e2887

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Journal of Archaeological Science

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Early Cambodian gold and silver from Prohear: composition, trace elements
and gilding
Sandra Schlosser a, *, Andreas Reinecke b, Roland Schwab a, Ernst Pernicka a, Seng Sonetra c, Vin Laychour c
a
Curt-Engelhorn-Centre for Archaeometry (CEZA) Mannheim, C 5 Zeughaus, 68159 Mannheim, Germany
b
Commission of Archaeology of Non-European Cultures of the German Archaeological Institute, Dürenstraße 35-37, 53173 Bonn, Germany
c
Memot Centre, Ministry of Culture and Fine Arts, Phnom Penh, Cambodia

a r t i c l e i n f o a b s t r a c t

Article history: Rescue excavations in Prohear, southeast Cambodia, recently saved the last untouched graves of one of
Received 5 August 2011 the richest prehistoric sites in Southeast Asia. Many Iron Age burials dating from the 2nd century BC to
Received in revised form the 1st century AD contained gold and silver ornaments so far unknown from archaeological contexts
21 March 2012
together with indications for the presence of an immigrated elite. A first selection of 59 objects were
Accepted 8 April 2012
analysed by LA-ICP-MS to obtain detailed information about the composition, as well as minor and trace
elements. The majority of the ornaments consist of electrum and auriferous silver with low copper
Keywords:
concentrations, and two main groups indicating different alluvial gold sources can be distinguished by
Prohear
Iron Age
different concentrations of Pt, Ir, Bi and different Pd/Pt ratios, one group being related to rich burials with
Pre Funan culture non-local features. The SEM and EDX analyses of four objects revealed two different gilding techniques
Cambodia observed for the first time in Southeast Asian artefacts: foil-fusion gilding, related to special AgeAue(Cu)
Southeast Asia eSn alloys containing up to 4% tin, and depletion gilding.
Gilding Ó 2012 Elsevier Ltd. All rights reserved.
Gold
Silver
Electrum
Trace elements
LA-ICP-MS

1. Introduction The site is assigned to the Pre-Funan culture, which is charac-

At Prohear in Prey Veng province in southeastern Cambodia
(Fig. 1), one of the richest prehistoric sites in Southeast Asia was
unearthed during three rescue excavations conducted from 2008 to
2011 by the German Archaeological Institute in cooperation with
the Memot Centre in Phnom Penh (Reinecke et al., 2009, in press).
The large Iron Age cemetery, situated in the centre of the Prohear
village, had been looted almost completely during 2007 and
probably contained more than 1000 precious metal ornaments and
unique bronze items. Nevertheless, 76 burials dating mainly from
the end of the 2nd century BC to the 1st century AD were excavated
in the area of the main road, where at least some of the graves had
remained intact.
* Corresponding author. Present address: c/o Commission of Archaeology of Non-
European Cultures of the German Archaeological Institute, Dürenstraße 35-37,
53173 Bonn, Germany.
E-mail address: schlosser.archaeomet@googlemail.com (S. Schlosser).
terised by inhumation burials with the dead placed on their back,
wrapped in a fibre mat with their clothes, ornaments and imple-
ments surrounded by a number of ceramic vessels. The burial
custom, head orientation, the arrangement of the offerings and the
pottery types link Prohear well to other known cemeteries of the
local Pre-Funan culture (Fig. 1). But in its second phase, to which
most of the burials belong, also other influences not typical for Pre-
Funan appear. For example, stone pestles or a bronze bell were
found between the thighs, and in the richest burials the head was
deposited in a bronze drum or covered by a bronze bowl. Further-
more, offerings like 33 Heger-I bronze drums in Dong Son style e
the majority just reported by looters, bronze dishes, bracelets with
buffalo-horn-shaped ends and certain stone beads have to be
considered as imported elite goods (Reinecke et al., 2009, in press).
The quantity of precious metal ornaments is quite outstanding,
compared to the finds from other Iron Age sites (Miksic, 2011:
40e42). A total number of 93 gold and silver objects were found in
32 of the burials, while three more gold pieces were recovered in
the excavation units and 16 objects from looted burials could be

0305-4403/$ e see front matter Ó 2012 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jas.2012.04.045
2878 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887

Fig. 1. Mainland Southeast Asia with important Iron Age sites (black dots) including Prohear and Bit Meas (black triangles) in southeastern Cambodia.

documented at least photographically. Most ornaments are simple
wire works like open rings, bracelets and small spirals, the latter
representing about half of the objects. Complete spirals show up to
10 coils, but mostly were found as fragments with broken or chisel
cut ends. Other ornaments comprise a pair of biconical earrings
adorned with granules at the edges (Fig. 2), cylindrical gold sheets
and ribbed earrings (Fig. 3), the latter of which have parallels on
Java and in central or southern Vietnam (Miksic, 2011: 122e123;
Reinecke et al., 2009: 153e154). In contrast to other sites, where
beads represent the majority of early gold objects, only one single
gold bead was documented from a looted burial at Prohear.
The most specific archaeological information is provided by 14
finger rings and 7 earrings. Especially one finger ring with the
depiction of a horseman (Fig. 14:3) is very interesting in view of the
presence of non-local features. Horses are not native in Southeast
Asia, and horseman images are not found as decoration on Early
Iron Age objects in the southern part of Southeast Asia, but are very
popular in the Dian culture of Yunnan, south China. However, gold-
silver finger rings with a broadened head are neither typical of Dian
nor of Han dynasty (206 BCe220 AD) or any early East Asian
cultures. Therefore, it is likely that this finger ring was made in the
tradition of workshops of Bactria or around the northwest of India,
but its shape and decoration style are still clearly different.
Altogether, the finds from Prohear give the impression that an
‘import wave’ of gold and silver objects arrived together with other
non-local artefacts. As discussed in detail in Reinecke et al. (2009:
 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887 2879

Fig. 2. Pair of biconical earrings from burial 3, Prohear, Prey Veng province. Left: silver coloured (85% silver, dm. 2.4 cm), right: gold coloured (68% silver, dm. 2.1 cm). (For
interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

165e170), a strong relationship to the north and a possible immi-
gration of leaders of the Nan-Yue people from northern Vietnam,
evading the Chinese expansion during the Han dynasty since the
end of the 2nd century BC, could be an explanation.
The present knowledge on ancient Southeast Asian exploitation
of precious metal resources and trade routes is still mainly based on
the early written Indian and Chinese records. They cover the time
from the Han period to the arrival of the Europeans in Southeast
Asia in the 16th century and do not mention any gold deposits,
mining or gold production in Cambodia (Reinecke et al., 2009:
156e157), but e in context of Cambodia e refer to gold and silver
from China (e.g. Zhou, 1297/2007: 71). Nevertheless, gold deposits
exist and are presently being exploited in Cambodia (Zhou et al.,
2003; Sotham, 2004), as well as in many other regions of South-
east Asia (Bennett, 2009). Apart from the larger deposits in use
today, also smaller occurrences of gold veins or placer gold have to
be considered as resources in earlier times. There is some archae-
ological record of ancient gold mining from Sumatra, Laos and
central Vietnam, the latter being the closest to Prohear (Bennett,
2009: 100; Lê, 1776/2007: 282e287). Silver deposits are less
frequent in Southeast Asia, but are known from the ‘silver road’
between southwestern China and northeastern Myanmar, which
existed since the Han dynasty period (Yang, 2004; Fiskesjö, 2010)
and was connected with southeast Cambodia by the Mekong River.
In view of this background, the aim of the chemical analysis of
a first selection of gold and silver objects was to reveal information
about the types of raw material used for their production and to
establish groups which characterise the artefacts in terms of
composition and trace elements. In addition to the Prohear finds,
two gold earrings from Bit Meas, a contemporary but completely
looted Iron Age cemetery situated 8 km south of Prohear, were also
included in this study for comparison.
To obtain as much information on the material as possible, LA-
ICP-MS (Laser Ablation-Inductively Coupled Plasma-Mass Spec-
trometry) was chosen as analytical method, because it allows the
measurement of major, minor and trace elements all at once and

Fig. 3. Ribbed earrings from looted burials in Bit Meas (1, 3; dm. 1.7 cm) and from burial 46 (2; dm. 2.0 cm) in Prohear, Prey Veng province.
2880 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887
Fig. 4. Atomic number contrast of a hypoeutectic silver-copper alloy with dendrites of
silver rich solid-solution and interdendritic eutectic. Cross section of a granule from
the silver coloured biconical earring (MA-100972).
requires only small samples. Since the basic works of Gratuze et al.
(1993) and Watling et al. (1994), this method has developed from
a qualitative or semi quantitative to a quantitative multi-elemental
analysis with high sensitivity and has been applied successfully to
ancient gold and silver objects (Devos et al., 1999; Gondonneau and
Guerra, 2002).
2. Methods and analyses
A selection of 59 gold and silver artefacts e 57 from Prohear and
two from Bit Meas e were either sampled in Cambodia (31 larger
and more valuable objects) or transferred to Germany for direct
analysis and additional sampling (28 small objects and fragments),
resulting in a total number of 62 samples. They were analysed with
LA-ICP-MS, scanning electron microscopy (SEM) with attached
energy dispersive X-ray spectrometer (EDX) and energy dispersive
X-ray fluorescence (EDXRF) at the Curt-Engelhorn-Centre for
Archaeometry (CEZA) in Mannheim.
The LA-ICP-MS measurements of 58 samples were carried out
using a solid-state Nd:YAG laser operating at 213 nm (Microprobe
Fig. 5. Detail of the cross section of a gilded spiral ring (MA-090063) from burial 4 in
Prohear, showing three superimposed gold layers and the zones of interdiffusion (BSE
image).
Fig. 6. Thermal false colour scale of gold (black ¼ highest concentration) of the gilding
layer and silver core of spiral ring MA-090063, showing clearly the interdiffusion of
gold and silver. (For interpretation of the references to colour in this figure legend, the
reader is referred to the web version of this article.)
II, integrated with LUV213 Laser, New Wave Research) coupled to
an XSeriesII quadrupole ICP-MS (Thermo Electron Corporation)
with collision cell technology (CCT). In case of four samples which
were analysed later, a 193 nm ArF excimer laser system (M-50-E,
Resonetics) substituted the Microprobe II. The laser-generated
aerosol, after passing a spiral particle filter to eliminate large
particles (Guillong et al., 2003), was mixed in a glass Y-piece with
a nebulised 2% nitric acid blank before entering the ICP-MS to
maintain stable wet plasma conditions.
A combination of elements common in trace element studies of
both artefact and natural gold (Taylor et al., 1997; Outridge et al.,
1998; Guerra et al., 1999) had been chosen in an earlier project
(Schlosser et al., 2009) and was applied slightly modified to the
Cambodian samples. The isotopes 63Cu, 107Ag, 197Au, 48Ti, 52Cr,
55
Mn, 56Fe, 59Co, 60Ni, 68Zn, 75As, 80Se, 103Rh, 105Pd, 111Cd, 118Sn,
121
Sb, 125Te, 193Ir, 195Pt, 205Tl, 208Pb and 209Bi were analysed quan-
titatively; 101Ru, 189Os and 201Hg semi-quantitatively. They had
Fig. 7. Foil and fusion gilded spiral ring fragment from burial 4 in Prohear (MA-
090063), showing the edges of the overlapping foil (arrows), SE image. In the left
corner the broken end of spiral ring fragment MA-090060, burial 3 in Prohear, showing
the gold coating (BSE image).
 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887
Fig. 8. Qualitative false coloured X-ray map for Au, Ag and Cu of the cross section of
a granule from the gold coloured biconical earring (MA-100973), showing the thin gold
layer on the surface. (For interpretation of the references to colour in this figure legend,
the reader is referred to the web version of this article.)
been selected previously from almost 50 isotopes to be the most
suitable for our measuring conditions (Table 1), which include the
removal of polyatomic ions (CCT), kinetic energy discrimination
(KED) and the recording of the Au and Ag signals in custom reso-
lution mode to reduce the high signal intensities (Heinrich et al.,
2003). The data acquisition sequences consisted of blocks of five
samples at most, each ablated three times, which were enclosed by
blocks of calibration solutions, solid reference materials and
jewellery alloys included to monitor higher silver and copper
contents, each measured twice. The data and standard deviations
for the gold reference materials NA-AU-30 and NA-AU-31 (Nord-
deutsche Affinerie, Hamburg; Kovacs et al., 2009) are given in
Table 2.
On the fragments and small objects, direct laser ablations were
carried out in single-hole drilling mode (spots) to leave the surface
as intact as possible while sampling the interior. On the samples
which had been extracted with a scalpel (maximum weight of
1 mg), the ablations were done in line mode on the cut surface. The
Fig. 9. BSE image of the gilding layer of the cross section of a granule from the gold
coloured biconical earring (MA-100973), showing the porous surface morphology of
depletion gilding.
2881
Fig. 10. 3d scatterplot of Ptnorm, Bi and the Pd/Pt ratio showing group I and II. Unal-
loyed silver sampes are not shown.
compatibility of spot and line ablation data is shown in Table 2; the
relative standard deviation of the means of spot and line ablation
values is smaller than the relative standard deviation of all values.
The details of the laser ablation and pre-ablation are provided in
Table 1.
Special attention was paid to corrosion and silver surface
enrichment on silver objects. Before measurement, the patina and
loose particles were removed by pre-preablation with the laser
disconnected to the ICP-MS. During the measurement, ClO was
monitored at mass 51, and in case of a signal, indicating the pres-
ence of silver chlorides, the ablation was aborted and repeated at
another location. However, due the generally good preservation of
Fig. 11. Scatterplot of the Pd/Pt ratios versus the silver contents showing group I and II
with subgroups. Unalloyed silver sampes are not shown.
2882 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887
Fig. 12. PteAu scatterplot of all group I samples showing the subgroups. The lines
indicate the field of gold and platinum concentrations resulting from hypothetical
alloying of silver to three electrum samples, which embraces the field of the aurifeous
silver samples analysed.
most metal objects, this was only necessary with four objects; two
of unalloyed silver, where the patina was then removed with
a scalpel in a 1 mm area for the new spots, and two which turned
out to be made of alloys most susceptible to corrosion (Rehren et al.,
1996) with 6e7% gold and almost equal amounts of copper.
The quantification method was based on the measurement of all
components and their normalisation to 100% (Leach and Hieftje,
2000). As matrix-matched liquid calibration proved to be appli-
cable with LA-ICP-MS (Kovacs et al., 2009) three calibration
Fig. 13. Scatterplot of the Pd/Pt ratios versus the silver contents comparing types of
objects with metal groups. Unalloyed silver sampes are not shown.
solutions as described in Schlosser et al. (2009) were used. They
consisted of two solutions prepared from the ICP Multi Element
Standards (MES) XVI and XXI (MERCK) and single-element stan-
dards (Cu, Ag) diluted in 2% nitric acid, and one solution prepared
from single-element standards (Cu, Rh, Pd, Sn, Te, Ir, Pt, Au) by first
preparing a stock solution in 7% HCl, which was always freshly
diluted with nitric acid to 5% aqua regia. One nitric acid solution
(with MES XXI) was set to contain 1 mg g1 Ag, the aqua regia
solution to contain 1 mg g1 Au, while all three solutions were set to
contain 1 mg g1 Cu as internal standard and 50 ng g1 of the other
elements.
After data evaluation and background correction using the
Plasmalab software (Thermo), the obtained results were normal-
ised to 100%. The limit of detection was calculated for each isotope
in each ablation as the concentration equivalent to three standard
deviations of the background signal, which contained about 20 data
points.
Although a systematic analysis of technological characteristics
was not part of this study, some details that were observed in the
course of the measurements were examined using an SEM fitted
with a silicon drift detector with a specified energy resolution
better than 127 eV at MnKa and standardless analysis. After
studying the surface structures of two objects and two granules,
they were sampled to investigate the techniques of gilding and
soldering. Suitable flat-polished samples were prepared for quan-
titative microanalysis, in case of the soldering several times itera-
tively. Absolute concentrations were calculated without
normalisation and with overlap correction through peak decon-
volution (Eggert, 2006). The method is controlled regularly by
measurements of standards under defined and reproducible
conditions. In gold and silver reference materials, an accuracy of
1e2% is achieved for the main components and of 5e20% for minor
components. The etched microstructures were also investigated
with optical microscopy.
For comparison, the cross sections were also analysed with
EDXRF with standard-based fundamental parameter correction.
However, the gilding could not be analysed, as the smallest possible
collimator size of 200 mm was still too large. The results comparing
LA-ICP-MS, EDX and EDXRF data are given in Table 3.
3. Results and discussion
3.1. Composition, alloys and gilding
The artefacts show a wide range of composition from practically
pure silver (99%) to high-grade gold (95%), electrum with about 60%
gold as the most frequent alloy (Table 4). The copper concentra-
tions, around 0.3% in most samples, show a tendency to higher
values in the silver rich samples, but rarely exceed 1%, which is not
different to the range in native gold-silver alloys (Boyle, 1979),
although in alluvial placer gold generally lower concentrations can
be found due to the depletion of copper and also silver (Morteani,
1995; Chapman et al., 2006).
Five samples show higher contents of 3e5% and 7%, indicating
that copper was added in some way. In these hypoeutectic alloys,
the copper content is lower than the maximum solubility of copper
in the aAg-phase. They typically consist of two phases in the cast
condition, due to the rapid change of solid solubility of copper in
silver with decreasing temperature (Fig. 4). Copper increases
strength and workability and a range of properties can be obtained
by different heat treatment, which could explain an intentional
addition of even small quantities. However, copper at these
concentration levels would have no effect on the colour of the
alloys because of the high silver contents (Cretu and van der Lingen,
1999).
 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887 2883

Fig. 14. Analysed finger rings from burials 4 (1; dm. 2.0  1.8 cm), 10a (2; dm. 1.9  2.1 cm) and 18 (3; dm. 2.1  1.7 cm).

In five samples, tin contents of 2e4% were detected. The
regarding alloys vary in composition from 72 to 29% gold and can be
grouped into AueAgeSn and AgeAueCueSn alloys. A contamina-
tion with tin from the addition of bronze is not even probable in the
two samples with high copper content, regarding the Cu:Sn ratios
of 3:3 and 5:2, and there is no reason that the tin should have been
added deliberately. But there is a certain correlation of gold and tin,
suggesting a connection between the two elements. Usually e and
also in most samples of the present study e tin is present as minor
or trace element (Guerra et al., 1999; Brostoff et al., 2009) that
indicates that the gold was extracted from a tin-bearing placer
deposit (Dube, 2006). It seems to be an important element for the
comparison of artefact gold with placer gold (Ehser et al., 2011).
Most likely it enters the gold through joint panning of placer gold
with cassiterite (SnO2) and consequent melting under reducing
conditions (Dube, 2006). Native tin has also been reported from
gold deposits (Schmiderer et al., 2007). Considering the proximity
of the Southeast Asian tin belt, and in view of the archaeological
evidence pointing to a relation with northern Vietnam, especially
the rich tin deposits of the Yunnan province (Golas, 1999), it cannot
be ruled out that even such high concentrations of tin in gold could
be of natural origin.
The samples with high tin content are perhaps exclusively
related to foil-fusion gilding, which in contrast to common foil
gilding has not been reported from Southeast Asia to our knowl-
edge so far (Bunker, 2008). This technique could be identified in
three objects, and the gilding foil was made from AgeAue(Cu)eSn
alloy in all cases. The two remaining samples of this group probably
also derive from foil-fusion gilded silver objects, but the regarding
artefacts were not available for direct study yet. Two spiral ring
fragments investigated by SEM and EDX allowed examining the
technique in detail. The gilding layer, which varies in thickness
from 25 to 120 mm, is compact and well bonded to the silver core by
interdiffusion of gold and silver (Figs. 5 and 6). But some small
cuprite inclusions and crevices suggest that up to three layers of
thin gold foil are superimposed (Fig. 5) and were not completely
bonded in some parts. The SE image of the surface of one of the
spiral rings (Fig. 7) shows that the foil was wrapped around the core
wire like a bandage, overlapping at the edges still visible in some
parts. The next step would have been a gentle heating to enable
interdiffusion, but avoiding the ‘whitening’ of the gold by the rapid
diffusion of silver. As is well known, temperature has the most
profound influence on the diffusion path and time; therefore the
heating temperatures should have been in the range between
600  C and 900  C.
In one of the mounted granules belonging to a biconical earring
(MA-100973), a different gilding method could be documented. The
X-ray dot map of gold, silver and copper (Fig. 8) shows a thin and
smooth gold layer of 3e10 mm covering the surface. In addition, the
BSE image (Fig. 9) shows that the gold layer is not compact and still
preserves the porous structure, which is characteristic for depletion
gilding or surface enrichment of gold (Scott, 2000). This iterative
process consists of oxidizing the less noble metals and removing
the oxides using natural corrosive substances, certain acidic salts or

Table 1
Operating conditions for ICP-MS and Laser Ablation.

Laser ablation system Microprobe II M-50-E

Wavelength 213 nm 193 nm
Pulse length 4 ns 5 ns
Laser fluence 24e30 J cm2 e
Preablation pulse rate 4 Hz 6 Hz
Preablation energy 30e70%, depending on sample surface 5 mJ
Preablation spot size 75 mm 58 mm
Preablation duration Spots: 4e8 s, depending on sample surface e
Lines: 1 pass (500e600 mm, 15 mm s1) Lines: 2 passes (200e400 mm, 15 mm s1)
Washout 35 s 35 s
Ablation pulse rate 4 Hz 8 Hz
Ablation energy 100% 5 mJ
Ablation spot size 50 mm 44 mm (gilding: 20 mm)
Ablation duration Spots: 50 s e
Lines: 1 pass (500e800 mm, 15 mm s1) Lines: 1 pass (200e400 mm, 15 mm s1)
Carrier gas flow 1.1 L min1 He 0.6 L min1 He
ICP-MS
Nebulizer gas flow 0.7 L min1 0.82 L min1
Biases Pole Bias 12.9, Hexapole Bias 13.0 (slightly KED) Pole Bias 12, Hexapole Bias 6 (non KED)
Collision gas 6.0 mL min1 H2eHe mixture (8% H2, 92% He)
Detector mode Dual (pulse and analogue counting mode)
Dwell time 10 ms
2884 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887

Table 2
LA-ICP-MS data of reference materials compared to reported values, including the comparison of spot and line ablation. Reference materials do not contain Ir.

% Au % Ag mg kg1 Cu mg kg1 Pd mg kg1 Pt mg kg1 Sn mg kg1 Pb mg kg1 Bi

NA-AU-31 (formerly NA2)
ETH Zuricha avg 5.4 1062 1096 1119 1114 108 110
sd 0.4 e 24 66 6 2 3
CEZA avg all (n ¼ 30) 93.8 5.4 1031 1074 1103 1104 128 134
sd 0.2 0.2 82 70 68 98 24 21
rsd % 0.2 3 8 7 6 9 19 16
avg lines (n ¼ 12) 93.8 5.5 1031 1103 1127 1065 110 129
avg spots (n ¼ 18) 93.8 5.4 1031 1057 1095 1127 139 138
rsd % 0.02 1 0.03 3 2 4 16 5
NA-AU-30 (formerly NA1)
ETH Zurich1 avg 0.9 99 58.7 68.0 53.2 11.5 11.1
sd 0.1 e 0.8 4.0 0.8 1.5 1.2
CEZA avg all (n ¼ 30) 98.9 1.0 99 59 67 53 11 13
sd 0.1 0.1 7 5 3 6 2 2
rsd % 0.1 8 7 9 5 11 17 19
avg lines (n ¼ 16) 98.9 1.0 99 59 68 56 10 13
avg spots (n ¼ 14) 98.9 1.1 98 59 67 52 12 12
rsd % 0.1 4 1 0.5 0.4 6 12 3
a
Values from Kovacs et al. (2009), Table 3.

plant juices for example (Grimwade, 1999; Scott, 2000). The gold of Pd, Ir and Pt for easier comparison of alloys with different
resulting gold layer on the surface is generally very thin (typically gold contents (see below). Of the other elements, the concentra-
3e10 mm) and porous, if not polished afterwards (La Niece and tions of Cr, Co, Ni, Se, Cd, Te, Tl, Ru and Os were near or below the
Meeks, 2000). A possible source for such acid plant juices in limits of detection in most samples. The elements Ti, Mn, Fe, Zn, As,
Southeast Asia could be the wild form of the Giant Taro (Alocasia Sb and Hg did not show considerable differences throughout the
macrorrhizos), which is rich in oxalic acid. Depletion gilding is well samples, and correlations of MneFe and ZneAseSb were observed.
documented for pre-hispanic South America (e.g. Grimwade, 1999; Rhodium is not considered because it correlates perfectly with Pt in
Scott, 2000), very scarce for the Near East (Oddy, 2000), but all samples.
unknown from Southeast Asia so far (Bunker, 2008). In many of the The concentrations of the platinum-group elements (PGE) and
studied objects, the yellow surface colour is not consistent with the their ratios are useful and decisive factors for gold fingerprinting
measured gold content of the alloy. As there is no evidence for foil (Guerra et al., 1999; Brostoff et al., 2009). The presence of PGE
gilding in these objects, we suspect that they are depletion gilded indicates that the gold was extracted from secondary deposits, i.e.
as well. placers (Meeks and Tite, 1980), as they generally derive from
different rock types and primary deposits than gold. In analogy to
3.2. Trace element patterns and groups cassiterite, platinum-group minerals can be included in a gold
placer and are panned together with the gold. During melting and
The trace and minor element data of Pd, Ir, Pt, Sn, Pb and Bi are processing, Pd, Rh and Pt distribute homogenously in the gold,
provided in Table 4, which also includes the values normalised to while Ru, Os and Ir remain as minute inclusions in the gold matrix
(Meeks and Tite, 1980; Dussubieux and Van Zelst, 2004; Brostoff
et al., 2009), whereas Ir tends to appear also outside these inclu-
Table 3
Comparison of different methods on 6 samples (polished cross sections). sions, showing a somewhat intermediate behaviour. As platinum-
group minerals appear in placers all over Southeast Asia (Weiser,
% Au % Ag % Cu % Sn % Pb
2002), the presence of PGE in ancient gold is not unusual and
MA-100972, biconical earring, silver coloured does not delimitate the area of origin of the gold.
LA-ICP-MS 14 85 1 510 mg kg1 89 mg kg1
EDX 13 86 0.9 <0.3 <0.1
Based on the Pd/Pt ratios and the concentrations of Pt normal-
EDXRF 14 85 0.87 <0.05 0.02 ised to gold and of Bi, two main groups can be distinguished
MA-100973, biconical earring, gold coloured (Fig. 10). Group I comprises the majority of the samples and is
LA-ICP-MS 31 68 0.3 30 mg kg1 5 mg kg1 characterised by higher Pd/Pt ratios averaging around 0.15 and by
EDX 31 69 0.5 <0.3 <0.1
low Ptnorm and Bi concentrations. Group II with lower Pd/Pt ratios
EDXRF 31 69 0.36 <0.05 <0.01
MA-090060, spiral ring fragment, gilding averaging about 0.03 shows higher concentrations of Bi and Ptnorm,
LA-ICP-MSa,b 72 24 0.2 3 13 mg kg1 the latter being accompanied by the occurrence of minute
EDX 71 27 0.3 1.5 <0.1 RueOseIr inclusions (which were excluded from the signal evalu-
MA-090060, spiral ring fragment, silver core ation). Iridium concentrations also support the two groups,
LA-ICP-MSa 0.4 99 0.2 50 mg kg1 92 mg kg1
EDX 0.7 99 0.2 <0.3 <0.1
whereas tin and lead appear more erratic and are not discrimi-
EDXRF 0.50 99 0.22 <0.05 <0.01 nating (Table 4). Lead concentrations exceed 200 mg kg1 only in
MA-090063, spiral ring fragment, gilding two samples, which is regarded as the maximum concentration in
LA-ICP-MSa,b 65 32 0.4 2 130 mg kg1 native gold (Guerra et al., 1999). The presence of tin again points to
EDX 67 31 0.6 1.5 <0.1
an alluvial origin for both groups (see Section 3.1).
MA-090063, spiral ring fragment silver core
LA-ICP-MSa 0.04 99 0.2 1 mg kg1 185 mg kg1 According to the silver content, the unnormalised Pt concen-
EDX <0.1 99 0.2 <0.3 <0.1 trations and typological aspects, three subgroups can be estab-
EDXRF 0.06 99 0.4 <0.05 0.02 lished within group I (Fig. 11): gold (Ia), electrum (Ib) and auriferous
a
Ablated with M-50-E eximer laser. silver (Ic). (The term auriferous silver is used in a more general way
b
Only one ablation run possible. in this paper to refer to silver dominated alloys.)
 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887 2885

Table 4
Analytical results of 62 samples from 59 gold and silver objects from Prohear and Bit Meas, determined by LA-ICP-MS. The values are averages of three ablation runs per sample.
Limits of detection (averages, mg kg1): Au 24; Ag 21; Cu 4; Pd 0.5; Ir 0.1; Pt 0.4; Sn 2; Pb 0.3; Bi 0.3. RSD%: Au 0.3e11 (avg 3); Ag 0.1e9 (avg 3); Cu 1e17 (avg 8); Pd 2e34 (avg
15); Ir 3e48 (avg 22); Pt 2e32 (avg 13); Sn 1e45 (avg 22); Pb 0.6e61 (avg 23); Bi 2e41 (avg 18).

Composition (%) Pd/Pt Trace elements (mg kg1) Sample Object (burial number)
ratio
Au Ag Cu Sn Pd Pdnma Ir Irnma Pt Ptnma Sn Pb Bi
Group I I a (gold) 95 5 0.03 e 0.11 6 6 0.1 0.1 57 57 205 13 0.3 MA-093161 Open ring, band-shaped (14)
n ¼ 37 85 15 0.1 e 0.10 7 8 0.3 0.3 67 75 37 1 0.6 MA-093155 Cylindrical gold sheet (46)
83 17 0.1 e 0.21 14 16 0.2 0.2 67 76 14 3 <0.3 MA-093153 Ribbed earring (46)
82 18 0.1 e 0.15 8 9 0.2 0.2 54 62 22 1 0.6 MA-093154 Cylindrical gold sheet (33)
80 20 0.1 e 0.16 9 11 0.2 0.2 56 67 66 5 0.9 MA-093156 Cylindrical gold sheet (33)
75 25 0.3 e 0.16 7 9 0.1 0.1 45 57 70 114 4 MA-093152 Ribbed earring (Bit Meas)
74 26 0.1 e 0.14 5 7 0.1 0.1 37 48 530 6 4 MA-093151 Ribbed earring (Bit Meas)
I b (electrum) 66 34 0.2 e 0.17 8 12 0.1 0.1 49 71 146 7 2 MA-100806 Spiral ring fragment (unit C)
64 36 0.3 e 0.12 6 9 0.1 0.1 51 76 285 21 7 MA-092128 Spiral ring fragment, square wire (43)
63 37 0.2 e 0.16 9 13 0.1 0.1 54 82 48 4 0.9 MA-100807 Spiral ring fragment (22)
62 38 0.3 e 0.13 7 11 0.3 0.5 54 83 54 4 4 MA-093162 Leech-shaped earring (4)
62 38 0.1 e 0.20 8 12 <0.1 e 40 62 56 5 1 MA-100802 Spiral ring (25)
62 38 0.3 e 0.16 9 13 0.1 0.1 54 83 121 4 2 MA-092131 Spiral ring fragment (26)
62 38 0.2 e 0.14 7 11 0.1 0.2 53 83 76 6 1 MA-093166 Spiral ring fragment (22)
60 39 0.5 e 0.15 8 12 0.1 0.1 52 82 130 18 3 MA-092118 Spiral ring fragment (27)
59 40 0.2 e 0.19 9 15 0.1 0.2 50 80 184 33 2 MA-092132 Spiral ring fragment (35)
59 41 0.2 e 0.12 7 11 0.1 0.2 56 91 26 4 24 MA-092134 Spiral ring fragment (8)
58 42 0.2 e 0.18 7 11 <0.1 e 36 59 7 4 2 MA-100808 Spiral ring (16)
56 44 0.2 e 0.12 7 12 0.5 0.9 58 100 32 2 16 MA-090064 Spiral ring fragment (4)
55 44 0.3 e 0.20 8 14 <0.1 e 42 73 4 5 2 MA-093160 Spiral ring (16)
52 48 0.2 e 0.17 6 11 0.1 0.1 37 67 84 19 5 MA-093157 Ring, one end protruding (14)
52 48 0.9 e 0.18 13 24 0.5 0.9 72 132 41 1 3 MA-090059 Spiral ring fragment (3)
51 49 0.1 e 0.17 7 13 0.1 0.1 40 75 39 2 0.8 MA-100803 Open ring (20)
50 49 0.9 e 0.14 7 14 0.3 0.5 50 95 36 2 3 MA-093165 Finger ring (10a)
I c (auriferous 41 59 0.1 e 0.18 6 15 <0.1 e 36 83 26 2 0.9 MA-092130 Spiral ring fragment (45)
silver) 37 63 0.2 e 0.17 4 11 <0.1 e 24 63 <2 3 5 MA-100814 Spiral ring fragment (24)
37 63 0.2 e 0.13 5 12 <0.1 e 36 94 7 0.4 1 MA-092122 Spiral ring fragment (34)
36 64 0.2 e 0.14 4 11 <0.1 e 30 79 2 0.6 2 MA-092120 Spiral ring fragment (10b)
32 68 0.3 e 0.20 6 19 0.1 0.2 31 95 4 3 4 MA-090067 Spiral ring fragment (25)
26 73 0.8 e 0.12 5 16 0.2 0.8 38 137 2 2 1 MA-092117 Spiral ring fragment (22)
25 74 1 e 0.14 5 19 0.3 1 35 134 2 2 7 MA-092116 Spiral ring fragment (22)
24 75 1 e 0.16 5 20 0.3 1 31 126 9 6 11 MA-092125 Spiral ring fragment (22)
21 79 0.1 e 0.16 2 10 <0.1 e 14 64 10 1 0.9 MA-100804 Open ring (20)
I (no subgroup) 75 24 0.3 e 0.10 12 15 0.6 0.8 111 140 137 38 16 MA-092124 Open ring, U-shaped (27)
57 43 0.2 e 0.13 7 12 0.2 0.3 53 90 1020 28 3 MA-090066 Spiral ring fragment (25)
41 59 0.2 e 0.17 5 11 <0.1 e 28 65 640 20 6 MA-093163 Spiral ring fragment (23)
41 59 0.5 e 0.15 6 13 0.1 0.3 38 89 2330 310 6 MA-092133 Spiral ring fragment (35)
Intermediate samples n ¼ 4 44 56 0.1 e 0.09 4 10 <0.1 e 48 104 93 9 5 MA-092121 Spiral ring fragment (44)
39 60 0.7 e 0.07 4 9 0.3 0.7 56 137 19 3 10 MA-093164 Spiral ring fragment (3)
32 67 1 e 0.07 7 21 0.6 2 101 300 3 0.9 8 MA-093159 Open ring (2)
31 68 0.3 e 0.08 4 12 <0.1 e 48 146 30 5 41 MA-100973 Biconical earring, gold coloured (3)
Group II 47 52 0.9 e 0.02 10 21 2 4 570 1150 1800 52 52 MA-100812 Spiral ring (4)
n ¼ 10 37 62 0.8 e 0.02 17 43 1 3 860 2200 250 23 70 MA-100811 Spiral ring fragment (4)
24 76 0.5 e 0.04 5 20 0.8 3 138 550 139 4 32 MA-100809 Spiral ring fragment (2)
21 78 1 e 0.03 7 30 0.9 4 220 1000 58 106 94 MA-092140 Leech-shaped earring fragment (4)
18 81 0.7 e 0.03 6 30 1 5 181 950 85 4 40 MA-092136 Spiral ring fragment (2)
17 82 1 e 0.05 6 35 0.5 3 118 660 10 3 10 MA-090062 Spiral ring fragment (2)
17 80 3 e 0.03 4 24 2 9 128 710 <2 9 49 MA-100810 Finger ring (4)
16 83 0.5 e 0.03 5 30 0.2 1 176 1030 7 2 21 MA-090065 Leech-shaped earring fragment (4)
14 85 1 e 0.03 3 21 <0.1 e 99 680 510 89 26 MA-100972 Biconical earring, silver coloured (3)
6 90 4 e 0.05 2 37 0.9 15 45 770 2 9 100 MA-092126 Leech-shaped earring fragment (24?)
Ungrouped 72 27 0.3 e 0.02 4 6 1 2 250 330 145 160 10 MA-093158 Finger ring with horseman image (18)
n¼2 7 86 7 e 0.21 5 67 0.4 5 23 320 61 12 140 MA-090061 Open ring, square wire (3)
b,c
Tin bearing Ungrouped 72 24 0.2 3 0.04 98 130 18 24 2500 3300 e 13 27 MA-090060 Spiral ring fragment: gilding (3)
b,c
alloys 65 32 0.4 2 0.07 35 51 1 2 520 760 e 130 390 MA-090063 Spiral ring fragment: gilding (4)
n¼5 To group II 57 38 0.7 4 0.03 12 19 4 6 430 710 e 110 28 MA-100805 Leech-shaped earring, gilding? (4)
46 47 3 3 0.03 13 26 6 13 430 890 e 89 15 MA-092129 Leech-sh. earring frgm.: gilding (12)
29 64 5 2 0.03 5 17 0.9 3 180 590 e 1770 76 MA-100813 Open ring, gilding? (4)
c
Unalloyed silver 0.4 99 0.2 e 0.3 2 e 0.1 e 4 e 50 92 64 MA-090060 Spiral ring fragment: silver core (3)
n¼4 0.2 99 0.6 e 1 1 e <0.1 e 1 e 11 59 66 MA-092135 Leech-shaped earring (4)
0.1 99 0.4 e 0.7 3 e 0.1 e 4 e 750 142 17 MA-092129 Leech-sh. earring frgm.: silver core (12)
c
0.04 99 0.2 e 6 6 e 0.1 e 1 e 1 185 820 MA-090063 Spiral ring fragment: silver core (4)
a
Concentration normalized to 95% gold.
b
Only one ablation run possible.
c
Ablated with M-50-E eximer laser.

The gold and electrum subgroups show similar ranges of Sn and sheets and a unique small, band-shaped open ring with ribbed
unnormalised Pt concentrations and may well be interpreted as ornament, exclusively appear in this subgroup (Fig. 13), underlining
natural alloys deriving from placers with similar geological back- its definition. They probably come from a specialised workshop,
ground. The Ia gold objects, three ribbed earrings, three cylindrical which also provided the two ribbed earrings from Bit Meas that fit
2886 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887
well to the single one from Prohear. The gold object not grouped to
Ia (MA-092124), although still considered as group I, is different:
The thick, U-shaped open ring with one cut end is well burnished
and without parallels among the finds.
The Ib electrum objects in contrast mainly consist of spiral rings
and simple open rings, corresponding in style and technique to the
objects made of auriferous silver (Ic). In fact, Ib and Ic represent one
single workshop and can only be distinguished from each other
chemically, as the artefacts show the same variety of yellow to
yellowish golden surface colour probably due to depletion gilding.
But the chemical difference is interesting: subgroup Ic with higher
silver contents than Ib shows lower unnormalised Pt and Sn
concentrations. As Fig. 12 demonstrates, decreasing Au concentra-
tions correlate with decreasing Pt concentrations between the two
subgroups, indicating that both elements were diluted by the
addition of silver, i.e. that the Ic auriferous silver was produced by
alloying high-grade silver to the Ib electrum. Most probably,
subgroup Ic represents an artificial alloy, as a geological origin is not
very likely for auriferous silver (Rehren et al., 1996).
The group II objects are mainly made from auriferous silver, but
with higher silver contents of 76e90% and heterogeneous tin and
lead concentrations. In five samples (MA-092126, MA-092140, MA-
100811e13), bismuth is positively correlated with silver, which at
least for these samples could be regarded as the source of the
higher Bi concentrations in this group. The gilded silver object MA-
090063 containing about 800 mg kg1 Bi provides a good example.
The placer gold used for alloying, with its high PGE concentrations
(Table 4) and different ratio of Pd to Pt, must have come from
a deposit with geological background different to group I gold and
electrum.
Of the AgeAue(Cu)eSn alloy samples, three are closely related
to the group II placer gold source and only differ in the tin content,
if considered of natural origin, while two AueAgeSn alloy samples
are different, also from each other, in Pd/Pt ratio, Ptnorm and Bi
(Table 4). However, as in their case only one ablation was possible
on the gilding layer on the cross sections, the values have to be
considered with care and require further validation from new
samples.
Regarding style, elaboration and object type, the AgeAue(Cu)e
Sn alloy samples form a group with other group II objects, con-
sisting of two thick spiral ring fragments, a well shaped thick open
ring, one whole and four fragmented leech-shaped earrings
(Fig. 13), to which another whole leech-shaped earring made of
unalloyed silver corresponds. Their shapes are very uniform and
well-balanced, in contrast to another leech-shaped earring
belonging to subgroup Ic: It is one of three not fragmented earrings
of this type, all found in burial 4, but resembles the workmanship of
the Ib-Ic objects and could be interpreted as a copy.
There is a second object suggesting the idea of imitation of
group II objects in the Ib-Ic workshop: One of a pair of biconical
earrings found in burial 3 (Fig. 2) differs from the other in
composition and trace elements, as well as in colour (depletion
gilding), diameter, manufacturing and elaboration, and obviously
was not made in the same workshop. While the more elaborate
silver coloured earring belongs to group II, the gilded one belongs
to a group of four objects with element patterns somewhat inter-
mediate between group I and II, although partly closer to group I.
Typologically and technologically, three of them (Fig. 13) corre-
spond to the artefacts of subgroups Ib and Ic, indicating that also
the gilded biconical earring was produced in this workshop. The
intermediate position of these four objects in Fig. 11 provokes the
idea that they could be the result of mixing Ib electron with the
auriferous silver of group II, perhaps indicating recycling.
The unalloyed silver objects are all related to group II and the
AgeAue(Cu)eSn alloys, either by the object type (leech-shaped
earrings) or the foil-fusion gilding. The low lead and bismuth, as
well as the high gold concentrations probably indicate that the four
objects are made from silver which was not extracted from
argentiferous lead ores by cupellation, which usually results in lead
concentrations of a few per mil to per cent in the silver (Meyers,
1999). But it cannot be ruled out that lead was removed to
a greater extent due to repeated processing, especially considering
MA-090063 and MA-092129, making it unlikely to determine the
origin of the silver. As a consequence, the interpretation of the
other trace elements is not clear. However, the (not gilded) leech-
shaped earring MA-092135 and the gilded spiral ring MA-090060
are very similar in composition and trace elements, while the
other two differ in the concentrations of Au, Pd, Sn and Bi.
Of all gold and silver finds, the finger ring with horseman
depiction (MA-093158) does not only stand out for its style and
type, but also for its trace elements (Table 4). With its high gold
content, intermediate Ptnorm concentration, low Bi concentration
and low Pd/Pt ratio, it is clearly different from both groups and
represents another alluvial gold source. The other two analysed
finger rings (Fig. 14) belong to the Ib electrum subgroup and to
group II, and differ much in type, style, manufacturing and
elaboration.
Although not all objects have been analysed so far and many of
the excavated burials were partly disturbed, the analysed objects
deriving from 24 burials provide first indications regarding the
relation of metal groups and contexts. The number of precious
metal artefacts in these graves ranged from one to six, the majority
containing one or two, while the outstanding “burial of the fine old
lady” (burial 4) with a complete bronze drum included 13 gold and
silver ornaments. Most of the objects of burial 4 belong to group II,
and also in the other rich burials with 5 and 6 pieces, group II is
represented. Vice versa, in the burials with fewer gold-silver
objects, group II is missing, not regarding a leech-shaped earring
fragment (MA-092126) with unsure affiliation to burial 24.
Apparently, group II is related exactly to the elite burials with non-
local features like bronze drums, stone pestles etc. Electrum and
auriferous silver objects of subgroup Ib and Ic are distributed
equally in all graves, while the Ia gold ornaments appear only in
those with five to two ornaments, being absent not only in the
burials with only one piece, but also in the richest.
4. Conclusions
A selection of 57 gold and silver objects found during the rescue
excavations at Prohear and two from the nearby looted cemetery of
Bit Meas could be characterised successfully in terms of composi-
tion and trace elements by LA-ICP-MS and give a completely new
impression of the precious metal working in Southeast Asia during
the last century BC and the first century AD. Two main groups
representing different alluvial gold/electrum placers bearing plat-
inum minerals and cassiterite could be established based on the
concentrations of Pt, Ir, Bi and especially the Pd/Pt ratio. The
majority of the ornaments belong to group I and most likely come
from two workshops, one specialising in certain types of gold
objects as ribbed earrings for example, and one producing mainly
spiral rings from electrum and auriferous silver. Group II is closely
related to the rich burials with non-local features, representing
different object types, e.g. leech-shaped earrings, deriving from
a technically more advanced workshop.
SEM-EDX analyses revealed two different gilding techniques so
far unknown from Southeast Asia, foil-fusion gilding of silver
objects and depletion gilding. The first is related to group II and to
special AgeAue(Cu)eSn alloys as gilding foil, which contain up to
4% tin of perhaps natural origin. Depletion gilding was observed on
one object and is suspected for many of the group I ornaments
 S. Schlosser et al. / Journal of Archaeological Science 39 (2012) 2877e2887
made from auriferous silver and electrum. The occurrence of this
technique is currently being examined systematically in the course
of the ongoing investigation of the Prohear finds, which also
continues the analysis of the remaining gold, electrum and silver
finds in order to complete this interesting finding.
The application of LA-ICP-MS to silver samples proved to be
useful and reliable under certain conditions. In order to select the
least corroded inner parts, it is advisable to ablate on polished cross
sections or, in case of direct ablation from the object, it should be
ascertained that enough surface material is removed. Thus, for
silver artefacts, laser ablation cannot be as minimal invasive as for
gold objects.
Acknowledgements
We thank the Ministry of Culture and Fine Arts, Phnom Penh,
Cambodia, and the Memot Centre for providing all possibilities to
conduct the research on gold and silver objects from Prohear and
Bit Meas. The German Archaeological Institute funded fieldwork
and metal analyses of the Prohear project upon which this study is
based. We are also grateful for inspiring ideas and discussions to
Verena Burnett, CEZA Mannheim (especially for the later
measurements), Thilo Rehren (London), H.E. Chuch Phoeurn,
Secretary of State, and H.E. Hab Touch, Director General of Heritage,
Ministry of Culture and Fine Arts of Cambodia.
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