Non-destructive handheld XRF study of archaeological composite silver objects—the case study of the late Roman Seuso Treasure

Abstract

This study details the non-destructive chemical analysis of composite silver objects (ewers, situlas, amphora and casket) from one of the most significant late Roman finds, the Seuso Treasure. The Seuso Treasure consists of fourteen large silver vessels that were made in the fourth–early fifth centuries AD and used for dining during festive banquets and for washing and beautification. The measurements were systematically performed along a pre-designed grid at several points using handheld X-ray fluorescence analysis. The results demonstrate that all the objects were made from high-quality silver (above 90 wt% Ag), with the exception of the base of the Geometric Ewer B. Copper was added intentionally to improve the mechanical properties of soft silver. The gold and lead content of the objects shows constant values (less than 1 wt% Au and Pb). The chemical composition as well as the Bi/Pb ratio suggests that the parts of the composite objects were manufactured from different silver ingots. The ewers were constructed in two ways: (i) the base and the body were made separately, or (ii) the ewer was raised from a single silver sheet. The composite objects were assembled using three methods: (i) mechanical attachment; (ii) low-temperature, lead-tin soft solders; or (iii) high-temperature, copper-silver hard solders. Additionally, two types of gilding were revealed by the XRF analysis, one with remnants of mercury, i.e. fire-gilding, and another type without remnants of mercury, presumably diffusion bonding.

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ORIGINAL PAPER
Non-destructive handheld XRF study of archaeological composite
silver objects—the case study of the late Roman Seuso Treasure
Viktória Mozgai
1
&Bernadett Bajnóczi
1
&Zoltán May
2
&Zsolt Mráv
3
Received: 22 November 2020 /Accepted: 15 March 2021
#The Author(s) 2021
Abstract
This study details the non-destructive chemical analysis of composite silver objects (ewers, situlas, amphora and casket) fromone
of the most significant late Roman finds, the Seuso Treasure. The Seuso Treasure consists of fourteen large silver vessels that
were made in the fourth–early fifth centuries ADand used for diningduring festive banquets and for washing and beautification.
The measurements were systematically performed along a pre-designed grid at several points using handheld X-ray fluorescence
analysis. The results demonstrate that all the objects were made from high-quality silver (above 90 wt% Ag), with the exception
of the base of the Geometric Ewer B. Copper was added intentionally to improve the mechanical properties of soft silver. The
gold and lead content of the objects shows constant values (less than 1 wt% Au and Pb). The chemical composition as well as the
Bi/Pb ratio suggests that the parts of the composite objects were manufactured from different silver ingots. The ewers were
constructed in two ways: (i) the base and the body were made separately, or(ii) the ewer was raised from a single silversheet. The
composite objects were assembled using three methods: (i) mechanical attachment; (ii) low-temperature, lead-tin soft solders; or
(iii) high-temperature, copper-silver hard solders. Additionally, two types of gilding were revealed by the XRF analysis, one with
remnants of mercury, i.e. fire-gilding, and another type without remnants of mercury, presumably diffusion bonding.
Keywords Late Roman .Composite silver objects .Handheld XRF .Seuso Treasure .Chemical composition .Gilding
Introduction
The Seuso Treasure is one of the most significant treasure
finds from the late Roman Imperial period (Painter 1990;
Mango and Bennett 1994; Mráv and Dági 2014; Dági and
Mráv 2019). The Treasure is composed of 14 large, domestic
silver vessels (Fig. 1), as well as the copper cauldron in which
they were hidden. The name originates from the owner, Seuso,
which is written in the metric inscription of one of the platters.
The pieces are typical of the period, representing parts of a
dining set used during festive banquets and also including
vessels for washing, bathing and beauty treatments. The ob-
jects of the Seuso Treasure are amongst the largest known late
Roman silver vessels, and they are outstanding in both their
artistic and material value. Most of the silver vessels were
manufactured in the fourth century AD, although some may
have also been produced in the early fifth century AD. They
were likely hidden in NE Pannonia (present-day Hungary)
when the Romans fled from a “barbarian”attack in the late
fourth or early fifth century AD (Mráv and Dági 2014;Dági
and Mráv 2019).
During the final centuries of the Roman Empire, other sil-
ver hoards were similarly hidden underground in various parts
of the Empire (e.g. Hoxne (England); Mildenhall (England);
Kaiseraugst (Switzerland); Vinkovci (Croatia); Esquiline,
Rome (Italy); Traprain Law (Scotland)). X-ray fluorescence
(XRF) analysis has been used to examine most of the other
Roman silver treasures (Hughes and Hall 1979;Langetal.
1984; Feugère 1988;Hughesetal.1989; Lang 2002;Cowell
and Hook 2010; Hook and Callewaert 2013; Minning and
*Viktória Mozgai
mozgai.viktoria@csfk.org
*Bernadett Bajnóczi
bajnoczi.bernadett@csfk.org
1
Institute for Geological and Geochemical Research, Research Centre
for Astronomy and Earth Sciences, Eötvös Loránd Research
Network (ELKH), H-1112 Budaörsi út 45, Budapest, Hungary
2
Institute of Materials and Environmental Chemistry, Research Centre
for Natural Sciences, Eötvös Loránd Research Network (ELKH),
H-1117 Magyar tudósok körútja 2, Budapest, Hungary
3
Hungarian National Museum, H-1088 Múzeum körút 14–16,
Budapest, Hungary
https://doi.org/10.1007/s12520-021-01321-4
/ Published online: 17 April 2021
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Ponting 2013; Sánchez and Lansing Maish 2014;Langand
Hughes 2016;Greiff2017; Angelini et al. 2019; Arias et al.
2019), although other techniques were also used to determine
the elemental composition of the objects, such as emission
spectroscopy (Lang et al. 1977;Berthoudetal.1988;
Mango and Bennett 1994) and particle-induced X-ray emis-
sion spectroscopy (PIXE) (Tate and Troalen 2009;Doračić
et al. 2015;Vulićet al. 2017).
Non-destructive handheld X-ray fluorescence spectrom-
etry (hXRF) is one of the most popular elemental analytical
methods in the fields of archaeology and cultural heritage
(Shackley 2012; Frahm and Doonan 2013;Zlateva2017),
and it is often utilised in the analysis of archaeological and
historical metal objects, particularly in the elemental anal-
ysis of precious metal objects (e.g. Karydas et al. 2004;
Cesareo et al. 2008; Melcher et al. 2009; Parreira et al.
2009; Asderaki-Tzoumerkioti and Karydas 2011;Pardini
et al. 2012; Mass and Matsen 2013; Zori and Tropper
2013; Lehmann et al. 2014;Živkovićet al. 2014; Mozgai
et al. 2017;Mozgaietal.2018; Horváth et al. 2019a;
Szenthe et al. 2019;May2020;Mozgaietal.2020). XRF
is a simultaneous, multi-element analytical method, where-
by the concentrations of most elements of the periodic
table (Z = 12–92, from Mg to U) can be determined (major,
minor and trace elements).
The elemental analysis of silver objects is essential to
understand the contemporaneous raw material use,
alloying practice and manufacturing and decoration tech-
niques. The major element content helps us to understand
whether any conscious technological choice of alloys was
applied for the different parts of the composite silver ob-
jects. The minor and trace element content can provide
information about the used ore sources, raw materials and
metallurgical techniques. Non-destructive analytical
methods, such as handheld XRF, are particularly useful
in the analysis of precious metal objects, where sampling
is not or only limitedly allowed due to the high value of the
objects. By using hXRF, the objects can be measured sys-
tematically at numerous points in situ in the museums, and
semi-quantitative elemental information can be gained
quickly. Moreover, sampling sites for more detailed anal-
ysis, e.g. quantitative elemental, lead isotopic and metallo-
graphic analysis, can be planned based on the hXRF
measurements.
However, the hXRF method has some limitations,
which must be taken into consideration during data evalu-
ation. Because XRF is a surface analytical method, the
measured concentrations represent the outer part (usually
a few tens of microns) of the analysed objects. The signal
comes from different depths, depending on the element and
the matrix (Tate 1986;MassandMatsen2013). Metal ob-
jects can be chemically heterogeneous for several reasons,
such as phase segregation in silver-copper alloys during
manufacture; acid treatments after preparation (etching),
which dissolve copper from the surface layers; polishing
during and after manufacture; corrosion and tarnishing;
remnants of gilding, etc. (Mass and Matsen 2013).
Surface enrichment of silver alloys is a well-known phe-
nomenon, during which base metals (e.g. copper and lead)
are leached out from the surface, while silver and gold are
enriched towards the surface (Hall 1961;Lejček et al.
2010), artificially exaggerating the silver and gold content
at the expense of copper. Therefore, non-destructive sur-
face analytical results, like hXRF data, may not represent
the core metal composition. Surface enrichment can affect
high-quality (> 90 wt%) silver objects as well, observed on
silver coins (e.g. Beck et al. 2003;Becketal.2004;Caridi
et al. 2013;Hrnjićet al. 2020;Hrnjićet al. in press). In
order to reduce the effect of the surface enrichment,
polishing or abrasion of a small area before XRF analysis
is usually carried out (e.g. Hughes and Hall 1979;Lang
et al. 1984;Lang2002; Lang and Hughes 2016;Greiff
2017).
Metal samples taken from objects in the Seuso Treasure
were previously analysed by ICP-OES and scanning electron
microscopy (Mango and Bennett 1994). However, no analy-
ses were performed on the Hippolytus Ewer, and only one
metal sample was measured from the Toilet Casket, which is
Fig. 1 The Seuso Treasure: 1.
Geometric Platter; 2. Meleager
Platter; 3. Achilles Platter; 4.
Seuso (or Hunting) Platter; 5.
Hippolytus Ewer; 6. Hippolytus
Situla A; 7. Hippolytus Situla B;
8. Animal Ewer; 9. Dionysiac
Ewer; 10. Amphora; 11. Toilet
Casket; 12. Geometric Ewer A;
13. Basin; 14. Geometric Ewer B.
The red numbers indicate the
composite objects discussed in
the present paper (photo: A.
Dabasi and J. Kardos (HNM))
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comprised of three parts. The ICP-OES results are sometimes
inaccurate, as concentrations of gold were noticeably low in
most cases. These limitations justify the utilisation of new,
more detailed elemental analyses on the objects.
The aim of this study is to determine the elemental com-
position of the late Roman Seuso Treasure silver vessels
using handheld XRF to classify the objects, to detect chem-
ical differences between the objects, as well as chemical
inhomogeneity within the objects, to determine the raw
material (ore) used and to characterise the gilding and join-
ing techniques. These results contribute to a more detailed
reconstruction of late Roman craftsmanship, including sil-
versmithing, manufacturing, alloying, decoration and as-
sembling practices.
The Seuso objects were in good condition; thus, no ad-
ditional surface cleaning (polishing or abrasion) was per-
formed before this study’s hXRF measurements. In return
for the lack of cleaning, we performed measurements at
several points on each part of the objects. Our approach
differs from archaeometric studies performed on other
Roman silver hoards, because those objects were usually
only measured at a few points (1–20 points) per object
(Lang et al. 1977; Hughes and Hall 1979;Langetal.
1984;Berthoudetal.1988;Feugère1988;Hughesetal.
1989;Lang2002; Cowell and Hook 2010; Hook and
Callewaert 2013; Minning and Ponting 2013;Doračić
et al. 2015;LangandHughes2016;Greiff2017;Vulić
et al. 2017;Angelinietal.2019; Arias et al. 2019), where-
as our hXRF analysis eventuated a much larger data set (~
1600 points). Due to the high number of measurement
points, surface cleaning was even more impossible, as the
importance of the treasure meant that it was not appropriate
to abrade the surface in order to expose the underlying
metal over an area of about 3–8mmindiameter(7–50
mm
2
), large enough to match the XRF beam, especially
on the highly decorated, clearly visible sides.
Two of the platters (Seuso/Hunting Platter and
Geometric Platter) manufactured from single casts were
previously analysed by hXRF alongside two other late
Roman platters (Ribbon Platter and Rosette Platter from
the Sava River find), which revealed a slight variation in
the concentration of silver and copper along the radii of the
plates manufactured from high-quality silver (> 95 wt%
Ag) (Mozgai et al. 2017). The two other large, silver plat-
ters (Meleager Platter and Achilles Platter) and the Basin,
also made from high-quality silver, have a more homoge-
neous composition (Mozgai et al. 2020). In this paper, we
focus on the composite objects (ewers, situlas, amphora
and toilet casket), which are assembled from several parts,
and examine, in detail, the chemical differences between
the various parts of the objects. Furthermore, the hXRF
data are compared with the previously published ICP-
OES data (Mango and Bennett 1994).
Materials and methods
Materials: the composite silver objects of the Seuso
Treasure
Technological observations suggest that composite objects are
composed of several parts (body, base, handle, lid, upper
beaded rim, thumbpiece, feet) and were manufactured from
different silver casts (Mango and Bennett 1994; Dági and
Mráv 2019). They are classified into groups based on their
shape and function (for parameters and decoration
techniques of the objects, see Table 1).
The relief-decorated Amphora is embellished with
Dionysiac motifs, animal fighting scenes and xenia images,
and its shape and decoration suggest that it was used to serve
wine. It was constructed from several parts: a body, a base,
two panther-shaped handles and a stopper connected with a
chain. The body was manufactured either with the lost-wax
casting technique (like the Baratti amphora was, Arias et al.
2019) or was hammered out of a single piece of silver, with no
visible joins or seams. The cast base was hammered, and a
centring point for a lathe is visible on it. The handles were
likely cast using the lost-wax technique.
The Animal Ewer is decorated with chased figures and a
variety of geometric patterns. It may have belonged to a bath-
ing set, or it may have been used to serve wine, like the
Amphora was. The body and base were cast or raised from a
single piece of silver by hammering, while the upper beaded
rim was cast separately and soldered to the body. The lid,
made from a piece of silver, shows traces of hammering.
The handle was cast from a small bar of silver.
The Dionysiac Ewer is the smallest ewer in the Seuso
Treasure. Based on its decoration with Dionysiac imagery
(depicting the thiasos, the retinue of Dionysus), it was proba-
bly used to serve wine. The body, the base and the neck were
cast or hammered from a single piece of silver. The octagonal
rim was made separately by casting or hammering and was
then soldered to the body. The handle was cast from a single
bar of silver.
Geometric Ewers A and B are decorated with identical
chased geometric motifs. The ewers likely formed a set with
the Basin. The bodies were hammered out of individual pieces
of silver, while the bases were made separately by hammering
and were then mechanically attached to the bodies. The upper
beaded rims were cast separately and were soldered to the
bodies, whereas the handles were cast from small bars of
silver.
The Hippolytus Ewer depicts scenes from Greek mytholo-
gy (episodes from the Hippolytus story) and comprises a bath-
ing set, along with two situlas. The body was cast or raised by
hammering from a single silver piece. The base was cast and
hammered from a separate piece of silver, after which it was
mechanically attached and soldered to the body. The upper
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beaded rim was cast separately and was then soldered to the
body. The lid, handle and lion-shaped thumbpiece were made
using the lost-wax technique.
The Hippolytus Situla A and B form a bathing set and are
decorated with the same Greek mythological scenes as the
Hippolytus Ewer is. The bodies were cast or hammered out
of single sheets of silver. The beaded rims were cast separately
and were then soldered to the bodies, while the three feet were
cast using the lost-wax technique and were also soldered to the
bodies. The handles were cast and riveted to the decorative
busts, which were likewise soldered to the body.
The Toilet Casket was probably stored smaller ointment con-
tainers using in daily toiletries. Both the body and the lid were
cast or manufactured by hammering from single sheets of silver.
The interior pierced disc was produced from a hammered sheet
of silver and contains seven pierced holes for flask storage.
The objects of the Seuso Treasure were examined, restored
and conserved at the Institute of Archaeology at University
College, London between April and December of 1989
(Bennett in Mango and Bennett 1994). Some of the objects
were covered with calcareous encrustations, silver corrosion
products and patches of green copper corrosion products.
Furthermore, some parts of the objects were harshly cleaned
and chemically polished during the period between the exca-
vation and the restoration in 1989. Unfortunately, noinforma-
tion is known about this period. During the restoration in
1989, a 15% solution of ammonium thiosulphate and distilled
water was used to remove silver corrosion products and cal-
careous encrustations from all visible surfaces. Green copper
corrosion products were carefully removed with a 10% solu-
tion of formic acid and distilled water. After cleaning, each of
the objects were washed several times in distilled water baths
for 2–5 days. A thin layer of Paraloid B-72 was used to con-
serve the objects (Bennett in Mango and Bennett 1994).
Methods
After thorough macroscopic observation, the objects from the
Seuso Treasure were systematically analysed by handheld X-
ray fluorescence spectrometry (hXRF) along a pre-designed
grid at several points on each object (see Online Resource 1).
The number of measurement points ranged from 2 to 70 points
per part, depending on the size of the measured part of each
object.
In this study, two hXRF instruments from different manu-
facturers were used: (i) a Thermo Scientific Niton Xl3t
GOLDD+ (Waltham, Massachusetts, USA) and (ii) a
SPECTRO xSORT Combi (Kleve, Germany) (see Table 2
for the analytical conditions). During the measurements, the
concentrations of the following major, minor and trace ele-
ments were determined: Ag, Cu, Au, Pb, Bi, Sb, Sn, Zn and
Fe (see Online Resource 1for the detection limits of each
hXRF instrument). The built-in calibrations of each instru-
ment were used for the measurements (Table 2). The
Thermo Scientific Niton Xl3t GOLDD+ instrument measured
Bi and Sb using the ‘General Metals’calibration, whereas the
‘Precious Metals’calibration was used for the rest of the ele-
ments. The quantitative evaluation was performed with the
built-in fundamental parameters (FP) method, using
Compton normalization. The results were normalised to
100%, and no calibrations in data were applied. The precision
and accuracy of the hXRF instruments were determined by
separate measurements taken of a Roman silver spoon and on
modern silver-copper alloys (see Online Resource 1for
details).
The XRF spectra were evaluated by using NITON Data
Transfer Version NDT_REL_8.0.0 (Thermo Scientific Niton
Xl3t GOLDD+) and XRF Analyzer Pro v.1.9. (SPECTRO
xSORT Combi) software programs. The data points were
Table 1 Parameters and decoration techniques of the analysed
composite silver objects from the Seuso Treasure. *repoussé technique:
method of decorating metals in which parts of the design are raised in
relief from the back or the inside of the object by means of hammers and
punches. The name derives from the French word re-+ pousser meaning
to push back (Untracht 1968; Maryon 1971; McCreight 1991)
Find name Height (cm) Weight (kg) Capacity (litre) Repoussé technique* Dot-
punching
Chasing Gilding Niello inlays
Ewers and amphora
Amphora 38.5 2.5 –XXXX
Animal Ewer 51.0 3.98 4 X X X X
Dionysiac Ewer 43.5 3.0 4 X X X X
Geometric Ewer A 52.8 2.65 4 X X X
Geometric Ewer B 55.0 2.8 4 X X X
Hippolytus Ewer 57.3 4.05 –XXXX
Cylindrical objects
Hippolytus Situla A 22.7 4.44 –XXXX
Hippolytus Situla B 22.9 4.48 –XXXX
Toilet Casket 32.0 2.05 –XXX
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plotted by using Microsoft Office Excel Professional Plus
2016 and CorelDraw Graphics Suite 2018 (v.20.1.0.708) soft-
ware programs.
The relative error of the Thermo Scientific Niton Xl3t
GOLDD+ instrument is less than 0.5% for silver, less than
5% for copper, less than 6% for gold, less than 10% for lead
and less than 20% for bismuth. The relative error of the
SPECTRO xSORT Combi instrument is better, namely less
than 0.1% for silver, less than 0.5% for copper, less than 2%
for gold, less than 5% for lead and less than 10% for bismuth.
At some points (less than 7% of the total measurements),
higher relative errors were calculated, but none is above
50%. These points do not show a systematic distribution,
and not related to anobject or to a specific feature of the object
(e.g. geometric problems).
For optimal measurements, the handheld XRF instrument
requires ideal and reproducible surface geometries, such as
flat surface that are parallelto the spectrometer head. The lack
of suitable and reproducible geometries can cause an error of
0.5% or more, if the objects have complex geometries (e.g.
ewers, vessels, statues) (Mass and Matsen 2013). Therefore,
we aimed to measure surfaces that were as flat as possible, as
well as to analyse the same locations on eachobject with each
instrument.
We compared the performance of the two hXRF instru-
ments based on the analysis of the composite objects of the
Seuso Treasure and concluded that only the data measured
by the same XRF instrument, under the same analytical
conditions and using the same built-in calibration can be
reliably compared (see Online Resource 1). As a result,
hereafter we handle the data of the two instruments sepa-
rately and compare the chemical compositions within these
separate, independent data sets (according to Brand and
Brand 2014).
Results
Chemical composition of the composite objects of the
Seuso Treasure
In general, the objects were manufactured from high-quality
silver alloyed with copper (79.6–99.4 wt% Ag; 0.1–18.6 wt%
Cu) (Table 3;Figs.2,3and 4). The gold content is around or
below 1 wt% (except the Animal Ewer, discussion below)
(Table 3;Figs.2,3and 4). The lead content is usually below
1 wt% (Table 3; Online Resource 2), and the bismuth content
of the objects is heterogeneous, even within one object
(Table 3;Figs.2,3and 4). The tin, zinc and antimony contents
are below the detection limit, with except for some parts of
some of the objects (discussion below).
The various parts (base, body, handle, stopper) of the
Amphora differ chemically from each other. The stopper
contains the least amount of copper (0.8–1.2 wt%), whereas
the base contains the most (3.0–3.8 wt%) (Fig. 2). The gold
and lead contents are not homogeneous between the
Amphora’s parts. The bismuth content of the parts is very
variable, ranging from 0 to 2600 ppm (Fig. 2; Online
Resource 2).
The chemical composition of the various parts of the
Animal Ewer is also different. The body and the base contain
the least amount of copper (0.6–3.3 wt%), whereas the upper
beaded rim, lid and handle contain the most (1.0–7.3 wt%)
(Fig. 2). The gold and lead contents are generally below or
around 1 wt%. At several points, the gold content of the parts
was elevated (> 1 wt%) (discussion below) (Fig. 2). The bis-
muth content of the parts is homogeneous (100–1400 ppm)
(Fig. 2). In the upper beaded rim and the handle, 0.5–0.8 wt%
tin was detected. The chemical composition of the body and
the base is identical, but the handle, upper beaded rim and lid
were manufactured from silver alloys of different
compositions.
The chemical composition of the various parts of the
Dionysiac Ewer is different. The base and the body have the
lowest copper content (1.1–1.8 wt%), whereas the handle and
the thumbpiece have the highest (2.7–4.3 wt%) (Fig. 2). The
body and the base have the same chemical composition; how-
ever, the thumbpiece, handle and upper octagonal rim were
made from different silver alloys. The silver and copper con-
tents of the upper octagonal rim fall between the composition
of the thumbpiece and handle and the base and body, respec-
tively. The gold and lead contents are below 1 wt% (Fig. 2;
Online Resource 2). The bismuth content of the Dionysiac
Ewer is the highest (1200–3200 ppm) of all the Seuso objects
(Fig. 2). In the thumbpiece and handle, 0.5–0.6 wt% zinc was
detected.
Table 2 Comparison of the analytical conditions of the two handheld XRF instruments used for analysing the Seuso Treasure
Instrument SPECTRO xSORT Combi Thermo Scientific Niton Xl3t GOLDD+
Detector Energy-dispersive SDD Energy-dispersive LDD
X-ray tube 50 kV; Rh-anode 50 kV, Ag-anode
Built-in calibrations ‘Light Elements’‘General Metals’and ‘Precious Metals’
Spot size 3 mm 3 and 8 mm
Acquisition time 60 s 50 s and 40 s
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Table 3 Chemical composition of the composite objects of the Seuso
Treasure. Ag, Cu, Au, Pb are given in wt%, Bi is given in ppm. N =
measured using Niton Xl3t GOLDD+ hXRF; S = measured using
SPECTRO xSORT Combi hXRF. The minimum–maximum values are
given. The Au/Ag and Bi/Pbratios were calculated for each measurement
points and the minimum–maximum values are given as well
Instrument No. of analyses Ag Cu Au Pb Bi Au/Ag Bi/Pb
Amphora
Base N 8 93.7–94.9 3.3–3.8 1.0–1.2 0.6–0.9 1400–1900 0.011–0.013 0.21–0.24
S4 94.0–94.8 3.0–3.6 0.9–1.0 0.6–0.9 1100–1400 0.010–0.011 0.16–0.18
Body N 54 96.1–98.0 0.5–1.9 0.6–1.2 0.4–1.5 0–500 0.006–0.013 0–0.08
S27 96.2–97.7 1.1–1.8 0.5–0.8 0.6–1.0 0–200 0.005–0.008 0–0.03
Handle N 4 95.8–96.2 2.3–2.6 0.4–0.5 1.0–1.1 200–300 0.005 0.01–0.02
S4 95.5–95.9 2.3–2.5 0.4–0.5 1.1 100–200 0.004–0.005 0.01–0.02
Stopper N 2 97.7–98.1 1.1–1.2 0.3–0.5 0.2 2000–2600 0.004–0.006 0.95–1.23
S2 98.2–98.4 0.8 0.3 0.1–0.2 1500–1600 0.003 0.99–1.00
Animal Ewer
Body N 64 94.9–97.9 0.8–3.3 0.9–2.4 0.2–0.9 400–1000 0.009–0.025 0.09–0.40
S31 94.2–97.9 0.6–2.2 0.8–1.9 0.1–0.9 100–700 0.008–0.020 0.06–0.25
Base N 11 96.4–98.3 0.5–1.7 0.5–1.6 0.2–0.3 500–900 0.005–0.017 0.26–0.34
S4 95.9–97.0 1.3–1.6 0.9–1.0 0.2–0.3 400–500 0.010 0.16–0.21
Handle N 7 92.9–94.6 3.2–4.7 0.7–1.7 0.4–0.7 900–1100 0.008–0.018 0.15–0.23
S4 94.0–94.5 3.4–4.1 0.8–1.1 0.4–0.5 600–900 0.009–0.011 0.16–0.17
Upper beaded rim N 5 93.7–95.4 2.4–4.0 1.0–1.1 0.3–0.5 700–1400 0.011–0.012 0.21–0.31
S3 94.6–95.0 2.6–3.2 1.2–1.4 0.2–0.4 500–600 0.012–0.015 0.15–0.22
Lid N 10 90.5–96.7 1.0–7.3 0.4–1.4 0.3–0.9 300–1100 0.004–0.015 0.04–0.17
S3 93.2–93.8 3.3–3.7 0.7–0.8 0.7 700–800 0.008–0.009 0.11
Dionysiac Ewer
Body N 61 96.6–98.0 1.1–1.8 0.4–1.2 0.1–0.3 1400–2400 0.004–0.013 0.54–1.64
S14 96.4–97.9 1.3–1.6 0.3–0.5 0.1 1200–1700 0.003–0.005 1.13–2.21
Base N 8 97.2–97.8 1.3–1.8 0.4–0.5 0.1–0.2 1600–2000 0.004–0.005 0.86–1.46
S7 97.5–97.9 1.2–1.5 0.3–0.4 0.1 1200–1300 0.004 0.87–2.28
Thumbpiece N 3 94.0–95.0 3.2–4.2 0.5–0.6 0.2–0.3 2800–3200 0.005–0.007 1.05–1.14
Handle N 6 93.2–95.6 2.7–4.3 0.5–0.7 0.2–1.1 2500–3200 0.005–0.007 0.29–1.20
S2 91.2–94.7 3.8–4.1 0.4–0.5 0.2–0.5 2100–2200 0.004–0.006 0.44–1.26
Upper octagonal rim N 6 95.6–96.4 2.3–2.6 0.5–0.6 0.1–0.6 2800–3200 0.005–0.006 0.52–2.31
S5 95.8–96.4 2.3–2.5 0.5–0.6 0.1–0.4 2100–2500 0.005–0.006 0.57–2.62
Geometric Ewer A
Body N 70 93.9–97.8 0.9–2.9 0.7–1.1 0.5–1.1 900–1400 0.008–0.012 0.10–0.19
S30 96.3–97.9 0.9–1.6 0.7–0.9 0.4–0.7 500–1000 0.007–0.009 0.09–0.15
Base N 14 94.5–97.1 1.4–4.1 0.7–1.1 0.2–0.5 500–1100 0.008–0.011 0.16–0.25
S9 94.3–96.2 1.1–3.7 0.8–1.1 0.1–0.6 100–700 0.008–0.011 0.04–0.14
Handle N 7 92.3–94.7 3.8–6.1 0.8 0.6–0.8 1000–1200 0.008–0.009 0.13–0.19
S5 93.0–94.8 3.5–5.2 0.7–0.8 0.7–0.8 800–1000 0.007–0.009 0.10–0.14
Upper beaded rim N 4 93.0–95.2 3.7–5.8 0.8–0.9 0.3–0.6 500–900 0.008–0.010 0.17–0.21
S4 91.6–93.0 4.5–6.5 0.7–1.0 0.2–0.6 400–700 0.008–0.010 0.11–0.23
Geometric Ewer B
Body N 62 95.2–97.1 1.6–3.2 0.8–1.1 0.2–0.4 600–1000 0.009–0.011 0.17–0.21
S16 95.4–96.4 1.9–2.5 0.7–1.1 0.2–0.3 400–700 0.008–0.011 0.14–0.19
Base N 11 79.6–94.0 4.5–18.6 0.8–1.1 0.4–0.5 700–900 0.009–0.011 0.17–0.31
S7 84.9–93.5 4.5–10.9 0.7–1.0 0.3–0.5 500–800 0.008–0.011 0.15–0.27
Handle N 11 92.4–94.6 3.7–5.9 0.7–0.9 0.6–0.8 800–1100 0.008–0.009 0.11–0.15
S5 93.5–94.2 3.6–4.8 0.7–0.8 0.8 700–900 0.007–0.009 0.09–0.11
Upper beaded rim N 5 90.2–95.6 2.0–7.1 0.7–1.0 0.6–1.3 500–1100 0.008–0.010 0.04–0.17
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The two Geometric Ewers (A and B) have a similar chem-
ical composition. The bodies contain the least amount of cop-
per (0.9–3.2 wt%), whereas the base of Geometric Ewer B
shows an elevated amount of copper (4.5–18.6 wt%), with a
very heterogeneous distribution. The base of Geometric Ewer
A exhibits a lower concentration of copper (between the com-
position of the body and the upper beaded rim and handle)
(Fig. 3). The gold and lead contents are below 1 wt% (Fig. 3;
Online Resource 2). The bismuth content is homogeneous
(Fig. 3). The chemical composition of the various parts of each
ewer (body, handle, base, thumbpiece, upper beaded rim) in-
dicates that they were manufactured from silver alloys of dif-
ferent compositions.
Based on the observed variation in the chemical composi-
tion of the different parts (lid, body, base, handle, upper
beaded rim) of the Hippolytus Ewer,theyweremanufactured
from different silver alloys. The lid has the highest copper
content (3.4–6.9 wt%), whereas the base has the lowest
Table 3 (continued)
Instrument No. of analyses Ag Cu Au Pb Bi Au/Ag Bi/Pb
S2 89.6–95.5 1.4–4.6 0.8–1.0 0.6–0.9 0–400 0.009–0.011 0.009–0.011
Thumbpiece N 3 93.5–94.8 3.4–4.6 0.8–0.9 0.7–0.8 1000–1200 0.008–0.009 0–0.07
Hippolytus Ewer
Body N 32 94.4–96.8 1.8–4.1 0.6–1.0 0.4–0.6 900–1500 0.007–0.011 0.21–0.28
S15 96.2–96.8 1.6–2.1 0.6–0.8 0.4–0.5 700–1000 0.007–0.008 0.16–0.23
Base N 15 95.7–98.4 0.8–2.9 0.5–1.0 0.2–0.4 700–2600 0.005–0.010 0.19–1.09
S8 94.3–97.5 1.3–2.8 0.5–1.0 0.1–0.4 500–1200 0.005–0.010 0.16–0.98
Lid N 8 91.4–95.1 3.6–6.9 0.6–1.0 0.5–0.6 500–900 0.006–0.010 0.09–0.16
S4 92.2–94.2 3.4–6.2 0.5–0.6 0.4–0.6 400–600 0.006–0.007 0.08–0.11
Handle N 9 93.9–97.1 1.6–5.0 0.6–1.1 0.3–1.1 700–2000 0.007–0.011 0.11–0.56
S2 94.8–96.2 2.3–3.4 0.8–0.9 0.3–0.4 400–1300 0.009 0.12–0.40
Upper beaded rim N 8 94.0–97.5 1.5–3.2 0.5–0.9 0.3–1.4 1500–2300 0.005–0.010 0.16–0.62
S4 95.2–97.0 1.7–3.2 0.5 0.2–0.6 1400–1700 0.005–0.006 0.30–0.72
Hippolytus Situla A
Handle N 9 95.6–97.2 1.8–2.7 0.6–0.9 0.4–0.7 400–900 0.007–0.009 0.10–0.16
S4 96.6–97.1 1.8–2.0 0.6 0.2–0.5 200–500 0.006–0.007 0.06–0.10
Feet N 8 95.4–97.6 0.8–2.6 0.9–1.1 0.3–0.8 400–1100 0.010–0.011 0.08–0.29
S2 95.2–96.2 2.1–2.6 0.8–0.9 0.4–0.7 600–700 0.008–0.010 0.10–0.14
Body N 32 96.2–98.2 0.6–2.8 0.5–0.9 0.1–0.3 200–900 0.005–0.010 0.07–1.47
S21 95.7–97.2 2.1–2.6 0.4–0.6 0.1–0.2 0–200 0.005–0.006 0–0.12
Upper beaded rim N 5 98.9–99.2 0.4–0.6 0.3–0.4 0–0.1 0–1400 0.003–0.004 0–3.20
S4 95.3–99.0 0.3–0.5 0.3 0–0.04 400–800 0.003 0–6.28
Hippolytus Situla B
Handle N 11 96.6–97.7 1.2–2.1 0.6–0.8 0.3–0.5 300–800 0.006–0.008 0.08–0.30
S 4 97.3 1.6–1.7 0.5–0.6 0.3 0–300 0.005–0.006 0–0.10
Feet N 8 94.6–97.3 1.1–2.9 0.7–1.1 0.2–1.3 700–1200 0.008–0.012 0.09–0.33
S2 95.2–95.4 2.5–2.7 0.8 0.4–0.5 700 0.008–0.009 0.14–0.17
Body N 33 95.6–97.5 1.7–3.2 0.5–0.9 0.3–0.5 200–500 0.006–0.010 0.07–0.12
S22 92.5–97.4 1.7–2.7 0.5–1.0 0.2–0.5 100–400 0.005–0.011 0.02–0. 11
Upper beaded rim N 8 98.6–99.3 0.1–0.8 0.3–0.5 0–0.4 500–2000 0.003–0.005 0.18–2.60
S6 98.7–99.4 0.1–0.5 0.2–0.5 0–0.01 0–600 0.002–0.005 0–6.41
Toilet Casket
Lid N 55 94.8–96.6 2.0–3.7 0.6–1.2 0.3–0.5 600–1300 0.006–0.013 0.14–0.33
S23 94.8–96.7 1.9–3.5 0.7–1.2 0.3–0.5 500–1000 0.007–0.013 0.13–0.22
Base N 49 94.9–97.5 1.2–3.6 0.8–1.2 0.2–0.5 400–900 0.009–0.013 0.10–0.20
S24 95.0–96.9 1.0–3.4 0.8–1.0 0.2–0.5 100–500 0.009–0.011 0.03–0.11
Pierced disc N 12 93.4–93.8 4.3–4.7 0.8 0.7 1300–1500 0.009 0.19–0.21
S6 91.8–94.1 3.9–4.5 0.7–0.8 0.6–0.8 1000–1200 0.008 0.14–0.16
Archaeol Anthropol Sci (2021) 13: 83 Page 7 of 20 83
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(0.8–2.9 wt%) (Fig. 3). Although the gold and lead contents
are constant and fall below 1 wt%, the upper beaded rim and
handle contain a slightly higher percentage of lead (0.2–1.4
wt%) (Fig. 3; Online Resource 2). The bismuth content is
Fig. 2 Silver vs. copper and gold vs. bismuth content of the Amphora, the
Dionysiac and the Animal Ewers based on the hXRF measurements,
previous ICP-OES data are shown for comparison. Measured with 1:
Niton Xl3t GOLDD+; 2: SPECTRO xSORT Combi; 3: ICP-OES
(Mango and Bennett 1994)
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much more heterogeneous than the gold and lead content of
the parts. The bismuth content of the body, lid and handle is
400–1500 ppm, and the upper beaded rim and part of the base
exhibit higher concentrations (500–2600 ppm) (Fig. 3).
Fig. 3 Silver vs. copper and gold vs. bismuth content of the Hippolytus
and the Geometric Ewers based on the hXRF measurements, previous
ICP-OES data are shown for comparison. Measured with 1: Niton Xl3t
GOLDD+; 2: SPECTRO xSORT Combi; 3: ICP-OES (Mango and
Bennett 1994)
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The various parts of the two Hippolytus Situlas (handle,
feet, body and upper beaded rim) differ chemically from each
other. The upper beaded rims have the highest silver content
of all the Seuso objects; in fact, they were manufactured from
Fig. 4 Silver vs. copper and gold vs. bismuth content of the Hippolytus
Situlas and the Toilet Casket based on the hXRF measurements,
previous ICP-OES data are shown for comparison. Measured with
1: Niton Xl3t GOLDD+; 2: SPECTRO xSORT Combi; 3: ICP-OES
(Mango and Bennett 1994)
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almost pure silver (> 99 wt%) (Fig. 4). The gold content is
heterogeneous. The feet have the highest gold content (0.7–
1.1 wt%), while the upper beaded rim has the lowest (0.2–0.5
wt%). The gold content of the handles and the bodies is sim-
ilar (0.5–1.0 wt%). The lead content is constant and falls be-
low 1 wt%, whereas the bismuth content is heterogeneous,
ranging from 0 to 1500 ppm (Fig. 4; Online Resource 2).
The parts (lid, base, pierced disc) of the Toilet Casket have
different chemical compositions, indicating that they were
manufactured from silver alloys of different compositions.
The pierced disc contains the most copper (3.9–4.7 wt%),
and the lid and base contain similar amounts of copper (1.0–
3.7 wt%) (Fig. 4). The gold and lead contents are constant and
fall below or around 1 wt% (Fig. 4; Online Resource 2).
Bismuth is present in slightly lower concentrations in the base
(100–900ppm)thaninthelid(500–1300 ppm) and the
pierced disc (1000–1500 ppm) (Fig. 4).
Gilding
Each of the composite objects was selectively gilded, except the
Toilet Casket, and the gilding is quite worn in some places (Fig.
5). The gilding was analysed at several points, ranging from 2 to
60 points per object, depending on the object and the extent of
the gilded surfaces. The gold content of the gilded surfaces
ranges from 1.0 to 76.2 wt% depending on the thickness of the
gilding (Online Resource 3). The relative thickness of the gilding
was estimated based on the macroscopic observations and on the
gold content of the gilded areas. In the case of the Amphora,
Animal Ewer, Dionysiac Ewer and the Hippolytus set, mercury
was detected in the gilded parts (Fig. 5g). Gold spans the edge of
the gilded area, particularly in the case of the Animal Ewer,
whose flat surfaces were gilded. On the ribs of the Animal
Ewer, which separate the different sections of the body, gilding
was not observed by the naked eye, only at the very edges, in
deeper depressions, but the elevated gold content indicates that
the entirety of the ribs was originally gilded (Online Resource 3;
Fig. 5a, b). In contrast, the gilding of the two Geometric Ewers
wasanalysedin61and68points,respectively,andnomercury
was detected in any of analysed points by the handheld XRF
(Fig. 5g). The gilding appears to be very thin, is pale yellow
and generally follows the decoration lines (Fig. 5e, f).
Soldering
The various parts of the Seuso objects were assembled in
different ways. The joints were analysed at several points,
ranging from one to seven points per object. At the joints of
handles, feet, lids and thumbpieces, as well as at the ancient
repairs, elevated tin and lead contents were measured (1.4–
70.1 wt% Pb; 0.8–43.4 wt% Sn), indicating the use of a soft
lead-tin solder (Online Resource 3;Fig.6e). The soldering
material completely recrystallised, resulting in increased
volume and a detachment of the soldered parts (handles,
thumbpieces, lids) (Fig. 6a–c). At the joints of the bodies
and the upper beaded rims of the ewers and the situlas, green
copper corrosion products were observed by the naked eye,
which manifested in higher copper concentrations (31.9 wt%
Cu) (Online Resource 3; Fig. 6d).
Discussion
Major elements: silver and copper
Each of the objects was manufactured from high-quality
silver, which corresponds well with the observation that
high-purity (80–99 wt% Ag) silver objects were created in
the late Roman period (Table 4) (Hughes and Hall 1979;
Lang et al. 1984;Feugère1988;Lang2002;Tateand
Troalen 2009; Cowell and Hook 2010;HookandCallewaert
2013; Doračićet al. 2015; Lang and Hughes 2016; Greiff
2017;Vulićet al. 2017).
Pure silver is too soft to fashion everyday items from, be-
cause it dents, bends and wears easily. In the late Roman
period, the most common silver alloying element was copper,
as it added strength and hardness to the softer silver. The
hardness of an alloy depends not only on its chemical compo-
sition but also on the degree of working and heat treatment.
The hardnessincreases quickly up to 15% copper content, and
between 30 and 80% copper it reaches a rather constant value
(Hughes and Hall 1979). As the amount of copper that is
added to the molten silver increases, the more yellowish the
alloy will become. During silver extraction, the copper content
may be reduced to 0.2–1%; thus, higher copper concentrations
indicate intentional alloying (Hughes and Hall 1979). The
copper content of late Roman silver objects ranges from 0.1
to 15% (Table 4) (Hughes and Hall 1979;Langetal.1984;
Feugère 1988; Lang 2002; Tate and Troalen 2009; Cowell and
Hook 2010; Hook and Callewaert 2013; Doračićet al. 2015;
Lang and Hughes 2016; Greiff 2017;Vulićet al. 2017). The
copper content of the Seuso objects fits into this range. The
differences in the copper contents of the various parts of the
composite objects also indicate intentional alloying:
(i) The parts that are more exposed to mechanical effects,
such as handles, bases, rims, lids and feet (e.g. the base
and handle of the Amphora, the handles of the Animal,
Dionysiac, Hippolytus and Geometric Ewers, the bases of
the Geometric Ewers, the pierced disc of the Toilet
Casket), were usually made from alloys with higher cop-
per but lower silver contents.
(ii) The parts made with repoussé technique (e.g. the bodies
of the Animal, Dionysiac and Hippolytus Ewers, the
bodies of the Hippolytus Situlas, the lid and the base of
the Toilet Casket) were generally made from alloys
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containing a higher percentage of silver, which are more
malleable and make it easier to form the small details of
the figures and scenes (Greiff 2017).
(iii) The parts that were unequivocally manufactured by casting
(handles, thumbpieces, lids, feet, upper beaded and octag-
onal rims) usually have higher copper contents, because
alloys with higher copper contents require a lower melting
point, making it easier to cast the alloy. These parts in-
clude, e.g. the upper beaded rims of the Animal,
Geometric and Hippolytus Ewers, the octagonal rim of
the Dionysiac Ewer, handles of the Amphora, the lid of
the Animal and Hippolytus Ewers. The upper beaded rims
of the Hippolytus Situlas are exceptions; they were cast
from almost pure silver (> 99 wt% Ag). The use of silver
Fig. 5 Gilding on the Seuso
objects. a,bThe Animal Ewer:
gilding spreads over the edge of
the gilded area and is quite worn,
invisible with naked eye at the
ribs. cThe Hippolytus Situla A. d
The Amphora. e,fThe Geometric
Ewers A and B (photo: A. Dabasi
and J. Kardos (HNM)). ghXRF
spectra of the gilded areas on the
examples of the ewers measured
with SPECTRO xSORT Combi
instrument
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alloys with higher copper contents can also be economic
(Mango and Bennett 1994).
The results of the previous ICP-OES measurements made
on bulk metal samples taken from the Seuso objects (Mango
and Bennett 1994) show the same trends as our hXRF results
(Figs. 2,3and 4, Online Resource 4). However, as hXRF is a
surface analytical method, the effects of corrosion processes
are evident: the less noble copper was leached out, and the
more noble silver was enriched at the surface. Generally, ICP-
OES measured higher copper concentrations (0.5–5wt%
higher) compared to hXRF (Figs. 2,3and 4).
Minor and trace elements (impurities)
With the exception of silver and copper, the measured el-
ements are naturally occurring and unintentionally added,
deriving from the silver ore or from the copper used for
alloying (Hughes and Hall 1979). Their individual content
usually does not exceed 1% (except for gold at some points
in the Animal Ewer, discussion below).
In the Roman period, the primary source of silver was
silver-bearing lead ores (Tylecote 1962;Forbes1971). The
silver ores were roasted, melted and cupelled during silver
extraction. Cupellation cleansed the silver of impurities
(e.g. antimony, arsenic, tin, iron and zinc; less well from
copper, gold and bismuth). The volatile elements (antimo-
ny, arsenic, mercury, tin and zinc) disappear from the mol-
ten silver during cupellation (Pernicka 2014;L’Héritier
et al. 2015); however, they can be present in high concen-
trations (several %) in native silver (Pernicka 2014). The
absence of these volatile elements in the analysed objects
indicates that cupelled silver was used for manufacturing.
Thepresenceofzincandtininsomepartsoftheobjects
Fig. 6 Solders on the Seuso
objects. aRemnants of lead-tin
soft solder at the joint of the han-
dle to the body of the Dionysiac
Ewer. bRemnants of lead-tin soft
solder at the joint of lid to the base
of the Toilet Casket and at ancient
repairs. cThick, corroded, re-
crystallised lead-tin soft solder at
the joint of the handle of
Geometric Ewer B. dGreen cop-
per corrosion products along the
rim of the Hippolytus Situla A
indicating the use of copper-
containing hard solder (photo: A.
Dabasi and J. Kardos (HNM)). e
hXRF spectra of the soft solders
on the example of the ewers
measured with SPECTRO
xSORT Combi instrument.
Animal Ewer: at the joint of the
lid to the body; Dionysiac Ewer:
at the joint of the handle to the
body; Geometric Ewer B: at the
joint of the handle to the body at
the beaded rim; Hippolytus Ewer:
at the joint of the lid to the body
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(0.5–0.8 wt% Sn in the upper beaded rim and handle of the
Animal Ewer; 0.5–0.6 wt% Zn in the thumbpiece and han-
dle of the Dionysiac Ewer) indicates that brass and bronze,
respectively, were used as alloying metals instead of pure
copper. This is supported by the calculated Cu/Sn (~ 83%
Cu;~17%Sn)andCu/Zn(~87%Cu;~13%Zn)ratios
(Hughes and Hall 1979;Greiff2017). This alloying prac-
tice was indeed unusual in the Roman times, but later,
during the Migration Period, it was commonly practised
(Craddock et al. 2010;Horváthetal.2019b;Mozgai
et al. 2019). Though it is rare in Roman times, but it is
not without example. Elevated Zn content was found in
some of the pieces of the Hoxne hoard and concluded as
the result of alloying with brass typical of Roman period
(Cowell and Hook 2010). Hughes and Hall (1979) detected
elevated zinc content in some bowls from the Chaourse
hoard and in some Sassanian objects, and elevated tin con-
tent in some objects from the Sutton Hoo hoard, indicating
the use of brass or bronze scrap material for alloying.
Ancient Romans produced high-purity silver with a lead
content of 0.5–1% (Hughes and Hall 1979). If silver originates
from silver-bearing lead ores (galena, anglesite or cerussite),
the lead content in the silver alloy ranges from 0.001 to 3%
(Moorey 1985). The lead content of the analysed Seuso ob-
jects falls within this range. The lead contents of the objects
differ, because cupellation occurred in multiple steps, which
resulted in the different lead contents, or because silver ores
from different sources were used. The low and constant lead
content indicates that lead was not added to the silver ore
during smelting. As such, lead isotope analyses may help to
determine the provenance of the raw material. Lead in the
silver objects could derive from the alloying metal, if bronze
or leaded bronze was used, but in this case, we would expect
elevated tin content as well. Therefore, we assume that the
lead content of the Seuso objects derives from the silver ore.
Bismuth is also helpful in determining the raw material
provenance of silver objects, as its concentration does not
change significantly during cupellation (Pernicka and
Bachmann 1983; Pernicka 2014;L’Héritier et al. 2015). Dry
ores or native silver have bismuth contents below 0.05%
(Craddock 1995), whereas argentiferous galena contains
0.1–1% bismuth (Gale and Stos-Gale 1981). Based on cupel-
lation experiments, bismuth is oxidised in the final stages of
cupellation; therefore, bismuth in silver objects is correlated
with the degree of cupellation. However, the final Bi/Pb ratio
of the cupelled silver depends on the initial Bi content of the
silver-bearing lead ores (L’Héritier et al. 2015). The Bi/Pb
ratio indicates that the Seuso objects can be categorised as
having a homogeneous Bi/Pb ratio or a heterogeneous Bi/Pb
ratio in the various parts of the composite objects. The
Dionysiac Ewer has the highest Bi/Pb ratio (Table 3, Fig. 7).
The body, base, handle and thumbpiece have similar compo-
sitions, although the octagonal rim shows the highest Bi/Pb
ratio of all the objects. The Animal Ewer and Geometric
Ewers A and B have a very similar and homogeneous Bi/Pb
ratio, whereas the Hippolytus Ewer and the Amphora have a
heterogeneous Bi/Pb ratio. The bismuth contents of the body
and the handles of the Amphora fall below the detection limit
of the XRF (~ 150 and ~ 60 ppm, respectively, Online
Resource 1). The base and stopper are characterised by a
low and a high Bi/Pb ratio, respectively. The Bi/Pb ratios of
the body, handle and lid of the Hippolytus Ewer are similar to
the ratios of the Animal and Geometric Ewers, while the upper
beaded rim and the base have higher Bi/Pb ratios (Table 3,
Fig. 7). The Bi/Pb ratios of the Toilet Casket and Hippolytus
Situla A and B are low and homogeneous, with the exception
Table 4 Chemical composition of contemporaneous silver treasure finds including number of their analysed objects. The results are given in wt%
Treasure finds Analytical method No. of analysed objects No. of analyses Ag Cu Au Pb Bi
Mildenhall
1
XRF 20 124 93.7–98.0 0.3–4.2 0.4–2.6 0.2–2.2
Hoxne
2
XRF 96 106 85.0–99.0 0.1–4.7 0.1–1.0 0.2–4.4 0–0.3
Kaiseraugst
3
XRF 8 15 95.6–98.6 1.0–3.5 0.3–1.3 0.1–0.9
Vinkovci
4
PIXE 49 56 89.1–99.8 0.2–8.9 0.4–3.4 0.1–1.6 0–0.3
Esquiline
5
XRF 12 32 88.6–98.3 0.4–10.3 0.2–4.7 0.6–1.0
Coleraine
6
XRF 30 30 88.7–97.5 1.2–6.6 0.4–2.2 0.3–2.3
Carthage
7
XRF 20 52 94.3–97.7 1.9–4.5 0.3–1.1 0.1 –0.9
Caubiac (Thil)
8
XRF 4 4 93.8–98.2 1.1–4.3 0.4–0.8 0.2–0.6
Trier
9
XRF 1 20 81.9–95.1 2.2–14.6 1.1–2.5 0.3–1.9 0–0.2
Water Newton
10
XRF 13 17 88.6–97.9 1.8–9.9 0.2–4.4 0–0.8
Seuso
11
XRF 14
a
1620 79.6–99.4 0.1–18.6 0.2–2.4 0.1–1.5 0–0.3
a
The four platters and the Basin of the Seuso Treasure are also included. The minimum–maximum values are given. The number of analyses given for
the Seuso Treasure is the sum of the measurements of the two hXRF instruments.
1
Hughes and Hall 1979;Langetal.1977; Lang and Hughes 2016;
2
Cowell and Hook 2010;
3
Lang et al. 1984;
4
Doračićet al. 2015;Vulićet al. 2017;
5
Hughes and Hall 1979;
6
Hook and Callewaert 2013;
7
Lang 2002;
8
Feugère 1988;
9
Greiff 2017;
10
Hughes and Hall 1979;
11
Mozgai et al. 2017; Mozgai et al. 2020; present study
Archaeol Anthropol Sci (2021) 13: 83
83 Page 14 of 20
Content courtesy of Springer Nature, terms of use apply. Rights reserved.

of the upper beaded rims of the situlas, which exhibit hetero-
geneous Bi/Pb ratios (Fig. 7). The differences in the Bi/Pb
ratios indicate that different silver ingots were used to make
the different parts of the objects.
Gold is completely miscible with silver. During metallur-
gical processes, the gold content of silver does not change
drastically (L’Héritier et al. 2015). Consequently, the Au/Ag
ratio does not alter during cupellation (Pernicka 2014). The
gold content of argentiferous galena ranges from 0.01 to 1%,
whereas the gold content of cerussite and anglesite ranges
between 0.1 and 0.5% (Karydas et al. 2004 and references
herein). The gold content of late Roman silver objects falls
between 0.1 and 4.7% (Table 4) (Hughes and Hall 1979; Lang
et al. 1984; Feugère 1988; Lang 2002; Tate and Troalen 2009;
Cowell and Hook 2010; Hook and Callewaert 2013;Doračić
et al. 2015; Lang and Hughes 2016;Greiff2017;Vulićet al.
2017). There are several reasons that gold concentrations ex-
ceed 1%, such as the presence of remnants of former gilding,
the re-usage of scrap gilded silver or the use of gold-silver
ores. The gold content of the Seuso objects shows constant
values and falls within the range typical of late Roman objects.
This indicates that primary silver ore was used during manu-
facture, instead of the re-usage of scrap silver, which would
result in a wide range of variation in the gold values. The
differences in the gold content of the Seuso objects indicate
the use of different ingots.
The similarities and differences in the chemical composi-
tions of the various parts of the objects support the technolog-
ical observations (Mango and Bennett 1994; Dági and Mráv,
2019). The different compositions of the various parts of the
objects indicate the use of different ingots. Based on their
manufacturing techniques, the ewers can be classified into
two groups: (i) the body and the base were cast or raised from
a single silver sheet (e.g. Animal and Dionysiac Ewers) and
(ii) the body and base were made separately and were later
joined mechanically (e.g. Hippolytus Ewer and Geometric
Ewers A and B).
The previous ICP-OES analyses (Mango and Bennett
1994, Online Resource 4) systematically measured lower gold
contents in the bulk metal samples compared to our hXRF
values (Figs. 2,3and 4), possibly due to digestion problems;
thus, they are not included in this research. However, the
bismuth contents compared well and showed the same trend
as the hXRF results (Figs. 2,3and 4). Furthermore, our anal-
ysis also completes the previous ICP-OES measurements, as
we determined the chemical composition of each part of the
Hippolytus Ewer and the Toilet Casket and demonstrated the
use of different silver ingots for their manufacture.
When our results are compared to other contemporaneous
silver hoards, it is evident that most of them primarily contain
platters, plates and bowls, which were generally manufactured
from a single silver batch. The Seuso Treasure is unique, be-
cause it is mostly composed of large, composite objects
(ewers, amphora, situlas, casket) that were manufactured from
several parts. Ewers, the casket and the amphora from the
Trier, Vinkovci and Esquiline hoards were analysed at several
points (Online Resource 5) (Hughes and Hall 1979;Doračić
et al. 2015;Greiff2017;Vulićet al. 2017). Of these objects,
the Apostle jug from Trier exhibits a noticeable chemical dif-
ference between the various parts, indicating that it was not
manufactured from one, large, uniform batch of silver. The
body, which is heavily decorated, has the highest silver con-
tent (93.9–95.1 wt% Ag), whereas the handle and the
thumbpieces exhibit higher copper concentrations (81.9–
95.0 wt%) (Online Resource 5)(Greiff2017). This chemical
differencebetween the various parts of the Apostle jug isvery
similar to that of the ewers in the Seuso Treasure.
Gilding
The hXRF data show that the Seuso objects were decorated
with two types of gilding: (i) fire gilding, which contained
mercury; and (ii) a different gilding technique that did not
contain mercury. Mercury was detected in the gilding of the
Amphora, Dionysiac Ewer, Animal Ewer and the Hippolytus
set, indicating the use of fire gilding. In contrast, mercury was
absent from the gilding of Geometric Ewers A and B, indicat-
ing the possible use of a different gilding technique (Fig. 5).
Fig. 7 Au/Ag vs. Bi/Pb ratio of
the Seuso objects based on the
hXRF measurements. Measured
with Niton Xl3t GOLDD+ (ligh-
ter colours) and SPECTRO
xSORT Combi (darker colours)
instruments
Archaeol Anthropol Sci (2021) 13: 83 Page 15 of 20 83
Content courtesy of Springer Nature, terms of use apply. Rights reserved.

Fire gilding was likely invented in China in the fourth century
BC (Lechtman 1971; Lins and Oddy 1975;Oddy1981,1988,
1991,1993,2000). In the fire gilding technique, gold was
dissolved in hot mercury, and the resulting gold amalgam
was rubbed on to the cleaned metal surface, after which the
object was heated for a few minutes at 250–300 °C (below the
boiling point of mercury, 357 °C) until it changed from silver
to yellow. It is important to avoid overheating the object. If
silver is overheated, the gold discolours or even disappears
into the substrate. This phenomenon restricts the maximum
firing temperatures to approximately 350 °C. A firmly bonded
but porous, matte gilded layer will form, which must then be
burnished. This technique is still used in Nepal (Anheuser
1997; Oddy 2000). In the Roman period, fire gilding was
considered by Pliny the Elder (first century AD) to be a costly
and rarely utilised method. However, it became the standard
method of gilding in the third–fourth centuries AD and con-
tinued to be used throughout medieval Europe, until the in-
vention of electroplating in the mid-nineteenth century AD
(Lechtman 1971; Lins and Oddy 1975; Oddy 1981,1988,
1991,1993,2000). As such, the presence of mercury is com-
mon in the gilding of third century AD Roman objects, but
rare in the gilding of earlier Roman objects. This may be
because supplies of mercury became more available for com-
mon use in the third century AD. Another method of fire
gilding is to apply a layer of mercury to the metal surface to
be gilded and then lay pieces of gold leaf on top. The gold leaf
dissolves in the mercury, creating a gold amalgam in situ, after
which the object is heated and burnished. This method is still
used in Japan (Anheuser 1997;Oddy2000). Anheuser’s
(1997) experiments showed that 8–25% of mercury is retained
during fire gilding and can be detected later on. The typical
macroscopic features of fire gilding, such as gold spreading
over the edge of the gilded area, splashes of gold on ungilded
areas and thicker gold deposits in engraved lines, were ob-
served on the Seuso objects (Fig. 5a–d). Fire gilding was the
typical gilding method used on other contemporaneous late
Roman silver hoards (Lang et al. 1984;Feugère1988;
Hughes et al. 1989; Cowell and Hook 2010; Hook and
Callewaert 2013;Doračićet al. 2015; Lang and Hughes
2016;Greiff2017;Vulićet al. 2017).
The two types of gilding on the Seuso objects were also
supported by Mango and Bennett (1994), using mercury in
both cases: (i) a gold amalgam was prepared and rubbed onto
the surface ofthe object, after which the object was heated and
the mercury evaporated; (ii) the surface of the object was
amalgamated by rubbing mercury on to it or by dipping it into
a solution of soluble mercury salt, and then gold leaf (some-
times several layers) was laid on top, after which the object
was heated as before. It was thought that the Geometric Ewers
were gilded by the first method, whereas the Dionysiac Ewer,
Animal Ewer and the vessels of the Hippolytus set were dec-
orated with the second method. The gilding of the Amphora
was too worn to determine the method used (Mango and
Bennett 1994). Our present data do not support the use of fire
gilding for the Geometric Ewers, as mercury is always detect-
able in fire gilding (Anheuser 1997) but is absent from the
Geometric Ewers. Further invasive investigations are planned
to confirm whether diffusion bonding was used on the
Geometric Ewers. It is possible to bond gold leaf to pure silver
(or to pure copper) without the use of an adhesive, by burnish-
ing and minimally heating the object to promote interdiffusion
between the gold and silver. Diffusion bonding (or hot clad-
ding) was invented as early as 1200 BC, and was commonly
used on silver from the late Hellenistic and early Roman pe-
riods (Lechtman 1971;Oddyetal.1981;Oddy1981,1988,
1991,1993,2000). This method of gilding is thus far not
found on Roman silver objects from the fourth century AD.
However, microscopic examinations of Roman objects from
the Chaourse (second–third centuries AD) and Mâcon
Treasures (third century AD) (Hughes et al. 1989), as well
as of several earlier objects (e.g. an Elamite dish and a
Parthian bowl) (Oddy 1988), revealed the presence of diffu-
sion bonded gilding on these objects.
The lack of mercury could indicate some sort of restoration,
during which gilding could be lost due to, e.g. repeated an-
nealing, and was subsequently replaced. If the lack of mercury
would indicate some restoration, then it is highly unlikely that
the completegilding of the Geometric Ewers was restored and
no sign of restoration was found on the other Seuso objects.
Moreover, based on the description of the restoration process
performed in 1989 (Mango and Bennett 1994), no such resto-
ration, which would provide enough heat to drive off the mer-
cury, was performed on the Seuso objects.
Higher gold concentrations were measured at several
points on the Animal Ewer, in places where gilding could
not be seen by the naked eye (Fig. 5a, b). Mercury was also
detected at these points. These are residues of former gilding,
in which the gold diffused into the silver, but the gilding
became worn over time.
Assembling of the objects—joining techniques
There are several ways to join the different parts of a compos-
ite silver object: (i) make simple linkages by folding the edges
of the metal; (ii) use pins, rivets or twisted components; or (iii)
create a joint by applying heat to metal (e.g. welding, casting
on, sintering, brazing and soldering). Both brazing (or hard
soldering) and soft soldering require the use of filler metal,
such as low-temperature lead-tin soft solders, high-
temperature silver-copper hard solders and intermediate tem-
perature alloys of silver and mercury or of silver and tin (Lang
and Hughes 1977,1984,1988).
The various parts of the composite Seuso objects were
assembled in three different ways. The bases of the
Hippolytus and Geometric Ewers were mechanically attached
Archaeol Anthropol Sci (2021) 13: 83
83 Page 16 of 20
Content courtesy of Springer Nature, terms of use apply. Rights reserved.

to the body by inserting the bases of the ewers into a hole in
the foot and hammering the metal (Mango and Bennett 1994).
The handles, lids, feet and thumbpieces were attached with
using lead-tin soft solders (Fig. 6). Lead-tin soft solders were
also used for ancient repairs (e.g. on the body of the
Amphora). The upper beaded and octagonal rims were at-
tached to the body with silver-copper hard solders, indicated
by the presence of green copper corrosion products (Fig. 6).
The use of these soldering materials was common in the late
Roman period (Lang and Hughes 1988). Hard soldering oc-
curs at a higher temperature, which may be near to the melting
point of the body metal. In contrast, soft soldering requires a
lower melting point alloy and occurs at a much lower temper-
ature than the melting point of the body metal (Lang and
Hughes 1977). The temperature range of the solders available
to ancient Roman craftsmen varied from the melting point of
silver (960 °C) to Tinman’s solder containing 66% tin and
34% lead, which is very close to the eutectic point of the
system (183 °C) (Lang and Hughes 1984). The differences
in the chemical compositions of the soft solders potentially
indicate the use of different soldering alloys and different
working temperatures. The behaviour of a solder primarily
depends on its composition, as well as on the conditions under
which the soldering is performed (e.g. temperature, surface
finish, flux, reducing or oxidising atmosphere). If several op-
erations must be executed, the highest melting point solders
must be used first (Lang and Hughes 1988).
Conclusions
Non-destructive handheld X-ray fluorescence spectrometry is
a useful tool in the determination of the chemical composition
of composite silver objects, if a significant number of analyses
are performed and the same instrument is used for the mea-
surements. With enough analyses, the inhomogeneity
amongst the various parts of the objects and the similarities
and differences between the objects can be revealed, and the
objects can be classified. Moreover, raw materials,
manufacturing and decoration techniques used can be
characterised, which help to better reconstruct past technolog-
ical practices and craftsmanship.
The chemical composition of the objects of the Seuso
Treasure shares similarities with other late Roman period sil-
ver finds. The differences in the chemical composition of the
various parts of the composite objects are clear evidence that
different ingots of silver were used for each part, which sup-
ports the earlier technological observations (Mango and
Bennett 1994). The different copper contents explain the use
of intentional alloying. The constant gold content implies that
the objects were not manufactured from reused or remelted
scrap silver. The likewise constant and low lead content indi-
cates the use of cupelled silver. Based on the Bi/Pb ratio the
objects can be categorised, which suggests that different silver
ingots were utilised. The ewers were constructed in two ways:
(i) the base and the body were made separately, or(ii) the base
and the body were raised or cast from a single silver sheet. The
composite objects were assembled following three methods:
(i) mechanical attachment, (ii) lead-tin soft solders or (iii)
copper-silver hard solders. Two types of gilding were used
for decoration, one with remnants of mercury (fire-gilding)
and another without mercury (presumably diffusion bonding).
The results of previous studies performed on the Seuso
objects were interpreted and new observations were made,
specifically, that the chemical composition of every part of
every object (including the Toilet Casket and Hippolytus
Ewer) was determined, that the gilding and soldering of each
object were identified. Regarding the Geometric Ewers, diffu-
sion bonding was likely used instead of fire gilding, as previ-
ously hypothesised. The hXRF data serve as a guide with
which to select sites to sample (with minimal invasiveness)
for further lead isotope and bulk elemental composition anal-
yses, the results of which will be published in a subsequent
paper.
Supplementary Information The online version contains supplementary
material available at https://doi.org/10.1007/s12520-021-01321-4.
Acknowledgements The hXRF measurements were performed within
the framework of the Seuso Research Project supported by the State of
Hungary from 2014 to 2019. The authors are grateful to Balázs Lencz,
Tamás Szabadváry and András Szabó at the Hungarian National Museum
for their help during hXRF analysis. Ariana Gugora is thanked for proof-
reading the manuscript. Furthermore, the authors are thankful to Mária
Tóth, Norbert Németh and Balázs Lencz for providing the silver reference
materials.
Funding Open access funding provided by ELKH Research Centre for
Astronomy and Earth Sciences.
Open Access This article is licensed under a Creative Commons
Attribution 4.0 International License, which permits use, sharing, adap-
tation, distribution and reproduction in any medium or format, as long as
you give appropriate credit to the original author(s) and the source, pro-
vide a link to the Creative Commons licence, and indicate if changes were
made. The images or other third party material in this article are included
in the article's CreativeCommons licence, unless indicated otherwise in a
credit line to the material. If material is not included in the article's
Creative Commons licence and your intended use is not permitted by
statutory regulation or exceeds the permitted use, you will need to obtain
permission directly from the copyright holder. To view a copy of this
licence, visit http://creativecommons.org/licenses/by/4.0/.
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