Archaeological and Anthropological Sciences (2020) 12:190

https://doi.org/10.1007/s12520-020-01140-z

ORIGINAL PAPER

Ceramic chronology by luminescence dating: how and when it is

possible to date ceramic artefacts
Anna Galli 1,2 & Emanuela Sibilia 2 & Marco Martini 2

Received: 15 January 2020 / Accepted: 24 June 2020

# Springer-Verlag GmbH Germany, part of Springer Nature 2020

Abstract
This paper is intended as a compendium of good practices to assess whether luminescence dating can provide researchers with
valuable chronological information for ceramic samples. It is organized into two main sections. The first section provides an
introduction to luminescence dating, including its physical principles, the applied measurement procedures, and a brief summary
on a new dating technique (RHX) not based on luminescence. This section aims to provide non-specialists with a background on
the physical principles underlying luminescence dating, in order to enable an understanding of the issues that may affect the
reliability of luminescence ages and a critical assessment of the results from luminescence laboratories. The second section
presents a series of case studies which illustrate the use of these methods, how they can be applied, and what results can be
obtained.

Keywords Luminescence dating . TL . OSL . Chronological context

Premise ceramic firing (Gliozzo 2020b); the investigation of different

This paper seves as an anchor to the Topical Collection (TC)
“Ceramics: Research questions and answers” aimed at guid-
ing researchers in the study of archaeological ceramics from
excavation to study and preservation in museum collections.
Each contribution has a tutorial approach covering one of
the main issues pertaining to the study of ceramics: research
questions and sampling criteria (Gliozzo 2020a); the chemical
(Hein and Kilikoglou 2020) and mineralogical-petrographic
(Montana 2020) investigation of raw materials; the technolog-
ical character and suitability of raw materials (Gualtieri 2020);
the processing (Eramo 2020) and modelling (Thér 2020) of
clays; surface finishing (Ionescu and Hoeck 2020) and
coatings such as black glass-ceramic (Aloupi-Siotis 2020),
terra sigillata (Sciau et al. 2020), and glazes (Pradell and
Molera 2020); the isotopic study of particular types of prod-
ucts such as Chinese high fired ceramics (Henderson et al.
2020); the identification of post-burial transformations
(Maritan 2020); the dating of ceramics (this paper); and the
restoration and musealisation of ceramics (de Lapérouse
2020). This Topical Collection concludes with a tutorial on
statistical data processing (Papageorgiou 2020).
Introduction

This article is a Topical Collection on Ceramics: Research questions and One of the most often encountered issues in the field of the
answers Cultural Heritage is the dating of artefacts. In fact, this is a
fundamental point representing the typical intervention of sci-
* Anna Galli entific methods in supporting archaeological approach or the
anna.galli@unimib.it History of Art in other fields, typically when dealing with
dating paintings, frescoes, and buildings, to mention only
1
Istituto di Bioimmagini e Fisiologia Molecolare, Consiglio Nazionale those that are most often encountered.
delle Ricerche, IBFM-CNR, via F.lli Cervi 93, 20090 Segrate, (MI), Why is it important to date a ceramic artefact? Firstly, by
Italy
setting it in a chronological context, it is possible to under-
2
Dipartimento di Scienza dei Materiali, Università Milano-Bicocca, stand its significance in relation to previous and successive
via R. Cozzi 55, 20125 Milan, Italy
events. Furthermore, in many cases, we wish to understand
 190 Page 2 of 15
complex social and commercial relationships. Last, but not the
least, it contributes to the study of ancient civilisations.
In archaeology, the stratigraphic method allows a relative
chronological sequence (i.e. the stratigraphic matrix) to be
established, based on the physical relationships among layers.
Moreover, typological study of the finds may allow for abso-
lute dating (i.e. periodization) of the relative sequence, by
comparison with the chronological distribution of similar ob-
jects. Further indications can be derived from the study of
written sources or inscriptions, while comparison with other
artefacts that can be independently dated (e.g. coins) can ac-
curately specify the dating sequence obtained by stratigraphy.
However, well-preserved and perfectly datable coins are
not frequent, while ceramic is the most widespread material
in almost all archaeological excavations (see Gliozzo 2020a
and the references therein). Consequently, pottery and
stamped bricks are the most precious materials for the period-
ization of the stratigraphic sequence. On the other hand, there
are forms that have been produced over such a geographical
and chronological extension that they cannot be used as indi-
cators for narrow chronological frames or limits (i.e. terminus
ante quem or post quem). A major step forward in solving
such problems came in the second half of the twentieth cen-
tury, when archaeological methods began to be supported by
dating techniques such as dendrochronology (Hillam 2004),
radiocarbon (Arnold and Libby 1949), and thermolumines-
cence (Aitken et al. 1964; Aitken et al. 1968; Aitken 1985).
All of these experimental methods, with few exceptions, are
based on the measurement of physical quantities whose values
are associated, with certainty, to the time variable.
Dating an artefact using a scientific technique is based on
the presence of a kind of “clock” inside the object to be dated
and an event that “starts the clock”. The case of radiocarbon
(14C) is typical, whose concentration in an artefact of organic
origin diminishes from the death of the living being, such as a
tree that originated an artefact itself, for instance, a wood
sculpture. In this case, the “clock” is the radiocarbon concen-
tration and the starting event is the death of the living being.
Two cases are probably the best-known examples of dating
possibilities in the field of Cultural Heritage: the above-
mentioned radiocarbon (14C) and thermoluminescence (TL).
It is to be noted that both of these methods rely on radioactiv-
ity, either that produced in the high atmosphere by cosmic
radiation (in the case of radiocarbon), or by the continuous
low level of irradiation due to the ubiquitous presence of nat-
ural radioactivity (as we will see in the case of thermolumi-
nescence). While, for 14C, the organism that is the origin of the
artefact needs to cease living to make the clock starts, TL is
started by high-temperature heating in a kiln.
Interestingly, 14C and TL are rather complementary, in that
radiocarbon dating can be applied to organic materials (i.e.
artefacts that are derived from living organisms such as wood,
tissues, and bones). However, TL is currently applied to
Archaeol Anthropol Sci (2020) 12:190
inorganic artefacts, typically to ceramics. In this paper, we will
consider the latter technique, together with its characteristics,
precision, and limits, along with giving some examples. Other
alternative methods for dating ceramics will be introduced.
Studies on ceramics deal with the investigation of their
overall life cycle, from the acquisition and processing of raw
materials to production and distribution, through their use,
reuse, and discard. Such investigations include both the recon-
struction of the life cycle and its interpretation in terms of the
people producing, distributing, and using the artefacts.
Thus, such reconstruction involves establishing how,
when, and where the artefacts were made; to which use they
were conceived; where they were distributed; and how they
were used. We attempt, in this paper, to illustrate how the
question of “when” can be answered by means of scientific
techniques, briefly summarizing the present state of the art and
presenting the recent development of novel techniques.
TL dating, with its peculiar characteristics and applications
to ceramics, will be the main topic of this paper; however, it
must be mentioned that another luminescence technique has
been increasingly used in ceramics dating, optically stimulat-
ed luminescence (OSL), which will be introduced when deal-
ing with TL.
Another dating method which has not yet been fully tested,
but which has shown great potential for ceramics dating, is
rehydroxylation (RHX; Wilson et al. 2009). RHX is based on
the recombination over time of hydroxyl (OH−) groups in the
ceramic structure. The state-of-the-art RHX application to ce-
ramics dating is briefly summarized below.
For ceramics belonging to an archaeological site, dating ob-
tained by scientific techniques is used as a terminus post quem
and combined with the stratigraphic sequence, in order to frame
the life of the excavated site into an absolute chronological range.
The case of ceramics from museum collections is different
as, in most cases, a lack of information on the finding context
prevents precise and accurate dating: as we will see in the
following, sufficient precision in TL dating can be achieved
only when considering ceramics taken in their excavation con-
text. In fact, TL implies uncertainties in the calculated age,
mostly due to the level of information about the environment
where the piece of art comes from. When the object to be
dated is extracted from the place where it has been for centu-
ries, the information of its environment is almost completely
lost. This does not completely rule out the possibility of de-
termining an approximate chronological age, but the level of
precision is strongly reduced. Notwithstanding, it is possible
to determine at least the authenticity of the considered object,
as a recent forgery gives a very low level of TL (if any), while
an authentic piece has always a relatively high level of TL.
It must also be considered that only measurements of the
level of TL can support (or not) the clues about the authentic-
ity coming from some artistic feature, or aspect of composi-
tion and manufacturing style.
Archaeol Anthropol Sci (2020) 12:190 Page 3 of 15 190

How can luminescence help

in the chronological assessment of ceramics?

A great deal of materials, when variously stimulated, emits a

generally very weak amount of light which is currently known
as “luminescence”. A particular kind of this phenomenon is
phosphorescence, a delayed emission of light from crystalline
materials following the absorption of energy from an external
source. It is to be noted that phosphorescence is supported by
heat, in the sense that the emission of light is accelerated when
the temperature is raised. As a consequence, thermolumines-
cence can be considered a particular case of phosphorescence:
insulating crystals absorb a small amount of energy when hit
by ionizing radiation and give back this energy, in the form of
light (the luminescence), under further suitable stimulation.
When this stimulation is given by heat, we are dealing with Fig. 1 Typical glow curves of roman ceramics. To prepare the sample
thermoluminescence (TL). There is another way of supporting the fine grain technique was applied. (1) Background. (2) Response to
phosphorescence: if an irradiated material is stimulated by natural dose. (3) Response to 4 Gy of beta irradiation added to the natural
one. (4) Response to 8 Gy of beta irradiation added to the natural one
light, we consider it to be OSL.
TL is typically used for dosimetric measurements; that is,
the measure of the amount of radiation absorbed (called the intensity of the emitted light. Provided that the intensity of light
“absorbed dose”) by an object or person. Materials such as is proportional to the amount of energy absorbed during the
LiF TLD badges are used to measure the radiation dose that a interaction of ionizing radiation with matter, luminescence can
worker may receive while attending patients undergoing ther- be exploited as a dosimetric technique.
apeutic or diagnostic procedures with radionuclides or while This very same characteristic suggests the possibility of
working with x-ray-generating devices. dating ceramic objects by exploiting the TL properties of their
A particular dosimetric system lies at the basis of TL dat- crystalline inclusions. This was first proposed by Daniels et al.
ing. Small crystalline inclusions are practically always pres- (1953), Grögler et al. (1958), and Kennedy and Knopff
ent, to different extents, in all clays and thus in ceramics, (1960), exploiting the fact that the high temperatures (>
which act as dosimeters. Typically, quartz and feldspar are 500 °C) reached by pottery during firing in a kiln has the effect
the minerals most present in clay which are most suitable for of erasing the constituent mineral grains of any previously
dating. The external source of energy can be of different kinds accumulated dose. Further extensive studies by the group of
but, for dating purposes, the sources of irradiation are natural- at Oxford University headed by Martin Aitken (1964, 1968)
ly occurring ionizing radiation, mainly given by the radioac-
tive families of uranium, thorium, and 40K; a smaller contri-
bution is also being provided by 87Rb and cosmic rays. The
presence of such a natural radiation environment results in the
continuous irradiation of any object on Earth. In non-metallic
materials, this causes an accumulation of energy in the form of
trapped electrons. Their release requires the above-mentioned
stimulation, either heat (giving origin to TL) or light (resulting
in OSL).
TL is measured by heating a sample from room tempera-
ture to about 450 °C at a constant rate, while simultaneously
recording the emitted light. The result is a so-called glow
curve (see Fig. 1).
OSL is, instead, measured by illuminating the sample with
light of suitable wavelength, recording the light (having dif-
ferent wavelength) emitted consequently. The resultant curve
is called a shine-down curve (see Fig. 2). Fig. 2 Typical shine-down curves of roman ceramics. To prepare the
sample, the fine grain technique was applied ( Experimental
In principle, the application of luminescent materials to the conditions: PH 200 °C for 10 s, blue LED stimulation at 470 ± 30 nm).
dosimetry of ionizing radiation relies on the relationship between (1) Response to natural dose. (2) Response to 4 Gy of beta irradiation. (3)
the amount of absorbed energy (the absorbed dose) and the response to 8 Gy of beta irradiation
 190 Page 4 of 15
found that the luminescence intensity emitted by the pottery
samples is proportional to the age of the sediments from which
the samples were obtained, in agreement with the dates ob-
tained by radiocarbon. This result led to further refinements in
the dating protocols (Aitken 1985) and, from 1970 to 1990,
TL dating became available in many laboratories, reaching
high and undisputed reliability among archaeologists (Fig. 3).
A further impulse in luminescence studies occurred when
TL dating was used to date unheated sediments, due to the
capability of sunlight to erase, during the natural transporta-
tion of the mineral grains, previously accrued energy (Wintle
and Huntley 1979). In this case, the dated event is the last
exposure to sunlight before sedimentation. It has been dem-
onstrated that the exposure of sediments to sunlight may act
similarly to heating in pottery, reaching a similar zeroing ef-
fect on the previously accumulated energy in sediment grains.
Zeroing by sunlight is also usually referred to as “optical
bleaching”. However, the understanding of the process of so-
lar resetting of sediments was still problematic, and the accu-
racy of TL ages not so satisfactory.
Another fundamental step in luminescence dating was due
to Huntley et al. (1985), who reported that a light source could
stimulate energy release from a dosimeter during measure-
ment, instead of the heating used in TL. This led to the devel-
opment of OSL dating, which offered a number of advantages
over TL methods when dating unheated sediments. The tech-
nique has been greatly developed (Wintle 1997; Bøtter-Jensen
et al. 2003a; Bøtter-Jensen et al. 2003b), and is presently the
method of choice for dating detrital sediments of Late
Pleistocene and Holocene age. OSL can be used to date pre-
viously heated archaeological artefacts as well, similar to TL.
Fig. 3 At the 39th International
Symposium on Archaeometry:
“50 years of ISA”, Leuven,
Belgium, 28 May–1 June, 2012,
the team of Milano Lab with
Martin Aitken, considered the pi-
oneer scientist in luminescence
dating. From left to right:
Francesco Maspero, Anna Galli,
Emanuela Sibilia, Martin Aitken,
and Marco Martini
Archaeol Anthropol Sci (2020) 12:190
However, not much work has been carried out so far for OSL
ceramics dating (Barnett 2000; Guibert et al. 2001; Hong et al.
2001; Oke and Yurdatapan, 2000; Bortolussi et al. 2013), and,
often, ceramic materials produce OSL signals which are
weaker than the TL ones (Oke and Yurdatapan, 2000); fur-
thermore, heated and unheated materials may behave differ-
ently (Barnett 2000).
Comparing TL and OSL, we can conclude that, so far, TL
is still the most reliable method when dating heated ceramics,
while OSL is the best choice for dating sediments generally in
the field of Earth Sciences.
In luminescence dating, the light emitted by minerals follow-
ing heat or light stimulation is measured in a laboratory using
purposely designed instrumentation. The amount of light is
compared with the analogous emission following irradiation
given in the laboratory using calibrated radioactive sources, as
is shown in Figs. 1 and 2. By appropriate calculations, it is
possible to determine (with rather good precision) the amount
of absorbed dose during the centuries, which is referred to as the
“palaeodose”. In order to determine the age, the rate at which
such a dose was accumulated (i.e. the “dose-rate”) must be
measured as well. The ratio of the two quantities (see Eq. 1)
gives the age, that is, the time since the most recent heating to
high temperature of the dated object, generally corresponding
to its burning in a kiln, whether using TL or OSL.
Luminescence age ¼ palaeodose=dose‐rate ð1Þ
Typical values of palaeodose range from fractions of Gray to
a few tens of Gray.1 The dose-rate, generally reported as the
absorbed dose per year (the so-called annual dose-rate), usually
ranges from 1 to 10 mGy/year, as radioactivity concentrations
Archaeol Anthropol Sci (2020) 12:190
vary between different ceramics and soils. α and β radiations,
which are characterized by very short ranges, come from the
internal radioactivity of the ceramic itself while the environ-
ment contributes with γ radiation, which has a much higher
range, in the order of tens of centimetres and coming from all
around the sample. Besides, a minor contribution from the ubiq-
uitous cosmic rays is always present.
A synthetic account of the luminescent phenomenon refers
to the energy band theory in solid-state physics (Aitken 1985;
Aitken 1998; Chen and McKeever 1997). Ionizing radiation
excites electrons from the valence band (or ground state)
across an energy gap to the conduction band. In ideal crystals,
energy levels within the gap cannot be occupied but defects
allow metastable energy levels within the forbidden gap,
which can trap excited electrons or electron vacancies (holes).
Traps are emptied of these charge carriers by stimuli from
additional energy sources, such as heat or light. The probabil-
ity of escape, p, is governed by an Arrhenius relationship
which, for TL, is expressed as:
p ¼ sexpð−E=kT Þ
where s is a frequency factor; E is the trap depth (in eV unit),
which is the amount of energy required to move an electron
from the trap to the conduction band (or a hole to the valence
band); k is Boltzmann’s constant; and T is the absolute tem-
perature (in Kelvin). Equation (2) highlights that the probabil-
ity of an electron escaping out of a trap increases exponential-
ly with the temperature T. This explains why, for traps deep
enough, the probability of being emptied is negligible at room
temperature, while they can promptly release electrons when
the temperature is strongly increased.
A much more complex picture is relative to OSL, where the
phenomenon is heat-assisted, in the sense that the measure-
ment of the emitted luminescence under light stimulation is
strongly dependent on the temperature at which it is carried
on. Furthermore, trap emptying by light depends on the ener-
gy (i.e., the wavelength) of the stimulating light.
For OSL, additional terms related to the intensity of the
light and the ability of the trap to absorb particular wave-
lengths are required. Upon escape, the charge carrier may
recombine with opposite charges in other defect sites (known
as recombination centres), and, consequently, luminescence is
emitted. For a more detailed treatment of OSL mechanisms,
we refer to specific literature (see, e.g., Aitken 1998 and
Murray and Wintle 2000).
Thermoluminescence and optically stimulated lumines-
cence dating can, in principle, be applied to all materials
whose manufacturing requires high-temperature heating, typ-
ically, all kinds of ceramics; bricks; burnt flints; porcelains;
1
Gy is the SI unit of absorbed dose corresponding to 1 J/kg.
Page 5 of 15 190
cooked grounds; hearths; bronze clay-cores; and, tentatively,
mosaic glasses and metal melting by-products.
TL and OSL are absolute dating techniques, in that they do
not need comparisons with other objects or materials which
have been independently dated.
They are micro-destructive: the material that must be sam-
pled for each dating is on the order of 1 gramme. However,
measurements of the radioactivity content need an even higher
quantity of material.
The time interval in which the techniques can be applied
corresponds, in practice, to the entire period of ceramic
production—from a few tens of years to several thousand
years before present. For burnt flints and stones, the indicative
time interval is even larger, spanning from around 1000 to
more than 300,000 years ago.
TL dating is generally very meaningful in archaeological
excavations containing both organic and ceramic materials,
allowing for comparison between TL and radiocarbon dating
results. It is particularly useful in the cases and contexts in
which the radiocarbon technique is not applicable, both for a
ð2Þ lack of organic findings and for ages exceeding the radiocar-
bon limit (about 40,000–50,000 years). TL is also of great
help in dating cultural contexts characterized by the radiocar-
bon “plateau effect”, as happened in the first iron age; the so-
called Hallstatt plateau (Jacobsson et al. 2018). Furthermore,
after around 1700 CE when, following the industrial revolu-
tion, the release of high amounts of CO2 from the combustion
of fossil coal and oil occurred; as a result, there has been a
remarkable decrease in the concentration of 14C in the atmo-
sphere (the Suess effect, Keeling 1979), which prevents radio-
carbon dating of artefacts younger than about 300 years.
Consequently, TL is the main dating technique for the period
from 1700 CE on.
TL dating in more detail
Looking at the age Eq. (1), it can be seen that TL dating
requires the knowledge of two main quantities: the palaeodose
and the annual dose-rate. A short account of how they are
measured is summarized in the following, starting from a
few considerations about sampling.
Some practical tips for correct sampling
An important part of using luminescence dating in practice is
designing an appropriate sampling strategy. This is
constrained by the suitability of materials available at the site
but, ultimately, it is essential that the strategy is driven by a
clear idea of the archaeological question that is being asked.
As stated in the next paragraph, the dose-rate to the sample
is derived from both the ceramic and the surrounding soil. The
outer 2 mm of the sample is removed in the laboratory, such
 190 Page 6 of 15
that the beta dose-rate originates entirely from within the sam-
ple: thick shards are needed for this, and most laboratories
prefer ≥ 10 mm thick and 30 mm across. Therefore, the
amount of sample needed for dating is not negligible.
Moreover, at least three samples per layer are required. As
the surface is removed in the laboratory, the shard does not
have to be protected from light; thus, it can be washed and
recorded in the normal way prior to the dating procedure. A
close specimen of burial soil is also requested, if the environ-
mental radioactivity is not directly measured on site.
As the TL age is proportional to the radiation dose, radiog-
raphy must either be avoided or taken after sampling opera-
tions. Airport security X-ray devices impart a small radiation
dose, and their effect is negligible, in most cases.
How natural radioactivity is on the basis of
luminescence dating
The annual dose-rate is due both to the internal radioactivity of
the ceramic itself and to the environmental radioactivity, along
with a contribution due to cosmic rays. The main natural ra-
dioactive elements responsible for irradiating the ceramics are
isotope 40 of potassium and the radioactive families of thori-
um and uranium, which are present in concentrations on the
order of a few parts per million. They decay by emitting alpha
and beta particles and gamma radiation, which are responsible
for the ionization processes in the matter they pass through.
The depth of penetration of radioactive particles depends on
their type and energy. In quartz and for the decay products of
natural radioisotopes, the depth is a few tens of microns, some
millimetres, and tens of centimetres for alpha, beta, and gam-
ma radiation, respectively. Considering a ceramic fragment
buried in the ground, the alpha and beta particles that irradiate
the luminescent crystalline inclusions come from the radioiso-
topes contained in the ceramic itself, while the gamma radia-
tion comes from the outside. As already mentioned, typical
values of total absorbed dose are between less than 1 Gy and
some tens of Gray, while the annual dose-rate can vary be-
tween 1 and more than 10 mGy/year.
There are various techniques for measuring the annual
dose-rate. Some allow us to determine the alpha, beta, and
gamma components of the annual dose-rate from the measure-
ment of radioactive element concentrations: in particular,
gamma spectroscopy, alpha and beta activity measurements,
chemical analysis, and neutron activation are typically used.
The concentrations of uranium and thorium can be measured
by total alpha activity counting and potassium can be deter-
mined chemically by flame photometry. Gamma spectrometry
analysis also allows us to obtain the concentrations of all the
radioactive elements present in the sample and/or soil. From
these values, the various components of the annual dose-rate
are obtained using specifically calculated conversion factors.
Archaeol Anthropol Sci (2020) 12:190
With regard to the gamma and cosmic ray environmental
contributions, an alternative approach consists in the direct
measurement of the dose. Placing some dosimeters of sensi-
tive material in place of the ceramic to be dated for a few
months, the external dose value to which it was exposed is
recorded directly, without having to measure the concentra-
tions of ambient radioactivity (Aitken 1985).
The fundamental hypothesis on which these considerations
are based is that the annual dose-rate that is measured today is
a reliable estimate of the value of this quantity in the past. As
the ionizing radiation is the product of decay, the radioactivity
concentrations decrease and, thus, the annual dose. The hy-
pothesis would therefore seem to be incorrect in principle. It
is, however, necessary to consider the rate of decrease in nat-
ural radioactivity, whose half-life (i.e. the time that must
elapse in order to reduce its concentration to half its value) is
on the order of 109 years. For times of archaeological interest
(102–104 years), the variations in radioactivity concentrations
can, therefore, be neglected.
There are other possible causes of variation of the dose-
rate, due to radionuclide movements in the environment, to
disequilibrium in the radioactive series, to the escape of gas-
eous elements such as radon and thoron, or to the addition of
potassium fertilizers in an agricultural environment. Another
problem that affects the absorption of radiation is the water
content in the ceramic over time. It must be considered, in fact,
that it is necessary to measure the radioactivity concentration
in the ceramics and soils, in order to calculate the absorbed
annual dose-rate, as discussed above. However, part of the
energy released is absorbed by water, rather than by the ce-
ramics. In this respect, the normal fluctuations of soil moisture
related to the seasons and, to a greater extent, alterations due to
climatic, geological, or anthropic variations of the site can
determine variable concentrations of water in the ceramic mix-
ture, altering its density. Given the difficulty in estimating the
existence and extent of these changes, it is necessary to take
this into account by introducing specific margins of uncertain-
ty, which are added to the uncertainties associated with the
specific technical measurements of the annual dose.
Measurement of the palaeodose
Two main TL dating techniques have been developed, by
exploiting different radiation absorptions according to the size
of the mineral grains.
Pottery generally comprises a mixture of burnt clay and
coarser grained materials used to temper the pot. Providing
that the ceramic was fired to a sufficiently high temperature
when it was manufactured, TL measurements can be made on
either fine clay particles or on sand-sized quartz inclusions in
the temper.
The inclusion technique (Bell 1979) considers exclusively
quartz grains, a material having well-known TL characteristics.
Archaeol Anthropol Sci (2020) 12:190
Through magnetic separation or by deposition in heavy liquids,
grains approximately 100–200 μm in diameter are selected
from the ceramic body. These inclusions are then chemically
treated with hydrofluoric acid to eliminate the surface layer,
which is the only part of each grain hit by alpha radiation. For
grains treated in this way, the total absorbed dose is exclusively
due to beta and gamma radiation, eliminating the need to eval-
uate the TL production efficiency of alpha particles; which is,
on average, one order of magnitude less than the beta and
gamma radiation.
However, this technique has some disadvantages, such as
the high amount of material needed and the difficulty of pre-
paring homogeneous material samples and/or normalizing
their TL response to unit doses of artificial radiation.
Furthermore, the elimination of the alpha contribution from
TL means that the gamma component of the external dose
becomes relatively more significant, enhancing the impor-
tance of precise evaluation of the environmental contribution.
The second main technique is the fine grain technique
(Zimmermann 1971), which uses all the material that is obtain-
ed by drilling the ceramic as it is with a low speed drilling. A
granulometric selection is then carried out by deposition in
acetone for appropriate times, to separate the fraction of particle
size roughly between 1 and 8 μm. For these dimensions, the TL
is produced by all the radiations in a homogeneous way
throughout the grain volume. The advantages and disadvan-
tages are, in some way, complementary to those of the inclusion
technique: the reproducibility of the signal is very high, but it is
necessary to accurately assess the relative TL efficiency of the
alpha particles and their contribution to the annual dose-rate.
In both techniques, the measurement of the palaeodose is
obtained by comparing the TL signal accumulated from firing
to present with that induced by irradiation performed in the
laboratory with calibrated artificial radioactive sources (see
Fig. 1). The accuracy of this evaluation depends on the repro-
ducibility of repeated measurements and precision in the cal-
ibration of the radioactive sources. In most cases, the uncer-
tainty associated with this evaluation is between ± 3 and ± 7%.
The uncertainty of ages
The accuracy range of TL dating (i.e. the time interval within
which the firing of the ceramic is most likely placed) is be-
tween ±5 and ± 10% of the measured age (Berger et al. 1987);
only in particularly favourable cases can this be reduced to ±
4% (Martini and Sibilia 2006).
It should be added that reduction of the uncertainty could
be obtained through the dating of more samples that are
known to be contemporary. By increasing the number of sam-
ples and carrying out the weighted average of the individual
dates, a statistically significant reduction of the absolute un-
certainty can be obtained.
Page 7 of 15 190
We emphasize that a fundamental point in any dating pro-
cess is correct sampling. It is mandatory to collect detailed
information on the geological context (including photographs
and detailed field notes), particularly concerning the environ-
ment of sedimentary deposition and sediment overburden (in-
dication of post-sedimentary disturbance, hiatuses, and sedi-
mentation cycles). Present and past hydrological conditions
(sediment moisture) of the sample need to be assessed, as far
as possible. The sample should be taken from a homogenous
layer with a thickness of about 30 cm. Alternatively, on-site
measurement of gamma radiation (using a portable gamma
spectrometer or a gamma counter) can be utilized to minimize
the impact of inhomogeneity on the dose-rate calculation. It is
strongly recommended that researchers with limited experi-
ence in sampling for luminescence dating should contact an
expert prior to sample collection, in order to obtain informa-
tion on the specific requirements.
Moreover, if prior information about the analyzed samples
and provenance sites are available, by applying the Bayesian
statistical approach (Buck et al. 1996), it is possible to contex-
tualize the archaeological problem into a coherent
interpretation.
The Bayesian approach incorporates the a priori knowl-
edge with the analyses; that is, it combines the a priori prob-
ability with the data and interprets the posterior probability.
Therefore, it is possible to reduce the error ranges found in
individual samples by conditioning the probability with exter-
nal links (Maspero et al. 2016).
Authenticity test
From the brief description of the TL technique, it should be
clear that the dating of a ceramic is a rather complex experi-
mental operation, which requires the evaluation of different
physical quantities and the knowledge of various environmen-
tal parameters. It is not possible to date objects out of their
archaeological context, as already mentioned in the
“Introduction” section, when considering pieces from mu-
seums. It is, however, possible to use TL to verify the authen-
ticity of ceramics, especially when the question is to ascertain
whether an object is only a few 10 years old or hundreds or
thousands of years old. In brief, what is the difference between
an authenticity test and dating a piece? Authenticity aims to
distinguish between an original piece and a modern copy.
Dating aims to give a precise historical date to an object.
Authenticity tests are directly derived from standard dating
techniques (Aitken et al. 1964). The amount of material need-
ed is quite small (a hundred milligrammes, on average) and is
obtained by making a small hole (3 mm in diameter) with a
low speed drill (Fig. 4).
This amount may be slightly reduced, in the case of ex-
tremely small objects. The measure of the total amount of TL
 190 Page 8 of 15
Fig. 4 Sampling operations in Milano Lab. The artefact is a Red-Figure
Amphora supposed to belong to the sixth–fifth cent. BC. In the inset, the
green arrow highlights the area from which the ceramic powder was
sampled
of the sample, as compared with the TL produced by artificial
irradiation in the laboratory, allows checking for its compati-
bility with the expected age, inferred from stylistic and histor-
ical elements. In other words, the TL test only tells if a vase is
antique or young, allowing us to distinguish between an orig-
inal piece and a modern copy.
The result of the test, which is normally of the YES/NO
type, is often of crucial importance: consequently, although
the accuracy of the measurement is not as important as in the
case of dating, its reliability must be very high and the test
must be carried out with the utmost care by qualified person-
nel. Consolidated experience and expertise are required to
perform correct authentication analyses and to avoid incorrect
answers. The possibility of contamination of the sample with
soil or surface deposits—despite being an obvious problem—
is often underestimated, as well as the presence of carbonates
in the mixture which give rise to spurious emissions (Martini
et al. 1988), which a non-expert operator may not correctly
identify, assigning authenticity to a modern piece whose TL
emission is spurious. If an object to be tested has been re-
stored, it is recommended to take more than one sample, as
the component parts may differ in age.
Archaeol Anthropol Sci (2020) 12:190
A new and promising ceramic dating
technique: the rehydroxylation procedure
Rehydroxylation (RHX) has been recently proposed as a new
chronometric dating tool for fired clay, including ceramics.
This technique relies upon the known characteristics of
reheated porous ceramic vessels to regain water through the
two-stage process of rehydration (reincorporation of water)
and rehydroxylation (reincorporation of hydroxyl OH −
groups), which produces an increase in the weight of the spec-
imen. The dating clock is provided by the experimental obser-
vation that the RHX reaction follows a precise kinetic law,
such that the weight increases with the fourth root of the time
elapsed since firing.
The method consists in measuring the slow progressive
uptake of hydroxyl OH− groups in a small cubic-fired clay
sample (parallelepiped with 0.5 cm side and 0.2 cm thickness)
with a gravimetric microbalance following its complete de-
hydroxylation at 500 °C. Being a gravimetric technique, it is
experimentally rather simple and, advantageously, self-cali-
brating. However, the extremely small weight variation re-
quires exceptional precision in the measurements.
Furthermore, to produce an accurate age, measurements must
be carried out at a temperature as close as possible to the one
the sample has experienced over its lifetime: both the geo-
graphical origin and the temperature history must therefore
be known, if possible.
So far, RHX is a method which is actively under develop-
ment (Wilson et al. 2009; Barrett 2013). Despite its conceptual
simplicity, its application is not straightforward. The weight
variation to be measured is extremely small, and non-RHX
processes may surreptitiously contribute to the mass changes.
Moreover, unanimously accepted experimental methods are
still lacking. For these reasons, RHX dating is not yet routine-
ly nor commercially available, being still the subject of several
research and validation studies.
TL at work: a few examples of applications
Some practical examples of applications of TL dating tech-
niques in various archaeological fields are reported in this
section. Our selection of case studies shows the diversity of
the problems involved and how TL dating can support archae-
ological and archaeometric research.
The unexpected age: possible interpretation
Thermoluminescence has been widely used for brick dating,
in order to reconstruct the building chronology of urban com-
plexes. However, it can be sometimes inconclusive, as TL
assesses the firing period of bricks which can be reused in
different structures, even several centuries later.
Archaeol Anthropol Sci (2020) 12:190
As previously mentioned, dating reused samples can give a
post quem dating element, which is often useless or redundant.
This was not the case for the Abbey of Pomposa (Codigoro;
DMS 44° 49′ 53.35″ N, 12° 10′ 34.2″ E; from the Google Earth
Application), one of the most interesting examples of
Romanesque architecture in Northern Italy (Di Francesco
2000). The innovative and exceptional decoration of its atrium,
made with differently coloured carved panels, has posed unan-
swered questions about its history and production technologies.
Thanks to restoration works, several samples from the inward-
facing side of such cotton ornamental panels became available
for dating analysis. Their dimensions were very close to the
Roman bricks made in Northern Italy up until the second cen-
tury CE, such that the reuse of Roman bricks in the construction
of Pomposa Abbey was widely agreed upon. Quite surprising-
ly, TL dating results (Bevilacqua et al. 1999) spanned from the
sixth to ninth century, none of them being Roman or coeval to
the atrium (1008–1046 CE). The decorations appeared, there-
fore, to have been made with reused bricks, produced during
the fourth–seventh centuries (Late Antiquity) and eighth–tenth
centuries (Early Middle Ages), suggesting that local ceramic
makers were working in continuity with the past in a period
when local production was only suggested. This result stimu-
lates a new approach to the study of local industry and trades
which hitherto had only been proposed, but not proven.
The contribution of luminescence to construct a
chronology
To illustrate the application of TL dating in an archaeological
context, we describe two typical cases of deep stratigraphic
excavation sites.
Real Alto, one of the oldest organized villages in South
America
The site of Real Alto (Valdivia culture, Guayaquil province,
Ecuador; DMS 2° 22′ 25″ S, 80° 42′ 32″ W; from the Google
Earth Application) is the oldest and most extensively studied
ceramics site in the New World (Estrada, 1965). It was devel-
oped over about 3000 years during the prehistoric Formative
period (5000–1000 BC). Its relative internal chronology (Hill,
1972–1974), based on ceramic stylistic indicators, consists of
eight main cultural phases. Valdivia potters produced 50 dif-
ferent vessel forms throughout the whole sequence, most of
them being very good time markers (Marcos 1998).
The absolute chronology of Valdivia civilisation was based
only on a few radiocarbon dates until 1990, when a joint
project among the Universities of Guayaquil, Barcelona, and
Milano, supported by the E.U. (Martini et al. 1991), applied
TL dating to several tens of ceramic samples from controlled
stratigraphic excavations (Marcos 1998a).
Page 9 of 15 190
The most recent evaluation of the Valdivia chronology is
that of Marcos (1998), who combined radiocarbon determina-
tions with thermoluminescence assays of Valdivia pottery to
form a revised absolute chronology for the eight phases of the
Valdivia sequence. Selected pottery samples served to aug-
ment the radiocarbon analysis by filling in gaps where reliable
radiocarbon determination was not available. The general TL
characteristics of the shards were particularly suitable for dat-
ing. They had high TL sensitivity and stability, linear behav-
iour versus artificial irradiation up to relatively high doses
(30–40 Gy beta and 350–500 Gy alfa), absence of spurious
TL (Martini et al. 1988), and free of anomalous fading (Wintle
1973). Consequently, a very high precision in palaeodose
evaluation could be obtained (4–5%). The maximum water
uptake of samples (saturation water) was low (less than 6%),
due to their very low porosity. External dose-rates were mea-
sured by in situ dosimetry (Martini et al. 1983) and a high
homogeneity of the external radiation field was observed.
Due to these favourable conditions, the uncertainties in
dose-rate evaluation were particularly low and the derived
uncertainties in the calculated ages were consequently limited
to 5%, which is typically seldom achievable.
By combining the two independent dating methods (TL
and 14C), the absolute chronology for Valdivia was deter-
mined, as provided in Fig. 5.
The chronology based on ceramic style and technology
(e.g. shape, decoration, and surface finish) was substantially
confirmed. The two independent results were in good agree-
ment, except for Valdivia I, VII, and VIII. While TL data for
Valdivia I were obtained from ceramics whose shape ap-
peared only during the end of phase I (Valdivia Ib), others
suggested that they antedate the respective phases by a couple
of centuries. TL results for the intermediate phases also
allowed for improvement of the accuracy of the ages mea-
sured by radiocarbon dating on samples collected from wall
trenches and food preparation pits, among other secure con-
texts and associations (Marcos 1998b).
Digging in Sipán
The second stratigraphic excavation site is the Sipán archaeo-
logical complex, also known as Huaca Rajada, whose chro-
nology has been very challenging to study. Sipán is located on
the north coast of Peru (DMS 6° 48′ 22.19″ S, 79° 36′ 3.59″
W; from the Google Earth Application) and is formed by
sacred pyramids (or huacas). It has been recognized as the site
of the Lord of Sipán, renowned for a magnificent funeral kit.
The Lord of Sipán was a warrior ruler who led the Moches,
who lived in Peru between the first and seventh centuries CE.
This finding proved to be an important milestone in the ar-
chaeology of the continent, as it was the first royal tomb of a
Peruvian civilization prior to the Incas which was found to be
intact. During the following excavation, many other tombs
 190 Page 10 of 15
Fig. 5 Comparison between TL
and radiocarbon (RC) Valdivia
chronologies. Probability density
plot of the analyzed samples
were found, documenting the development and decay of the
settlement.
Despite the importance and centrality of Sipán in the con-
text of pre-Hispanic art and Peruvian archaeology, it could not
be precisely dated due to the lack of a satisfactory relative
chronology and to conflicting radiocarbon results. The
PRODESIPÁN project (a collaboration between the Museo
de Tumbas Reales de Sipán, the University of Milan, and
the University of Milano-Bicocca), made it possible to take
samples of organic material and ceramic fragments in optimal
condition from several excavated tombs.
Several tens of TL and 14C dating results made it possible
to cross-reference the data with those of the relative chronol-
ogy to define in a quite precise way—as had rarely happened
in other Moche sites—the construction sequence of the whole
Funeral Platform. The results were elaborated according to
Bayesian models, reaching one of the most solid chronologies
Archaeol Anthropol Sci (2020) 12:190
ever reached in a Moche site (see Fig. 6). They clarified that
the funerary platform was built between 350 ± 40 CE and 660
± 20 CE and that the occupation of the site continued until the
Late Horizon (1476–1534 CE) and, possibly, to the First
Colonial Period. These results imply the correction of the
presently accepted chronologies for the end of Moche V; like-
wise, some chronological models of the Northern region of the
Moche culture must also be partially corrected (Aimi et al.
2016).
Disentangling various over-imposing civilisations at
the same site
Another interesting example in excavation archaeology is the
case of Bet Gemal (DMS 34° 58′ 35″ E, 31° 43′ 28″ N; from
the Google Earth Application), an Israeli village inhabited
Archaeol Anthropol Sci (2020) 12:190 Page 11 of 15 190

Table I Ceramics from the site of Bet-Gemal. TL dating results

Lab. reference Archaeological reference TL dating (mean ± σ)

D1618 (a–c) Area C: US 2074 260 ± 100 CE

D1619 (a–c) Area C: USM 2219 85 ± 110 CE
D1621 (a–c) Area C: US 2075 290 ± 110 CE
D1622 (a–c) Area C: US 2079 460 ± 100 CE
D1623 (a–d) Area C: US 2078 500 ± 90 CE
D1624 (a–c) Area C: US 2277 925 ± 70 CE
D1625 (a–c) Area C: US 2291 630 ± 70 CE
D1626 (a–c) Area C: US 2313 615 ± 80 CE
D1627 (a–b) Area C: US 2313 970 ± 70 CE
D1627 c 410 ± 100 CE
D1628 (a–c) Area C: room XV 945 ± 70 CE
D1629 (a–c) Area B: building K 995 ± 65 CE
D1630 (a–d) Area B: church 47 555 ± 85 CE

context of the Jewish–Roman Wars. For the two following

Fig. 6 Excavations at Sipán, Peru. Tomb 14 (detail)
from the second century BCE to the Islamic period (ninth
century CE).
The site displayed exceptionally well-preserved remains: a
Roman–Jewish quarter, a Christian Byzantine settlement with
several plants for oil and wine production, and an Islamic
dwelling place. Each group of remains is relative to different
chronological periods (Strus 2003). The archaeological evi-
dence allows for stating an approximate chronological inter-
pretation of the site, as well as its social and religious life. The
three main phases designate three historical periods labelled as
Roman, Byzantine, and Umayyad. Moreover, the long occu-
pancy of the site and the cultural and religious changes that
took place resulted in a complex and cumbersome stratigra-
phy, posing problems of absolute chronology regarding the
duration of the different occupations. TL dating was per-
formed on several domestic ceramics characteristic of the
three periods. Supported by the dating results (listed in
Table I), an absolute chronology of the site has been proposed.
For the Roman period, the archaeological evidence offers
some clues in view of a historical interpretation of the site
from the second century BCE to the first century CE. TL
dating of the retaining wall US2074 (samples D1618 (a–c)
in Table I) confirmed this hypothesis. The Jewish occupancy
had its break at the end of the first century CE, in the historic
centuries, the site may have been almost abandoned until the
third century CE, when repopulation of the site started and its
prosperity grew again; the remains of workshops for ceramics,
wine, and oil presses testify the economic prosperity of this
phase. Dating results of the shards from US 2079 (Table I,
samples D1622(a–c)) were very significant: these ceramics
date the stratum where an unidentified object (possibly a
weight or amulet) of good burnt ceramic holding an engraved
cryptogram was found. The discovery of this object was cru-
cial, as some of its engravings are ascribable to Jewish–
Christian inscriptions: it is, thus, the witness of religious con-
ceptions of the inhabitants of the site in the fourth century CE.
Successive development of the village occurred in the
Byzantine period, linked to new constructions such as a
church (church 47 in Table I) and a further oil press which
operated during the sixth century.
The final transformation of the village occurred, during the
seventh century CE, after large-scale destruction (likely due to
the invasion of the Persian army in 614 CE or to the local
Muslim victory over Byzantines in 643 CE). The destruction
was followed by a general recovery of life, marked by the re-
building of several houses and by new industrial and housing
projects, until the final abandonment of the village in the ninth
century.
The challenge of civilizations in the Far East
The Cham kingdom, one of the great civilizations of the
Indochinese peninsula, developed mainly between the fourth
and sixteenth centuries in present-day central-southern
Vietnam. The Cham, coming from India, maintained a strong
connection with the Hindu culture and religion, which is
 190 Page 12 of 15
particularly evident in their religious architecture. Their cul-
ture shows great affinity with the parallel civilizations of
Khmer in Cambodia and Thailand. Hundreds of remains of
Cham towers and brick buildings still characterize the pano-
rama of the coastal area of central Vietnam. The main site My
Son (the modern Vietnamese name means “beautiful moun-
tain”; DMS 15° 45′ 47″ N, 108° 07′ 27″ E; from the Google
Earth Application), which was proclaimed a World Heritage
Site by UNESCO in 1999, preserves the remains of a dozen
cult complexes, all of them in a severely altered or compro-
mised state of preservation.
Over the last 20 years, My Son has been the subject of an
important interdisciplinary project (Hardy et al. 2009), includ-
ing the archaeological excavation of the site (Fig. 7); the dat-
ing of its phases; architectural surveys of the buildings; and a
study of the materials and construction techniques, as well as
surveys on statics and degradation, restoration, conservation,
and use by the public (Martini et al. 2009).
A majority of the My Son towers were built in the tenth
century CE; many of them were damaged during the war and
are being preserved while awaiting decisions on future repair
work. In the area, 11 groups of tower temples (individuated
with the letters A–M) have been singled out. They are con-
structed of fired brick with stone pillars and decorated with
sandstone bas-reliefs depicting scenes from Hindu mythology.
The predominant style derives directly from India, but ele-
ments of Vietnamese art are also observed, namely, a few
boat-shaped roofs characteristic of Dong Son architecture
(Hardy et al. 2009).
The dating campaign focused on the remains in elevation
of the buildings of groups G and E, as well as excavations
Fig. 7 Emanuela Sibilia and
Marco Martini in the My Son Site
in central Quang Nam province,
Vietnam
Archaeol Anthropol Sci (2020) 12:190
carried out in their enclosures. Samples from over 250 ce-
ramics and bricks were taken, selected to cover the time ex-
tension of the complexes, whose chronology (performed on a
historical and documentary basis) is not completely agreed
upon by all experts in the field, leaving many open questions.
Group G, which was built during the first half of the twelfth
century, was selected from the various monuments due to its
unique characteristics. The group is located on an elevated
area unaffected by seasonal flooding and has never been re-
stored, except for some minor archaeological research in the
early 1990s. Group G, which had likely been originally con-
structed in one phase, presents an excellent model of a Cham
sacred area, with typical sacred Cham decorations.
The TL results for the foundation layer of the settlement G,
certainly dated to the twelfth century, were surprising. More
ancient material, dating back to the tenth and ninth centuries
(see samples labelled with red and green colours in Fig. 8)
were found, although there was no archaeological evidence of
masonry foundations in previous buildings. The archaeolo-
gists involved in the project thus hypothesised the existence
of an ancient wooden building with a roof made of bricks
(Hardy et al. 2009), the collapse of which may have been the
origin of the dated materials. The current G settlement, not
being the first of the area, was also suggested to be dated
between the seventh and tenth centuries, due to the age ob-
tained for numerous ceramics found in the excavation of the
original floor (see samples CO1–3 and CQ1–3 in Fig. 8).
Acknowledgements The passion of many researchers during the 40-year
activity of our laboratory made all this work possible. We would like
particularly to mention Laura Panzeri and Francesco Maspero, experts
in OSL and C14 dating techniques.
Archaeol Anthropol Sci (2020) 12:190 Page 13 of 15 190

Fig. 8 TL dating results from My

Son. Probability density plot of
the samples from settlement G

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