ARTICLE IN PRESS

Journal of Luminescence 130 (2010) 298–303

Contents lists available at ScienceDirect

Journal of Luminescence
journal homepage: www.elsevier.com/locate/jlumin

The correlation of fast OSL component with the TL peak at 325 3 C in quartz of
various origins
G. Kitis a,, N. Kiyak b, G.S. Polymeris b,c, N.C. Tsirliganis c
a
Aristotle University of Thessaloniki, Nuclear Physics Laboratory, 54124-Thessaloniki, Greece
b
Faculty of Science and Arts, Physics Department, ISIK University, 34980-Sile, Istanbul, Turkey
c
Archaeometry Laboratory, Cultural and Educational Technology Institute, R, C, ‘‘ATHENA’’, Tsimiski 58, 67100-Xanthi, Greece

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

Article history: The fast component of the optically stimulated luminescence (OSL) signal in quartz is the basic tool for
Received 2 December 2008 the optical dating. Its relation with the thermoluminescence (TL) glow-peak at about 325 3 C is well
Received in revised form established for naturally irradiated quartz. This relationship is also an important part of a general model
21 August 2009
for quartz on which many theoretical simulations of various OSL experimental results have been based.
Accepted 4 September 2009
In the present work this relationship is systematically investigated in nine quartz samples of different
Available online 12 September 2009
origin. The linearly modulated OSL (LM-OSL) curves of all quartz samples for stimulation time less than
PACS: 50 s consists of two components discriminated easily by a computerized curve deconvolution (CCD)
78.55.Hx analysis. By comparing the un-bleached to the respective bleached TL glow-curve, it is found that the
78.60.Kn
system of these two fast OSL components is directly related with only a small portion of the electron
traps responsible for the TL glow-peaks in the temperature region 2002400 3 C. By increasing the
Keywords:
stimulation times, besides the two fast components, the medium and the slow components are also
Thermoluminescence
Optically stimulated luminescence obtained. The medium and slow components are clearly related with the main body of the electron
Dating traps responsible for TL glow-peaks in the same temperature region 2002400 3 C. Despite their different
origin all quartz samples show an appreciable homogeneity concerning the number and time position of
the individual components, whereas, the relative TL/OSL intensities vary strongly from sample to
sample with the integrated TL intensity being generally much less than the integrated OSL intensity.
& 2009 Elsevier B.V. All rights reserved.

1. Introduction model [6] is extensively used to simulate various TL/OSL

The OSL signal of quartz usually used in practical dating
applications results either from a short stimulation of 0.1 s or by
integrating a few seconds from longer stimulation times [1]. This
optical dating signal termed fast OSL is considered to belong to an
OSL component appearing as a first one in any OSL experimental
curve, which, however, depending upon the stimulation time,
consists of many individual peaks [2–4]. This fast OSL component
in quartz can be used for dating applications when it originates
from a deep electron trapping kevel of very long half life. This
absolute requirement was shown unambiguously by Spooner [5],
for the case of natural TL signal of quartz. Spooner [5] found that
the optical dating signal is directly related with an electron trap,
which is responsible for the TL glow-peak at 325 3 C (depending
upon the heating rate).
The common electron trap of the fast OSL signal and of the TL
glow-peak at 325 3 C is a key element in the comprehensive
general model for quartz suggested by Bailey [6,7]. The Bailey
 Corresponding author. Tel./fax: +30 231099875.
E-mail address: gkitis@auth.gr (G. Kitis).
experimental results [8] as well as complete OSL dating protocols
[9].
The importance of the relation between the fast OSL signal and
the TL glow-peak at 325 3 C in both experimental and theoretical
research studies requires this relation to be universal as much as
possible. The aim of the present work is to investigate the
universality of this relation by extending the Spooner’s study [5]
performed on a naturally irradiated sample, to the artificial TL of
nine quartz samples of different origins.
2. Materials, apparatus and methods
2.1. Sample origin
The samples used here were all sedimentary quartz of different
origin. The samples with laboratory references of ALT, ATK, PDK
and SLE were from the coastal area of the Sea of Marmara and
Black Sea around Istanbul [10]. Sample INK (Inkumu, Bartin) is
also a coastal deposit collected from the central Black Sea coast.
PTR sample is proposed tsunami-laid deposits from the ancient

0022-2313/$ - see front matter & 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jlumin.2009.09.006
 ARTICLE IN PRESS
G. Kitis et al. / Journal of Luminescence 130 (2010) 298–303
city of Patara, located on Antalya’s Mediterranean coast in the
south of Turkey. The sample T-10 is from the Pleistocene Rehovot
Formation on the central coastal plain of Israel. The sample GZK
(Guzelkoy, Aydin) is fault deposit taken from Buyuk Menderes
Basin in the west part of Turkey and BTK (Bektemur, Amasya) is
fluvial terrace deposit from eastern Turkey.
2.2. Experimental protocol
The experimental protocol used in the present work consists of
two parts. It is based on the protocol used by Spooner [5] for
natural TL, modified appropriately in order to be applied to
artificial TL.
Part A: Used to obtain the unbleached TL.
Step 1: TL readout up to 500 3 C, at a heating rate of 1 K/s to
erase any natural signal.
Step 2: Test dose 100 Gy.
Step 3: TL up to 180 3 C with a heating rate 1 K/s to obtain the TL
glow-peak at 110 3 C for monitoring the sensitivity of the sample.
Step 4: TL up to 500 3 C with at heating rate 1 K/s to obtain the
un- bleached TL glow-curve.
Part B: Used to obtain the LM-OSL signal and the bleached TL.
Step 1: TL readout up to 500 3 C, at a heating rate of 1 K/s to
erase any natural signal.
Step 2: Test dose 100 Gy.
Step 3: TL up to 180 3 C at a heating rate of 1 K/s to obtain the TL
glow-peak at 110 3 C for monitoring the sensitivity of the sample.
Step 4: Blue LM-OSL at 125 3 C for 50 s, 0–100% LED power, to
receive the OSL signal.
Step 5: TL up to 500 3 C at heating rate 1 K/s, to obtain the
bleached TL glow-curve.
Step 6: Blue LM-OSL at 125 3 C for 50 s, 0–100% LED power to
obtain the OSL background signal.
The aim of the step 6 is, basically, to obtain the background
signal. However, the OSL of step 6 can additionally verify whether
or not some of the OSL components come from electron traps
beyond the temperature region of the TL glow-curves obtained in
step 6.
Spooner [5] had used naturally irradiated samples, so that the
TL signal was restricted in the temperature region of the 325 3 C
peak and beyond. In the present work the natural TL signal of the
samples is previously erased. The samples are then irradiated by a
laboratory beta dose and preheated up to 180 3 C prior to each LM-
OSL measurement. Therefore, in the case of Spooner’s protocol the
fast OSL signal has to be related with a TL signal around the 325 3 C,
whereas in the present work a substantial part of the TL glow-
curve below 325 3 C is included.
The stimulation time of 50 s for LM-OSL at 125 3 C in step 4 was
selected after many tests in order to receive a fast component with
a negligible contribution from the medium and slow components.
2.3. Equipment
The sample preparation was described in some detail recently
by Kiyak et al. [4]. All measurements were performed using the
automated Risø TL/OSL reader (model TL/OSL-DA-15), using an
internal 90Sr/90Y beta ray source of dose rate 0.1 Gy/s. Blue light
emitting diodes (LEDs) (470 nm, FWHM 40 nm, 40 mW=cm2 ) were
used for stimulation and the OSL signal was detected through U-
340 filters.
2.4. Method of analysis
The LM-OSL curves were de-convoluted using a first order
kinetics expression proposed by Bulur [11], which was modified
299
into an expression containing only the peak maximum intensity
Im and the corresponding time tm [12]. These two variables can be
extracted directly from the experimental OSL curves. The modified
expression used in our computerized procedure is
 
t t2
IðtÞ ¼ 1:6487  Im   exp  2 ð1Þ
tm 2tm
The background signal was simulated by an equation of the
form
GLM ðtÞ ¼ a þc  t ð2Þ
where a is the average in the first few seconds of a zero dose LM-
OSL measurement and c is a constant.
All curve fittings were performed using the MINUIT computer
program [13] while the goodness of fit was tested using the figure
of merit (FOM) of Balian and Eddy [14] given by
X jYExper  YFit j
FOM ¼ ð3Þ
A
i
where YExper is the experimental LM-OSL, YFit is the fitted LM-OSL
curve and A is the area of the fitted curve.
3. Experimental results
Fig. 1 shows the unbleached TL glow-curves (a), the bleached
ones due to the blue light stimulation at 125 3 C for 50 s (b) and
finally their difference (c). A first observation is that the
effectiveness of blue light to bleach the electron traps varies
strongly for the different quartz samples. The difference given by
the curve (c) in all figures is a measure of the electrons evicted by
the 50 s blue light stimulation from the electron traps responsible
for the respective TL glow-peaks. It seems that the blue bleaching
is continuous across the whole glow-curve and does not influence
a certain part of the glow-curve only. However, in some cases as
those of SLE, INK and BTK quartz samples the bleaching of TL is
predominant in the glow-curve region at the position of the
‘‘325 3 C’’ glow-peak.
A characteristic example of the LM-OSL curve shapes received
at 125 3 C and analyzed into its individual first order kinetics
components is shown in Fig. 2 for the case of SLE quartz. The LM-
OSL curve shapes of all other quartz samples are more or less the
same. A slight differentiation exists only in the contribution of the
component C3 . The curve (a) in Fig. 2 is an exponential curve
inserted in the curve fitting procedure to correct for the
phosphorescence decay at 125 3 C. It must be noticed that the
fitting is not possible without considering the phosphorescence
correction, whose contribution to the total signal ranges from 2%
to 6% of the total signal.
A basic observation is that the LM-OSL signal for a stimulation
time of 50 s is a composite signal consisting of the three
components with time maximum values shown in Table 1. Since
the third component C3 is not completed for the stimulation time
of 50 s, a new series of measurements were performed where the
experimental protocols were applied for an LM-OSL stimulation
time of 200 s instead of 50 s. All the new LM-OSL curves obtained
were de-convoluted and the new time peak maxima were found.
According to the first order kinetic theory the time maximum of
individual LM-OSL peaks for a stimulation time of 50 s must be
half of the respective time maximum for the stimulation time of
200 s. This was found to hold exactly for the components C1 and
C2 , so the values of the component C3 in Table 1 are those
resulting from the time maximum values of the stimulation time
of 200 s by dividing them over 2.
A critical point here is to define the term ‘‘fast component’’. A
definition given by Bailey [7] is based on the cross-section values.
According to a comprehensive quartz model suggested by Bailey
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300 G. Kitis et al. / Journal of Luminescence 130 (2010) 298–303

2000 ALT ATK 2000 PDK

1500 a
a
1500 a 1500
TL (a.u.)

TL (a.u.)
TL (a.u.)
1000 b
1000 b b 1000

c 500 c
500 c 500

0 0 0

0 100 200 300 400 0 100 200 300 400 0 100 200 300 400
Temperature (°C) Temperature (°C) Temperature (°C)

SLE 1200 a INK 2000 PTR

3000
a
1500
TL (a.u.)

TL (a.u.)
800 b
TL (a.u.)

2000 a
1000 b
b
1000 400 c c
500
c
0 0 0

0 100 200 300 400 0 100 200 300 400 0 100 200 300 400
Temperature (°C) Temperature (°C) Temperature (°C)

T10 GZK 1000 BTK

3000 400
a 800
a

TL (a.u.)
TL (a.u.)

300
TL (a.u.)

2000 b 600 a
b 200 400 b
1000 c
c 100 200 c
0 0 0

0 100 200 300 400 0 100 200 300 400 0 100 200 300 400
Temperature (°C) Temperature (°C) Temperature (°C)

Fig. 1. Glow-curves of all kind of quartz: (a) un-bleached glow-curve; (b) bleached glow-curve and (c) the difference between (a) and (b).

Table 1
SLE The time maximum positions of the fast LM-OSL components as obtained from the
computerized de-convolution analysis.
40000
Quartz tm1 tm2 tm3
LM-OSL (a.u.)

30000 C2 ALT 7.20 12.85 35.70

ATK 7.03 11.71 51.45
PDK 6.82 11.02 30.62
20000 SLE 5.25 8.64 28.91
INK 6.26 9.82 32.49
C1
PTR 7.13 12.57 27.95
T10 6.79 10.64 32.50
10000
GZK 6.22 11.70 37.50
a C3 BTK 5.40 11.24 50.60

0 10 20
Stimulation time (sec)
Fig. 2. LM-OSL curve of SLE quartz analyzed into its individual components using
first order kinetics.
[7], the optical bleaching cross section for the 110 3 C TL trap at
20 3 C was estimated to be s1103 C TL ¼ 1019 cm2 . Therefore, the LM-
OSL component, which is correlated with the 110 3 C TL glow-peak,
30 40 will yield optical bleaching cross section values of the same order.
Hence the fast OSL components will yield optical bleaching cross-
section values much larger than that of the 110 3 C TL glow-peak.
Alternatively, based on the above arguments the fast OSL
component is considered as that part of the LM-OSL curve
received at room temperature which is obtained in shorter times
than the LM-OSL component originating from the electron trap
corresponding to the TL glow-peak at ‘‘110 3 C’’ . The peak
maximum time, tm of this LM-OSL component cannot be
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G. Kitis et al. / Journal of Luminescence 130 (2010) 298–303 301

evaluated after room temperature LM-OSL measurements for 50 s
stimulation. However, Kiyak et al. [15] had found that the LM-OSL
component originating from the TL glow-peak at ‘‘110 3 C’’ had tm
values somewhat higher than the tm values of the component C3
listed in Table 1.
Since, for given stimulation conditions the cross-section
2
depends on 1=tm it is obvious from the values of Table 1 that
the possible cross-sections of the components C1 and C2 will be
within the same order of magnitude. The cross-section of the
component C3 will be an order of magnitude lower, but higher
than the cross-section of the LM-OSL component due to the
‘‘110 3 C’’ TL trap.
According to the definitions and the discussion above the
components C1 and C2 are undoubtedly fast components, whereas
the component C3 can be, more or less, considered as fast
component too.
Another important result is that the levels (electron traps or
recombination centers) responsible for these components have
been entirely emptied. The reason is that the LM-OSL peaks are
completed during stimulation. However, as it is seen in Fig. 1, the
emptied electron traps correspond to a small part of the total
electron traps available. Since, the main body of the electron traps
is unbleached the question is whether in a successive stimulation
the fast components can be obtained again. This question was
investigated by two series of separate measurements. The first
series of measurements involved successive LM-OSL measure-
ments at 125 3 C. The results are shown in Fig. 3 for SLE quartz. As
is seen once the fast components are received during the first LM-
OSL measurement they do not appeared during the second up to
the fourth LM-OSL measurements. The results are exactly similar
for all other quartz samples.
In the second series of measurements the third step in part B of
the protocol was changed as step 3: Blue LM-OSL at 25 3 C for 50 s,
0–100% LED power followed by a TL up to 180 3 C at a heating rate
of 1 K/s to erase the TL glow-peak at 110 3 C. It was found that once
the fast components were expired during the room temperature
stimulation for 50 s, then the subsequent LM-OSL measurement at
125 3 C does not contain the fast components. The situation is
exactly similar to that described in Fig. 3.
Finally, the experimental protocol was repeated for LM-OSL
stimulation times of 200 and 2000 s. The results show that the
blue light stimulation continues to bleach the electron levels
responsible for the high temperature TL glow-peaks after the fast
components are obtained, giving rise to the appearance of
medium and slow components.
SLE
40000
LM-OSL (a.u.)
The conclusion from the above results is that only a small part
of the electron traps responsible for the TL glow-peaks above
150 3 C, contribute to the fast OSL components, whereas the main
body of these electron traps continues to bleach, giving rise to the
appearance of medium and slow components.
The difference between unbleached and bleached TL shown in
the glow-curves of Fig. 1 corresponds to electrons evicted by the
optical stimulation giving rise to the LM-OSL signal. Therefore,
theoretically, the TL lost and the LM-OSL signal must be equal. The
analysis results concerning peak integrals are given in Table 2. The
second column of Table 2 gives the ratio of the TL lost due to the
50 s optical stimulation (difference between unbleached and
bleached TL) relative to the unbleached TL. This fast TL lost vary
from 12% to 20% of the unbleached TL with the exception of PTR
quartz. This represents the percentage contribution of the deep
electron traps to the fast OSL components.
A comparison between the TL bleached over the total LM-OSL
signal is given in the third column of Table 2. As is seen in the case
of seven out of the nine quartz samples, the TL bleached is less
than 20% of the total LM-OSL. In the case of ALT quartz the TL
bleached is higher than the total LM-OSL as also in the case of GZK
quartz for which, however, the statistics is very low. Therefore,
instead of being equal, the LM-OSL obtained is much higher than
the bleached TL. These results can be understood in the frame-
work of the thermal quenching [5,16,17] existing in quartz. The
thermal quenching efficiency is strongly temperature dependent,
so it will be very high as the glow-curve temperature increases.
The total LM-OSL signal is much higher than the bleached TL due
to the fact that the LM-OSL is measured at the stable temperature
of 125 3 C under the same value of the thermal quenching
efficiency, whereas the TL glow-curve above 150 3 C is measured
with thermal quenching efficiency much lower and moreover
increasing as a function of temperature. Therefore the ratio values
of third column in Table 2 could approach the values of thermal
quenching efficiency. The case of ALT quartz, is an exception,
which cannot be explained. However, it must be noticed that this
quartz sample is the only sample for which the main body of the
bleached TL corresponds clearly in the region of the TL glow-peaks
below 200 3 C, where the thermal quenching efficiencies have the
lower values relative to the rest glow-curve.
Finally the fourth and fifth columns of Table 2 show the
percentage of the sum of the components C1 , C2 and of the sum of
C1 , C2 , and C3 divided by the total LM-OSL signal from which
the phosphorescence and background signals were subtracted.
The results clearly show that the LM-OSL signal obtained under
the experimental protocols of the present work consists almost
entirely of fast components.
A specific relation between the three fast components with the
electron traps responsible for the TL glow-peaks above 150 3 C
cannot be obtained with the data available. Therefore, further
work is required in order to correlate each one of the fast LM-OSL
components C1 2C3 with a specific TL glow-peak at 150 3 C and

30000 a above. This correlation could probably be obstructed by the

20000 Table 2

Quartz (U-B)/B TL/OSL C12 =OSL C123 =OSL

10000
ALT 0.296 1.355 0.467 0.998
b c ATK 0.170 0.239 0.527 0.995
d PDK 0.245 0.232 0.732 0.983
0 bg SLE 0.148 0.124 0.639 0.999
INK 0.129 0.150 0.834 0.941
0 10 20 30 40 50 PTR 0.486 0.174 0.722 0.980
T10 0.171 0.197 0.786 0.968
Stimulation time (sec) GZK 0.154 1.184 0.500 0.533
BTK 0.127 0.170 0.549 0.996
Fig. 3. Successive LM-OSL curves received at 125 3 C for 50 s of SLE quartz.
 ARTICLE IN PRESS
302 G. Kitis et al. / Journal of Luminescence 130 (2010) 298–303
malign thermal quenching effect. Nevertheless, if accomplished,
this correlation will have major implications on the dating
protocols applied for OSL dating, such as the well established
SAR protocol [18]. While applying the latter, the preheat
temperature of all test-dose-measurements is different from that
of the regeneration-cycle measurements. In other words, the fast
OSL signal measured after the test dose administration could not
originate from the same electron traps to the respective natural
signal, or even the regenerated one. On the other hand, a preheat
plateau test for the OSL ages could possibly overcome this
problem.
As it was said above further work is required in order to
correlate each one of the fast LM-OSL components C1 2C3 with a
specific TL glow-peak at 150 3 C and above. On the other hand, even
with the present results a very basic question is drawn, which
needs some discussion. What is the difference between the ‘‘first’’
10–20% of the traps and the rest of them?
Before the discussion and a possible answer first of all it is
useful to remind here that TL and OSL are two very different
effects concerning both stimulation and recombination stages.
Their correlation exists since in both effects the same trapping and
recombination levels are involved. During thermal stimulation the
trapping levels are totaly emptied in series according to the E; s
pairs and then recombine in the same series according to the
recombination probabilities of each recombination center. On the
other hand during optical stimulation the trapping levels are
excited simultaneously according to their photo-ionization cross-
section and then recombine simultaneously according to the
recombination probabilities of each recombination center.
Based on the above difference between TL and OSL two
directions are opened for a discussion. The first direction is that
the difference between the ‘‘first’’ 10–20% of the traps and the rest
of them, comes from processes taking place during recombination
stage whereas the second direction from processes taking place
during stimulation stage.
By considering the first direction one must know the number
of recombination centers in quartz. In the extensive review by
Krbetschek et al. [19] (and references therein) it is shown that in
general the emission spectrum of quartz consists of two intense
and two weak emission bands, which are more or less observed
for the most kinds of quartz. Since two of the emission bands
could originate from different excited states of the same
recombination center it is concluded that the possible number
of recombination centers could be 4 or less. A simple model to
explain the difference between the ‘‘first’’ 10–20% of the traps and
the rest of them requires that the recombination probability in
one of the recombination centers be much higher than that of the
others. So, when during optical stimulation electrons are ejected
simultaneously, according to their photo-ionization cross-section,
from all trapping levels above 1503 C, then all of them recombine
with higher probability to this specific recombination center.
According to the present results a percentage of 10–20% of the
optically liberated electrons annihilates all these recombination
centers giving rise to the fast OSL component. All the other
electrons from the tapping levels above 150 3 C recombine to other
recombination centers giving rise to medium and slow OSL
components. It must be noticed, however, that according to this
model some difference in the emission spectrum of the fast
components and the medium and slow ones are expected.
By considering the second direction one has to know the
bleaching properties of quartz. In general the optical bleaching of
a single electron trapping level through a first order process has to
follow a simple exponential law [20,21]. An example is the case of
the ‘‘110 3 C’’ glow-peak of a milky quartz [22]. However, there are
many experimental results where the bleaching of TL as a function
of time in quartz does not follow the single exponential law. In
fact besides the exponential component expected, which is a fast
one, an additional component is also present which corresponds
to a slower bleaching rate and it was termed ‘‘hard to bleach
component’’ [23–25]. This is also the case in most TL dating
procedures of sedimentary deposits, where the sun does not
bleach entirely the TL trap under study, but instead leaves a
residual level of the TL signal. The very interesting experimental
result of the bleaching of a single trapping level through two
bleaching decay rates was modelled by Chen et al. [26] and
McKeever [27] (see also the reviews [20,21]). Therefore, from an
experimental point of view, the bleaching of some single trapping
levels are found to follow the exponential decay law expected in
some TL glow-peaks, whereas the bleaching of some other TL
glow-peaks takes place through two (or more) bleaching rates.
The latter case can be used to explain the difference between the
‘‘first’’ 10–20% of the traps and the rest of them. Indeed the ‘‘first’’
10–20% of the traps correspond to the fast bleaching rates
whereas the rest of them to the ‘‘hard to bleach components’’.
4. Conclusions
Based on the experimental results presented above the
following conclusions are drawn:
(1) There is no specific relation of the fast components with a
specific electron trap responsible for a specific TL glow-peak.
(2) The fast components must be related with all electron traps
responsible for TL glow-peaks in the temperature region
between 150 and 400 3 C.
(3) In most cases the stimulation time needed to obtain the fast
components bleaches only 10–20% of the total TL signal. So,
only those electrons released first from that part of the
electrons traps contributes to the fast components.
(4) Once the fast components are obtained and the optical
stimulation continues, the TL signal continues to bleach
giving rise to the medium and slow LM-OSL components.
(5) The LM-OSL signal resulting from the 50 s stimulation
corresponds entirely to the fast components. On the other
hand the total light sum of the fast components is much
higher than the total TL bleached during the 50 s stimulation,
probably due to the thermal quenching effect.
(6) Spooner’s protocol applied in the present work is found to be
very simple and effective for finding the system of traps
responsible for the fast components of any quartz sample. Its
results can act as a guide in verifying that the fast component
during artificial irradiations, as well as, during natural
irradiation comes from the same exactly electron trap.
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