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Advance Access publication 15 July 2011

doi:10.1093/rpd/ncr315

1

Archaeometry Laboratory, Cultural and Educational Technology Institute (C.E.T.I.), R.C. ATHENA,

Tsimiski 58, 67100 Xanthi, Greece

2

Nuclear Physics Laboratory, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece

*Corresponding author: dafouxen@ipet.gr

Received March 3 2011, revised May 12 2011, accepted June 17 2011

This paper exploits the possibility of using commercial software for thermoluminescence and optically stimulated luminescence

curve deconvolution analysis. The widely used software package Microsoft Excel, with the Solver utility has been used to

perform deconvolution analysis to both experimental and reference glow curves resulted from the GLOw Curve ANalysis

INtercomparison project. The simple interface of this programme combined with the powerful Solver utility, allows the analysis of complex stimulated luminescence curves into their components and the evaluation of the associated luminescence

parameters.

INTRODUCTION

The computerised curve deconvolution (CCD) analysis of thermoluminescence (TL) glow curves and

optically stimulated luminescence (OSL) decay

curves into their individual glow peaks and

components respectively have been recognised over

the last 30 y to be of major importance(1 5). The

information by the CCD concerning the trap energy

depth (E), frequency factor (s), kinetic order (b),

photoionisation cross section (s), etc, is very useful

in order to understand the luminescence mechanism

of materials.

The capabilities of several computer codes used by

the various research groups for CCD and their

assessment of the glow curve parameters were tested

by the GLOw Curve ANalysis INtercomparison

(GLOCANIN) project. Participants in the GLOC

ANIN project were asked to analyse the so-called

reference glow curves using their computer codes.

The results on synthetic as well as on experimentally

measured glow curves can be found in references(6, 7).

The application of the CCD consists essentially of

two steps: (i) deciding on the mathematical model that

describes a single TL/OSL peak and (ii) assessing the

values of the curve parameters that minimise the sum

of squares of the differences between the fitted model

and the experimental curve(8). Concerning the first

step, there is a number of well-established analytical

expressions in the literature describing single TL/OSL

peaks(6, 9, 10). Although a great amount of work exists

on deriving analytical single peak expressions and

despite the significant information that the CCD

analysis yield, the latter is not widely adopted by the

TL/OSL community as a basic tool, while the

any CCD analysis of relevant data. In authors

opinion, this could be partly attributed to the lack of

available commercial software; so every researcher has

to write his/her own program.

The aim of the present work is to offer a solution

to the aforementioned problem that will enable any

researcher to analyse easily and accurately even the

most complex TL/OSL curves consisting of many

overlapping individual peaks, employing the commonly used spreadsheet software package Microsoft

Excel, along with its Solver, add-in utility.

SINGLE TL/OSL PEAK ANALYTICAL

EXPRESSIONS

The analytical expressions used in the present work

are the well-known expressions for general and

mixed order kinetics, named GOK and MOK,

respectively hereafter(7, 11 14). The selection of these

expressions was based on the following:

(1) The GOK expression, although empirical is

almost exclusively used in the literature(7).

(2) The MOK expression, although rarely used in

the literature, is physically meaningful(11).

(3) The GOK expression for b 2 coincides with

second-order kinetics, whereas for b ! 1 coincides

with first-order kinetics.

(4) Similarly, the MOK expression for a ! 1

coincides with second-order kinetics and for a 0

coincides with first-order kinetics.

The advantage of those expressions is that

only one expression accounts for both first- and

second-order kinetics, and furthermore it can

# The Author 2011. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com

Downloaded from http://rpd.oxfordjournals.org/ at National Hellenic Research Foundation & National Documentation Centre on October 22, 2012

CURVES USING A POPULAR SPREADSHEET PROGRAM

D. AFOUXENIDIS ET AL.

advantage of the I (Im, Tm, E, b or a, T ) representation is not easily seen in the cases of experimental

curves with one single peak. However, it becomes

clear in cases of experimental curves consisting of

many overlapped peaks.

It must be noted that the proposed expressions

involving Im, Tm result as transformations of the

original expression involving n0 and s. The only

approximation in these expressions is the usual

approximation of the exponential integral appearing

in TL theory. The analytical TL expressions are

derived using two terms of the asymptotic series

approximation (ASA) of the exponential integral.

The transformed equations can include more terms

of the ASA through the term Dm, (see later text),

which should be simply replaced by the ASA

expressions above the third term. Details about the

ASA approximation can be found in reference(15)

SPREADSHEET PREPARATION

The steps needed to perform a CCD analysis with

an Excel spreadsheet are shown in Table 1. The

example used is that of a complex TL glow curve

consisting of two individual peaks using the GOK

expression.

In the first step, one ascribes the temperature and

TL intensity of the experimental glow curve to the

columns A and B. In the second step, the subsequent

columns C and D are ascribed to each one of the

individual peaks 1 and 2, respectively.

A

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

19

20

21

a

S I(T)fit

0.0003

0.0004

0.0005

jI(T)exp I(T)fitj

3.6E206

4.2E206

4.5E206

1

Imax

Tmax (K)

E (eV)

b

M.F.

Temp

301.01

302.02

303.02

Peak #1

0.04

417

1.3

1.0001

1000a

Integral

11 098

Freq factor (s 1)

7E15

FOM (%)

1.2

I(T)exp

0.0003

0.0004

0.0005

Peak 1

0.0003

0.0004

0.0005

Peak #2

0.05

456

1.5

1.0001

1000a

16 904

2.9E15

Peak 2

4.8E206

5.9E206

7.1E206

364

Downloaded from http://rpd.oxfordjournals.org/ at National Hellenic Research Foundation & National Documentation Centre on October 22, 2012

Concerning the decision between GOK and MOK,

one has to know that their greater difference, as it

was shown by Kitis et al.(12), is observed at about

b1.6 and this difference is ,4 %. Moreover their

difference is mainly at the high temperature range of

the TL glow-peak. Taking into account that these

differences were obtained using numerically generated peaks, one can conclude that these differences

are rather difficult to be seen in an experimental TL

peak. Therefore, in most practical experimental

cases yielding an error higher than 1 %, there is no

real dilemma in choosing between GOK and MOK,

since they will both produce similar results.

Another feature of the selected analytical

expressions is that they are of the form of I (Im, Tm,

E, b or a, T )(7, 11) and I (Im, tm, b or a, t)(13, 14), for

TL and linearly modulated (LM)-OSL, respectively,

instead of the form I (n0, s, E, b or a, T ) and I (n0,

l, b or a, t) of the original equations(9, 10), where

variable T is the temperature, Tm is the temperature

at maximum TL intensity, Im is the maximum intensity, n0 is the initial concentration of trapped electrons, tm is the time at maximum LM-OSL intensity

and l is the LM-OSL stimulation wavelength. The

advantage of the proposed presentation is that the

quantities Im, Tm and tm can be evaluated directly

and accurately from the experimental TL/LM-OSL

curves, whereas it is not possible to have any knowledge about the probable values of n0, s and E

appearing in the original form of the equations. The

b=b1

IT Im b

E T Tm

exp

kT

Tm

T2

b 1 1 D 2

Tm

b=b1

E T Tm

Zm

exp

kT

Tm

where

D

2kT

2kTm

; Dm

; Zm 1 b 1 Dm

E

E

be used to reproduce the first (lower Tmax) peak in

column C by dragging it to the entire column

C. Therefore a peak for the entire temperature

region is calculated, according to the temperature

T(K ) and its four trapping parameters that were preselected. This procedure is repeated for the next

glow peak in column D, by copying and pasting the

same expressions to cell D19 and dragging it to the

entire corresponding column.

In that way, two arbitrary glow peaks are

created without any other limitation. However, the

sum of these peaks should be similar to the total

experimental curve. This similarity is usually

checked by the linear regression coefficient (x 2),

which however does not provide an immediate

clue regarding the goodness of fit. In order to circumvent this problem, another mathematical index

was selected, which is termed the FOM(16) and is

defined as

P

p TLexp TLfit

P

FOM% 100

p TLfit

goodness of fit; the lowest its value, the best fit.

Therefore, every fitting attempt should result in

minimising the FOM index value, which is

achieved by changing the set of the parameter

values of each glow peak. This is achieved by

using certain optimisation software packages, the

Solver, the power full add in of Excel. A full

description for the latter is presented in the following section.

Returning to spreadsheet preparation procedure,

two more columns are required, for instance E and

F, in order for the sum of the fitted (calculated) glow

peaks and the absolute value of the difference

between each experimental and calculated data

point to be respectively presented. The main objective is to minimise the values in column F. Finally,

showing the FOM index value among the initial

cells of the spreadsheet is suggested.

The spreadsheet of Table 1 described earlier

stands as an example for the deconvolution of the

glow curve into its two overlapping glow peaks, in

order for the parameters associated with the individual peaks to be estimated. Only the first 21

rows are shown for the sake of brevity. Columns

(A19:A21) and (B19:B21) contain the experimental

data points for the TL glow curve, while columns

(C19:C21) and (D19:D21) contain the fitted data

points using the GOK model. Row nine holds the

value of a multiplier factor that is necessary for

further analysis and represents the order of peak

height intensity.

The heating rate used throughout the measurement is given in Cell B2 since it is a common parameter for all the glow peaks. Furthermore, the TL

integral of each glow peak (sum of the data in

column below row 19) is given in row 11 of the corresponding column, while in row 13, the corresponding frequency factors are shown. The frequency

factor values are calculated from the respective

equation(7) using the values of E, Tm and b obtained

from the curve fitting and using the heating rate

given in Cell B2.

ABOUT SOLVER

The Solver(17, 18) is an Excel Add-in, a software

program that could be found in the Tools menu; it

can be installed by checking the Solver Add-in following the path: Tools !Add-Ins. Solver is a

general-purpose optimisation package that is used in

order to find a maximum, minimum or specified

value of the target Cell. The Solver code is a

product of Frontline Systems Inc. The Solver can be

used to minimise the sum of squares of residuals

(differences between yobsd and ycalc) and thus

perform a least- square fitting. It can be used to

365

Downloaded from http://rpd.oxfordjournals.org/ at National Hellenic Research Foundation & National Documentation Centre on October 22, 2012

arbitrary but meaningful values for the parameters

Im, Tm, E and b for each single glow-peak. As can

be seen in Table 1, these values are inserted in the

rows 5 8 respectively in column C for the first peak

and column D for the second peak.

When the curve fitting procedure is completed, it

gives the net values of Im, Tm, E and b. However,

the evaluation of additional quantities such as the

integral of each glow-peak, the frequency factor and

figure-of merit (FOM) values (see later text) is also

feasible.

In the next step, the raw experimental data are

inserted in the same spreadsheet in a way that the

first data point appears in the 19th row of columns

A and B, corresponding to the temperature and

signal respectively.

Following that, the GOK analytical expression(7)

D. AFOUXENIDIS ET AL.

box) be minimised.

DISCUSSION

TL case

The synthetic glow curve REFGLOW.002 as well as

the measured glow curve REFGLOW.009 of the

GLOCANIN project (19) are used next as examples

in order to estimate their parameters, using the

earlier-mentioned procedure in Excel.

The synthetic glow curve REFGLOW.002 is the

sum of four glow peaks obtained by solving directly

the differential equation with trapping parameters

such as the glow curve structure of TLD-100, which

describes the charge transport in the TL material

according to the well-known Randall-Wilkins model

with the Bulirsch-Stoer method. This glow curve is

included in order to evaluate the accuracy in the

determination of parameters in the case of overlapping peaks.

Figure 2 shows the reference glow curve

REFGLOW.002 in open cycles together with the calculated curve as a solid line passing through them,

using the GOK model.

Table 2 gives the calculated parameters for the

peaks 2, 3, 4 and 5 for the GLOCANIN curve

REFGLOW.002 as found by applying the solver Addin on the functions for both GOK and MOK(7, 11),

using the Microsoft Excel spreadsheet.

As can be seen from the low FOM values (0.0090

and 0.0093 % for the GOK model and the MOK

model, respectively), the glow curve deconvolution

spreadsheet and the Solver Add-in under GOK model. In

the lower graph residual TL intensity versus temperature,

after curve fitting is presented.

366

fitting.

The Solver uses the Generalised Reduced

Gradient non-linear optimisation code. For each of

the changing cells, the Solver evaluates the partial

derivative of the objective function (the target cell)

with respect to the changing cell ai, by means of the

finite-difference method.

The Solver uses a matrix including the partial

derivatives to determine the gradient of the response

surface and thus decides how to change the values

of the changing cells in order to approach the

desired solution.

The Solver Parameter dialog box is presented in

Figure 1. In the Set Target Cell box the cell

containing the quantity that is going to be minimised, here the FOM (%), must be typed. Because

of the minimisation process, the Min button must

be checked. In the By Changing Cells box, the

Cells that contain the fitting parameter values

must be typedhere the values of Imax, Tmax, E

and b.

With Solver, some physically imposed constrains

can be applied to the solution. For example, in the

case of GOK, the value of the kinetic parameter b is

limited by the inequality 1,b 2 and in the case of

MOK, the value of the kinetic parameter a is

limited by the inequality 0 a , 1. So this constrains must be used for the above cases.

Since the Solver operates by a search routine, a

solution would be found most rapidly and efficiently

if the initial estimates that have been provided are

close to the final values. A chart of the data that displays both yobsd and ycalc is often useful to be

created, and then a good set of initial parameters

can be estimated by varying the parameters

manually.

It must be noticed that the initial values of the

fitting parameters and the optimised parameter

values are placed in the same cell because the Solver

requires that the user should define the cells that

have to be modified (by changing cells, on the Solver

parameter dialog box) so that the quantity selected

Table 2. Estimated TL parameters for both GOK and

MOK using Microsoft Excel Add-in, Solver for

REFGLOW.002 as well as the references values as reported

in the CLOCANIN project.

Peak 2

Peak 3

Peak 4

456.5

484

Tmax (K) 417.1

E (eV)

1.383

1.483

1.584

b

1.0006

1.0009

1.0009

TL

11 100

16 914

27 382

3.9E16

1.6E16 2.1E16

s (s21)

Mixed-order kinetic (FOM (%)0.009339)

413.6

451.6

478.0

tmax (K)

E (eV)

1.383

1.483

1.583

a

7.2E205

0

0

TL

11 098

16 896

27 397

1

5.6E16

2.5E16 3.3E16

s (s )

(19)

CLOCANIN

tmax (K)

417.3

456.8

484

E (eV)

1.383

1.483

1.583

1

3.9 E16 1.6E16 2E16

s (s )

TL

111 001

16 898

27 401

Peak 5

511.6

2.0038

1.0006

47 302

4E19

503.7

2.0038

0

47309

8.5E19

511.9

2.0038

4E19

47 302

according to the Randall-Wilkins model from the given

heating rate, E and s values.

values of peak temperature (Tmax), activation energy

(E) and Integral, for each individual glow curve presented, as well as the same order of magnitude of

frequency factor (s), indicate the agreement between

the used models. These values are in great agreement

with those reported in the GLOCANIN project (19),

indicating the computational power of Solver utility.

The value of the calculated parameter (b) that

stands for kinetic order according to the GOK has

been calculated as b1.00065 for peak 2, very close

to unity (b1) that stands for the first-order kinetics

model that has been used in order to obtain the

REFGLOW.002, according to the Randall-Wilkins

model. On the other hand, the value of the calculated parameter (a) that stands for kinetic order

according to the MOK has been calculated as

a 7.261025. For this value (a0), the MOK

model is equivalent with the first-order kinetic

model as has been described by Kitis et al.(12).

Reference glow curve REFGLOW.009 stems for a

highly irradiated (D600 Gy) TLD 700 sample.

Apart from the well-known glow peaks 2 5, it features a complex group of high temperature peaks.

These overlapping peaks make the fitting procedure

much more complicated.

Figure 3. Curve fitting of REFGLOW.009 using

excel spreadsheet and the Solver Add-in under

General-Order Kinetics model. In the lower graph

in open cycles together with the calculated curve as a solid

line passing through them, using the GOK model.

fitting is presented.

Table 3 gives the calculated parameters for the

peaks 1, 2, 3, 4, 5, 5a, 6, 7, 8, 9, 10 and 11 of the

GLOCANIN curve REFGLOW.009 as they were

estimated by applying the Solver add-in utility on

the function of the GOK(7), in the Microsoft Excel

spreadsheet. These values are in great agreement

with those reported in the GLOCANIN project (19),

indicating the computational power of Solver utility.

OSL case

As opposed to the case of TL, there is no project

such as the GLOCANIN for OSL. So, there are not

any reference LM-OSL curves with their corresponding parameters in order to evaluate the capabilities

of computer codes for fitting in LM-OSL cases.

Due to the lack of any reference LM-OSL curves,

simulation was necessary in order to obtain data for

reliable curve fitting. The latter was performed using

the equation(10)

sg b=1b

I tOSL n0 sgt 1 b 1 t2

2

where n0 is the initial concentration of electrons in

traps, s the photoionisation cross section, g the

stimulation increase rate and b the kinetic order parameter. To obtain numerical values for I(t) OSL, the

values for n0 100 000, s.g0.0001 and

b1.00000001 were used. The resulting data were

used to perform a curve fitting using the equations

for GOK and MOK of LM-OSL. Figure 4 shows

the simulated LM-OSL curve as open cycles and the

calculated curve as a solid line passing through them

under the GOK model.

367

TL parameters

D. AFOUXENIDIS ET AL.

Table 3. Estimated TL parameters for General-Order Kinetics using Microsoft Excel Add-in, Solver for REFGLOW.009 as

well as the reference values as reported in the CLOCANIN project.

Peak 1

Peak 2

Peak 3

Peak 4

Peak 5a

Peak 6

Peak 7

E (eV) 0.95

1.23

1.30

1.56

2.08

s (s 1) 11013 11015 21014 11016 51020

1.77

91016

1.46

1.37

1.86

1.97

11013 91011 71015 11016

1.75

31013

1.41

11010

GLOCANIN(19)

E (eV)

1.25

1.3

1.6

2.02

11015 21014 81016 81019

s (s 1)

Peak 8

Peak 9

Peak 10 Peak 11

using Microsoft Excel Add-in, Solver for Al2O3:C LM-OSL

curve structure.

Al2O3:C

Microsoft Excel spreadsheet and the Solver Add-in

according GOK model. In the lower graph values for

residual LM-OSL intensity versus stimulation time, after

curve fitting are presented.

Peak 1

Peak 2

93.552

415.368

tmax (s)

a

0.950

0.909

Integral

1 932 742

4 516 100

Peak 3

1316.279

0.914

3 318 872

tmax (s)

93.471

415.367

b

2.000

2.000

Integral

1 967 657

4 554 843

1316.277

1.916

3 245 255

Deviations (%)

tmax (s)

0.086

Integral

21.806

0.000

2.218

0.000

20.858

and MOK using Microsoft Excel Add-in, Solver for

simulated LM-OSL curve.

LM-OSL parameters

GOK

tmax (s)

b

Integral

FOM (%)

100.000013

1.000000001

99998.75394

0.00004929

MOK

99.99991708

0.000002696

99998.80336

0.000054287

Table 4 gives the peak parameters for the simulated curve as found by applying the Solver add-in

utility on the function of the GOK(13) and on the

function of the MOK(14), using Microsoft Excel

spreadsheet.

As can be seen from Table 4, the accuracy of the

fitting procedure using Microsoft Excel Add-in,

Solver, is extremely good, as described by the FOM

widely used Al2O3:C dosemeter (open cycles) together with

the fitted curve (solid line) using the MOK model. The

individual components of the Al2O3:C LM-OSL curve are

also shown in the same figure.

368

Peak 5

CONCLUSIONS

The deconvolution process for TL as well as linear

modulated optically stimulated luminescence curves

using a common Microsoft Excel spreadsheet was

outlined in this paper. Both GOK and MOK functions can be used for deconvolution. It should be

noted that the same process can be used for analysing the sum of a number of exponentials and is not

limited to TL and LM-OSL cases presented explicitly in this paper. For instance, CW-OSL curves can

be analysed in a similar way by applying the transformations proposed by Bulur.

The process uses the Solver utility, a Microsoft

Excel add-in, that is also briefly presented here;

Specific examples of both TL and OSL computerised curve deconvolution analysis using the

spreadsheet along with the Solver add-in, are given.

These examples show that the luminescence trapping

parameters can be estimated with a high accuracy

with a simple procedure without the need of complicated and specialised computer codes. The accuracy

of the results was further confirmed in the case of

TL by comparison with the results of the

GLOCANIN project.

This work shows the power of using a simple

interface commercial software such as Microsoft

Excel, in order to carry out complex scientific problems, such as computerised curve deconvolution

analysis. It should be noted that the authors strongly

recommend the usage of the Solver utility because it

is used within the familiar Excel environment; so

new commands and procedures do not have to be

learnt.

luminescence computerised curve deconvolution

analysis can be obtained on-line from the web site

(www.ipet.gr) of the Archaeometry Department, of

the Cultural and Educational Technology Institute

by filling a registration form with the contact information. The spreadsheets are offered free of charge,

as long as they are not used for commercial purposes

or as a part of a system for dose assessment (21).

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369

for the GOK model and 0.000054 % for the MOK

model. It should be noted that the estimated values

of the parameters in both cases are almost the same

with very small deviations.

In Table 5, the calculated peak parameters for the

experimental LM-OSL curve of Al2O3:C are given, as

they were estimated by applying the Solver add-in

utility on the function of the GOKand on the function

of the MOK, in the Microsoft Excel spreadsheet.

Figure 5. LM-OSL Curve fitting of Al2O3:C using

excel spreadsheet and the Solver Add-in under

General-order kinetics model. In the lower graph

values for residual LM-OSL intensity versus stimulation time, after curve fitting is presented.

As can be seen from the low FOM values (1.410

and 1.389% for the GOK model and the MOK

model, respectively), the curve deconvolution analysis process was very accurate. Deviations between

the estimated values of each of the components presented, in stimulation time at peak height (tmax), in

Integral, is also presented. These values are in great

agreement with those reported in the literature(20).

D. AFOUXENIDIS ET AL.

19. Bos, A. J. J., Piters, T. M., Gomez Ros, J. M. and

Delgado,, A. An intercomparison of glow curve analysis

computer programs: I. synthetic glow curves. Radiat.

Prot. Dosim. 47, 473 477 (1993).

20. Dallas, G. I., Polymeris, G. S., Stefanaki, E. C.,

Afouxenidis, D., Tsirliganis, N. C. and Kitis, G. Sample

dependent correlation between TL and LM-OSL in

Al2O3:C. Radiat. Meas. 43(2 6), 335 340, (2008).

21. Bos, A. J. J., Piters, T. M., Gomez Ros, J. M. and

Delgado,, A. An intercomparison of glow curve analysis

computer programs: II. Measured glow curves. Radiat.

Prot. Dosim. 51, 257 264 (1994).

370

Appl. Phys. 39, 1500, (2006).

16. Balian, H. G. and Eddy,, N. W. Figure-of-merit

(FOM), an improved criterion over the normalized chisquared test for assessing goodness-of-fit of gamma-ray

spectral peaks. Nucl. Instrum. Methods 145(2),

389 395 (1977).

17. Billo, E. J. Excel for Scientists and Engineers. Wiley

(2007).

18. Fylstra, D., Lasdon, L., Watson, L. and Waren, A.

Design and use of the Microsoft Excel solver. Interfaces

28, 29 55 (1998).

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