Infrared Physics & Technology 45 (2004) 93101

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Rapid, non-destructive and non-contact inspection

of solid foods by means of photothermal radiometry;
thermal eusivity and initial heating coecient
a,b a,*
A. Gijsbertsen , D. Bicanic , J.L.W. Gielen c, M. Chirtoc d

a
Laser Photoacoustic Laboratory, Biophysics Division, Department of Agrotechnology and Food Sciences, Wageningen University,
Dreijenlaan 3, 6703 HA Wageningen, The Netherlands
b
Laser Center and Department of Physical Chemistry, Vrije Universiteit Amsterdam, De Boelelaan 1083, 1081 HV Amsterdam,
The Netherlands
c
Department of Mathematical and Statistical Methods, Biometris, Wageningen University, Bornsesteeg 47, 6708 PD Wageningen,
The Netherlands
d
Institute of Isotopes and Molecular Technology, P.O. Box 700, 6400 R Cluj-Napoca 5, Romania
Received 9 January 2003

Abstract

CO2 -laser photothermal radiometry (PTR) was demonstrated to be suitable for the non-destructive and non-contact
characterization (both optical and thermal) of solid phase agricultural commodities (fresh vegetables, fruits) and
confectionery products (candy). Proper interpretation
p
of PTR signals enable one to calculate two parameters, i.e. the
well known thermal eusivity e (e kqcp , where k and qcp are the thermal conductivity and the volume specic heat,
respectively) and a newly introduced physical quantity termed initial heating coecient chi (v b=qcp , b is the
absorption coecient). Obtained values for e are in a good agreement with data reported in the literature. PTR enables
one to rapidly determine e via a single measurement. As opposed to this, the knowledge of two out of three thermo-
physical parameters (thermal diusivity, thermal conductivity and volume specic heat) is a condition sine qua non for
determining eusivity in the conventional manner.

2003 Elsevier B.V. All rights reserved.

1. Introduction of (temperature dependent) thermophysical pa-

There is a continuous and a widespread demand
in the food industry for accurate numerical values
*
Corresponding author. Tel.: +31-317-484954; fax: +31-317-
482725.
E-mail address: dane.bicanic@wur.nl (D. Bicanic).
rameters. Properties such as volume specic heat
(qcp ), thermal conductivity (k), diusivity (a) and
thermal eusivity (e) are required to predict heat
transfer rates needed for the design, operation and
control of numerous processes concerning foods
and are also related to the quality of foods [1]. In
principle, the thermal properties of foods can be
predicted if their composition, porosity and

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2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.infrared.2003.07.003
94 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101
temperature are known [2]. The earlier heat
transfer analysis of the heating and cooling of food
products was actually oversimplied, as it relied on
constant, uniform values of thermal properties.
Modern techniques are capable of dealing with
thermal properties that alter with time, tempera-
ture and location during the treatment of foods [3
7]. The two major reasons for the general lack of
data concerning the thermophysical properties of
foods are the complex nature and the ever in-
creasing number of available food products. The
fact that conventional characterization techniques
are destructive, time consuming and in addition
often require substantial quantities of test sample
for analysis, is stimulating research attempts to-
wards the development of new methods.
Photoacoustic (PA), photothermal (PT) and re-
lated methods are emerging as novel techniques for
the measurement of thermal and optical properties
of samples in practically any physical condition
[8,9]. Common to these techniques is the detection
of heat (or the eects of this heat) generated as a
result of the samples absorption of periodically
modulated (or pulsed) incident radiation.
So far, some PT methods have been used for the
thermal characterization of foods (solids, liquids,
pasty and gels) and a few biological materials. Two
recent examples are (i) the concept of a thermal
wave resonant cavity (compatible with non-
aggressive liquids) [10,11] that has proved useful in
highly accurate measurements of the thermal dif-
fusivity a and (ii) the inverse photopyroelectric
technique (IPPE), a simple and very ecient ap-
proach towards directly obtaining thermal eu-
sivity e [12,13]. The IPPE as well as its (Standard)
counterpart SPPE, require intimate thermal con-
tact between the detector and the sample under
investigation. Such a requirement is easily met for
(semi-) liquids and gels, but not for solid samples
that are usually investigated by photothermal
beam deection (PTBD), photoacoustic (PA)
spectroscopy and photothermal radiometry (PTR)
[14,15]. Both PTBD [16] and PA [17] enable the
experimentalist to obtain the thermal diusivity
(a). In addition, Balderas-L
opez et. al. applied the
temperature rise technique to determine the vol-
ume specic heat (qcp ) and then used this value to
calculate e [18].
In the past, argon-laser based PTR was used to
monitor qualitative changes induced in margarine
exposed to UV light [19] and to characterize the
drying of cheese [20], while infrared ash ther-
mography was used to monitor the rmness of
fresh apples and the ripeness of raw tomatoes [21].
The main drawback in using Ar-laser radiation for
the heating of biological tissue is (partial) trans-
lucence of such samples; this induces scattering
within the sample and generally a weak signal,
which complicates greatly the quantitative inter-
pretation. The problem of incomplete opacity is
less serious if CO2 laser is used for the excitation.
However, in this case there is the problem in that
the excitation wavelength (10.6 lm) and the
wavelength corresponding to the maximum of
spectral emittance (at room temperature) are
practically in the same wavelength region. This
might cause problems when trying to discriminate
between the incident laser radiation and the ther-
mal radiation emitted by the sample under inves-
tigation.
This article describes the application of the
CO2 -laser for quantitative PTR studies of solid
fresh agricultural commodities (vegetables and
fruits) and confectionary products. The thermal
eusivity (e) and initial heating coecient (v) of
these samples were obtained directly from the
phase and the amplitude of the PTR signal.
2. Theory
Essentially, PTR measures the emittance of the
sample, that depends on the surface temperature
(StefanBoltzmann law). In the experiments de-
scribed below, the sample is periodically heated
due to the absorption of laser radiation. Since,
relative to the ambient temperature, the periodical
change of the surface temperature is rather small
(of the order of 7 mK at 100 Hz), there is a direct
proportionality between the latter quantity and the
emittance and thus the PTR signal as well.
All test samples studied here are thermally and
optically thick, which means that their thickness
(L) is much larger thanqthe
penetration depth of
2a
the thermal wave (l x , where a is the thermal
 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101 95

diusivity, and x is the angular frequency) and the 

A

penetration depth of the optical wave (1=b). Since Te x; s F s exp  bx
only a part of the samples area illuminated by a s  ab2
r  r
modulated laser beam is actually projected on the a s
b exp  x : 4
active element of the detector, the use of a one s a
dimensional model is justied. Using the energy
Since the emitted radiation originates from the
conservation law, the following partial dierential
samples surface (water present in the test sample
equation can be derived [17].
has an absorption peak in the detection band-
Tt x; t aTxx x; t A
f t expbx; 1 width), one can substitute x 0 in Eq. (4), which
then reduces to:
with:
Te 0; s GsF s; with

bI0  r
A qcp
initial temperature gradient ( vI0 ) A
a
[K s1 ] Gs 1  b : 5
s  ab2 s
a k
qcp
thermal diusivity [m2 s1 ]
T temperature (relative to ambient temper- In Eq. (5), Gs is the transfer function, while F s
ature) [K] is the normalized input signal (i.e. laser intensity
I0 incident laser intensity (unmodulated) It divided by maximum intensity I0 ). As to Gs,
[W m2 ] it can be written in a more simplied form:
b absorption coecient per unit length A

[m1 ]. Gs p : 6
s b as

The unmodulated incident laser intensity I0 Assuming sinusoidal heating, the phase and am-
(It I0 f t) used in Eq. (1) is already corrected plitude response can be found after substituting
for reection loss at the surface of the sample with s ix, where x [rad s1 ] is the (angular) modula-
reectivity r. The incident intensity Iin and the in- tion frequency:
tensity I0 entering the sample are related through: A

Gix p : 7
I0 1  rIin : 2 ix b aix
Assuming that (i) the heat exchange between The amplitude (dT ) and phase (/) can now be
the sample and the surrounding air is negligible calculated by taking the absolute value and the
compared to the heat ow due to conduction into argument of Gix:
the sample and (ii) the initial temperature is uni- q
2 2
form, the boundary conditions (bc) and the initial dT jGixj RGix IGix ; 8
condition (ic) read as:  
IGix
bc1 : Tx 0; t 0; / argGix arctan : 9
RGix
bc2 : T 1; t 0;
ic : T x; 0 0: Substituting A
in Eq. (7) and thus obtained Gix
in Eqs. (8) and (9), gives the following expressions
The Laplace transform: L : T x; t ! Te x; s and for the amplitude and phase:
L : f t ! F s, changes Eq. (1) into:
bI0
dT q
p ; 10
o2 Te x; s s e A

 T x; s  F s expbx: 3 qcp xx b2 a b 2ax
ox2 a a
Solving this equation by using the boundary con- p !
2x
ditions given above, one obtains the temperature /  arctan 1 p : 11
function Te x; s in the Laplace domain: b a
96 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101

Thispequation
can be rewritten in terms of I0 bc
e kqcp [J m2 K1 s1=2 ] and v b=qcp H ix
qcp b c
[m2 KJ1 ]. The rst quantity is the well known p p
thermal eusivity, the latter is termed the initial ix ab c
 p p p p p :
heating coecient. Mathematically, this latter is ix ac ix ix ab
the time derivative of the surface (x 0) temper- 18
ature, when the laser initially (t 0) strikes the
sample. Both the phase dierence (h) between the modu-
lated incident laser radiation and the radiation
Tt x 0; t 0 vI0 K s1 : 12 emitted by the sample and the amplitude (dM) of
the radiation emitted by the sample can be calcu-
Eqs. (10) and (11) now become: lated by taking, respectively, the argument and the
vI0 absolute value of H ix:
dT q
p ; 13
xx e2 v2 ev 2x h argH ix; 19

p ! dM jH ixj: 20
2x
/  arctan 1 : 14 Eqs. (19) and (20) are not only cumbersome but
ev
in addition require the availability of one addi-
tional parameter (c) that must be estimated from
From Eqs. (13) and (14), one can calculate e and v
measured data. An attempt was made to use this
directly from the measured phase and amplitude.
improved model in order to t the frequency de-
p
2x pendent measured data for agar and to estimate
v ; 15 the model parameters i.e. b, c, a and qcp . More-
etan/  1
over, to reduce the number of model parameters
p one also tried to set b c thereby making it pos-
2I 0
e p : 16 sible to estimate e and v. Neither attempt, how-
2
xtan / 1dT ever, resulted in a signicant improvement in the
To some extent, a shortcoming of the model t to the frequency dependent measurement data
above is the fact that it relies on the amplitude and of the amplitude and phase dierence for agar.
phase of the time dependent surface temperature. Because of this and the simplicity of the surface
Such a model is only valid if the mean absorption temperature model, Eqs. (15) and (16) were used to
coecient (c) of the sample in the detection perform the calculations, the outcome of which is
bandwidth is much larger than that (b) at the laser described in this paper.
wavelength. If this is not the case, then the model
discussed above has to be improved by multiplying
the temperature function in Eq. (5) by ecx and 3. Materials and methods
then integrating the temperature spatially to ob-
tain the time dependent emitted radiation Ms in The experimental setup used for the PTR
the Laplace domain: measurements is shown in Fig. 1. The excitation
Z 1 source is a c.w. line tuneable waveguide CO2 -laser
A
(A) tuned to the 10P20 line (10.55 lm), providing
Ms F s exp  bx
s  ab2 0 as much as 3 W output power. At this wavelength,
r  r
a s the absorption of water exhibits a broad spectral
b exp  x ecx dx: 17 peak. Laser radiation, modulated by a home-made
s a
mechanical chopper (B), was reected at plane
The transfer function H s can be calculated after gold coated mirrors (C, G, H) and directed onto
integration; substituting s ix gives: the sample (K). A beam director (D) inserted be-
 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101
Fig. 1. Experimental set-up used for PTR studies in IR.
tween C and G enables one to identify (F) and to
measure (E), the power of the incident laser
emission.
For actual PTR measurements, CO2 laser ra-
diation was rst allowed to pass through an AR/
AR coated ZnSe lens (I, Laser Power Optics,
f 254 mm, 24:5 mm) and a circular hole
( 5 mm), drilled o-axis in a Leybold 389 24 B
aluminium parabolic (f 300 mm, 420 mm)
reector (J) before striking the sample (K). The
sample was mounted in a holder (positioned at
2f 600 mm from J) that itself was axed on a
xyz stage. The choice of the focal length and the
location of ZnSe lens were such that the diameter
of the laser beam on the sample was about 8 mm.
In order to prevent damage of the sample by in-
cident radiation, the output power of the laser was
reduced by adjusting the discharge conditions. For
the studies on agricultural commodities, the laser
power measured directly behind the chopper was
between 150 and 600 mW corresponding to 0.20.8
W cm2 intensity at the sample. The spatial dis-
tribution of the laser beam was controlled using a
thermal imaging plate.
At the excitation wavelength, the surface re-
ectivity from biological tissue varies from one
sample to the other, but it is generally weak.
Typical values for (1  r) for biological samples
and water span the range extending from 0.95 to
0.99 [22,23] at wavelengths around 10 lm. In this
study it is assumed that the surface reectivity for
all samples studied here is equal to that of agar;
This assumption results in a 45% experimental
97
error for e and v. The amplitude depends on r as
2
1  r (assuming that the reectivity at the laser
and at the detection wavelength is the same), while
the phase lag is surface reectivity independent.
Furthermore throughout all the measurements
thermal imaging plates where used to control the
spatial distribution of the laser beam.
The thermal radiation emitted by the absorbing
sample was collected by the same parabolic re-
ector (J) and then focussed on a high speed, li-
quid nitrogen cooled Mercury Cadmium Telluride
detector (L) from Infrared Associates (MCT-
13-1.0, ZnSe wedge) mounted on a scissor jack and
positioned in the same vertical plane as the sample.
To prevent the forward scattered laser radiation
from hitting the detector and causing undesirable
signals, a LiF lter (M) was used right in front of
the detectors entrance window. The LiF lter is
open for wavelengths shorter than 8 lm and
practically opaque for wavelengths longer than 9
lm. The detector sees radiation the wavelength
of which exceeds 5 lm. This means that the actual
detection takes place around the dominant ab-
sorption peak of water at 6.08 lm, implying that
the radiation to be detected originates from the
very surface of the sample. This justies the use of
the above-discussed model (Eqs. (15) and (16)),
which assumes that the detector sees solely the
surface and not the inside of the test sample.
The PTR signal from the detector was pre-am-
plied and then fed into a two phase 3961B Ithaco
lock-in amplier. The alignment of the set-up was
checked by measuring the lock-in signal obtained
either without the sample or from a strongly re-
ecting sample; in both cases the PTR signal was
approximately zero (<3% of signal for agar gel). In
addition, a TiNx surface absorbing reference
sample (dimensions 50 mm 50 mm 5 mm) of
quarts coated with 1.1 lm thick layer of TiNx
(DIN 50992-2, kindly provided by Phototherm Dr.
Petry GmbH) was used to test the set-up. For such
a reference sample the phase dierence should be
)45 and independent of the modulation fre-
quency [24]. Indeed, with TiNx as a test sample the
phase dierence was shown constant over the en-
tire frequency range, while p the
amplitude was di-
rectly proportional to 1= f as predicted by
theory. The result of a test measurement is shown
98 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101

in Fig. 2. At a given modulation frequency, the radiation. The modulation frequency was then
PTR signal from the selected site was measured changed and step (iv) repeated; such a procedure
during a 20 s long interval. was performed for at least six dierent frequencies
The TiNx reference sample was also used to spanning the range between 10 and 100 Hz and
determine the instrumental phase (IP []). On the completed by the control measurement of laser
other hand, agar gel (1% agar, with thermal output power. The test sample was then removed
properties same as water [25]) and graphite from the holder, agar (or graphite) mounted in-
(Ringdor) were used to obtain the instrumental stead and IC determined again to make sure that it
constant (IC [V W1 K1 ]). While IP represents the did not change during the measurement. If, during
frequency independent oset between the phase a measurement, the signal did not reach a constant
read from the lock-in amplier (/li ) and the real level (although both IC and power P did not
(theoretical) phase (/), IC is a constant giving the change) but instead continued to increase slowly
relationship between the amplitude reading of the due to a drying process induced by heating, the
lock-in Ali [mV] (normalized to the incident power sample was slightly displaced prior to performing
P [mW] of the laser) and the amplitude of the the next measurement. In this manner dierent
surface temperature (dT ): regions on the sample were irradiated in each
/ /li  IP; 21 consecutive measurement. Such a drying eect
causing a drop of e with time (which generally
Ali induces an increase of amplitude) was minimized
dT : 22 by reducing the laser output power.
P IC
Once IC and IP were determined, PTR mea-
surements on various test samples were made. The
4. Results and discussion
measuring protocol included the following steps:
(i) mounting of the sample, (ii) measurement of the
To demonstrate the potential of PTR to obtain
laser power P , (iii) selection of the modulation
the thermal eusivity of solid foods in a simple and
frequency and (iv) recording (lock-in amplier) the
rapid manner, one has studied fresh fruits and
amplitude and the phase of the PTR signal for
vegetables (tomato, pear, apple etc.) and confec-
about 20 s after exposing the sample to the laser
tionary products; the results are summarized in
Table 1. The test samples were purchased at a local
supermarket. Frequency scans obtained from
4
lock-in amplitude [mV]

several test samples are plotted in Fig. 3.

3 The standard deviation for v reported in Table
2 1 refers to ve consecutive measurements at 12.8
1
Hz. The standard deviation for e was calculated
using the data obtained from measurements con-
0
0 0.05 0.1 0.15 0.2 0.25 0.3 ducted at ve dierent frequencies at least. Based
1/sqrt(f) [1/sqrt(Hz)] on measurements on agar gel and graphite (these
80 reference samples have well known properties), a
lock-in phase [deg]

60
typical accuracy for e attained in PTR measure-
ments is estimated to be 5%.
40
It was found in this study that, dierent from
20
what was expected, all test samples exhibited a
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 slight decrease of v (depending on the sample this
1/sqrt(f) [1/sqrt(Hz)] decrease varies between 10% and 20%) for in-
Fig. 2. The amplitude (top) and the phase (bottom) of the PTR creasing modulation frequency. The initial heating
signal obtained from the TiNx reference sample used to test the coecient v is directly proportional to b via
experimental set-up. v qcbp . The reader is reminded that values for v
 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101 99

Table 1
Thermal eusivity and initial heating coecient of foods at 293 K acquired by PTR
Sample v (103 m2 KJ1 at 12.8 Hz) e (103 J m2 K1 s1=2 )
Chocolate (pure) 19.6 0.5 0.83 0.03
Chocolate (pure, melted) 21.7 0.3 0.622 0.005
Peppermint 36.0 0.6 0.562 0.012
Tomato (normal) 26.5 0.8 1.35 0.03
Tomato (fresh) 28.2 0.9 1.31 0.05
Butter bean 12.4 1.2 0.42 0.05
Apple (Granny Smith) 17.5 0.6 1.20 0.05
Apple (Jonagold, 12.8 Hz) 23 4 1.32 0.03
Apple (Jonagold, 98 Hz) 14.0 0.5 (at 98 Hz) 1.07 0.06
Pear (D. du Commice) 18.3 0.1 1.23 0.03

25
chocolate (pure)
simultaneous decrease of polymer structures on
20
peppermint
pear approaching the surface. The net result of such a
agar gel
phenomenon is a decrease of the absorption coe-
A [mV]

15

10 cient (b) (at wavelengths associated with polymer

5 structures) with increasing modulation frequency.
0 Similar phenomenon may also take place in the
10 20 30 40 50 60 70 80 90 100
f [Hz] waterlike samples such as those investigated in this
55 study.
50 For practically all investigated samples e was
phase [deg]

45 found to be independent of modulation frequency.

40
35
30
10 20 30 40 50 60 70 80
f [Hz]
Fig. 3. The amplitude (top) and the phase (bottom) of the PTR
signal obtained from four dierent samples plotted versus
modulation frequency. The IC and IP are 570 V W1 K1 and
106 respectively. The incident laser power P at 10P20 measured
at E (Fig. 2) was 560 mW for confectionary products as com-
pared to 600 mW for agar gel and fruits.
given in Table 1 refer to a measurement at 12.8 Hz
(at this lowest attainable frequency in our mea-
surements, the thermal diusion length is maxi-
mal). A possible explanation for the observed
dependence of v on f can be attempted using data
of Haas et al. [26], who conducted a PA study of
liquid water, heavy water and alcohol in the near
infrared. They concluded that these samples (ex-
hibiting the association to polymerlike structures
through hydrogen bonds) reveal a structural
modication from the interior of the liquid to-
wards the liquidgas boundary. This was ex-
plained [26] by an increase of monomers with a
The only exception was a Jonagold apple, that
exhibited relatively large dierences in both e and
v values. Presumably, this is due to dierences in
90 100
the properties of the skin and lower layers. It
might be that at 98 Hz it is only the skin that is
being probed, while the underlaying tissue plays a
role at 12.8 Hz. The large standard deviation for v
can probably be ascribed to the variations of the
skin thickness.
From Table 1 one concludes that e correlates
well with the moisture content of the sample;
butterbean that is rather dry has a low e. Clearly,
the higher the moisture content of the sample, the
closer the value of e to that of water, i.e. 1585
[J m2 K1 s1=2 ].
The use of PTR for the measurement of eu-
sivity is not limited to studies of fresh fruits and
vegetables. Other samples featuring low reection
or no reection at all can also be investigated, as
demonstrated here (Table 1) by studies on choco-
late (hard and melted as a result of interaction
with laser radiation) and peppermint candy. Val-
ues of e obtained by PTR for chocolate are close to
those from the literature [27]. While the eusivity
100 A. Gijsbertsen et al. / Infrared Physics & Technology 45 (2004) 93101
of melted chocolate was found to be slightly larger
than that of solid chocolate, the trend in the values
of v is just the opposite.
5. Conclusion
To the best of our knowledge, this paper de-
scribes the rst application of room temperature
CO2 laser PTR for studies of foods. The spectral
overlap of incident and emitted radiation (the
major experimental diculty normally expected in
this kind of studies) could be eectively suppressed
by inserting a LiF lter in front of the detector.
The results of this study conrm the suitability
of room temperature CO2 PTR for the precise
(5%) assessment of thermal eusivity (e) and the
initial heating coecient (v) of solid foods. The
eusivity values obtained by PTR agree with cal-
culated values reported in the literature [27]. The
information obtained from a PTR measurement is
related only to the properties of the surface layer
and near-surface layer. The PTR approach de-
scribed here requires a calibration with an opti-
cally opaque (b ! 1 at excitation wavelength)
reference sample having well known thermal
properties.
In conclusion, CO2 laser based PTR is a new
and practical technique for the rapid character-
ization of foods. Being by virtue of its operational
principle, non-destructive and non-contact, PTR
can in addition also be used for real time moni-
toring of e and v; practical examples include fol-
lowing processes in which e or v change; i.e.
drying, heating, cooling, melting etc. Another po-
tential application is the assessment of food
spoilage [28].
The technique can be adapted to allow studies
on liquid and pasty samples as well. Finally, the
feasibility of the PTR method for measurements of
e at elevated temperatures is anticipated.
Acknowledgements
The authors express their gratitude to H.G.
Walter (Jena), J.C. Krapez (Chatillon), W. Mastop
(FOM Rijnhuizen), R. Wolthuis (Rotterdam), K.
van Asselt, M. Schimmel and O. Ganguli (Wa-
geningen) for their help received during this study.
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