Sensors and Actuators B 161 (2012) 528533

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Sensors and Actuators B: Chemical

journal homepage: www.elsevier.com/locate/snb

Metal oxide sensor arrays for detection of explosives at sub-parts-per million

concentration levels by the differential electronic nose
K. Brudzewski a, , S. Osowski a,b , W. Pawlowski a
a
Warsaw University of Technology, Warsaw, Poland
b
Military University of Technology, Warsaw, Poland

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

Article history: The study presents an application of the differential electronic nose to the estimation and recognition of
Received 25 October 2010 the TNT, PETN and RDX in the complex environments under their storage. Generally there are two separate
Received in revised form 13 October 2011 problems in the eld of recognition of explosives: rst detection of the trace concentration of explosives
Accepted 31 October 2011
by analytical methods (gas chromatography, ion mobility spectrometry, neutron activation analysis) and
Available online 6 November 2011
the second the estimation of the state of explosives during their time storages in the military objects. In
the second problem the concentration of a vapor of explosives is at level of sub-parts-per million where
Keywords:
chemosensors technique is fully applicable. This paper is concerned with the second type problem. It
Explosives
Recognition
denes the recognition criteria providing stable and robust basis for the recognition of different explosive
Electronic nose materials. The important part of this procedure performs the 2-dimensional convolution of the differential
2 dimensional convolution signals formed on the basis of two sensor arrays used in the construction of the differential nose. The
experimental results of the recognition of TNT, PETN and RDX have conrmed the excellent recognition
ability of the developed system.
2011 Elsevier B.V. All rights reserved.

1. Introduction
The chemical sensors are important tools for the rapid detec-
tion of explosives and nd applications in tactical and humanitarian
demining, remediation of explosives manufacturing sites, as well
as forensic and criminal investigations. Although various advanced
methods of explosives detection such as the ion mobility spec-
trometers, gas chromatographs, mass spectrometers, and their
combinations [1,4,5,6] are available, the simple techniques are
often also very effective. The most known example of such tech-
nique is an electronic nose [3]. Actually it is used as an indirect
technique for sensing explosives packages, especially at an inves-
tigation of the time storage and time degradation of explosive
materials.
The materials such as trinitrotoluene (TNT), pentaerythritolte-
tranitrate (PETN) and cyclotrimethylenetrinitramine (RDX) are
examples of such explosives. Resistive sensing of the TGS sen-
sors is possible because these substances dissolve and emit volatile
components of the concentration depending heavily on ambient
temperature and humidity. In this way TNT emits mainly 2,4-
dinitrotoluene, 1,3-dinitrobenzene, 2,4,6-trinitrotoluene, while
Corresponding author.
E-mail address: brudz@ch.pw.edu.pl (K. Brudzewski).
RDX easily dissolves and emits many nitro-oxides. On the contrary
the PETN is very stable in ambient air although dissolves in water
(hydrolysis).
Very interesting approach to the detection of explosive mate-
rials is the application of the semiconductor gas sensor arrays,
sensitive to the explosive smells. Application of such arrays offers
several advantages low cost of production, quick procedure of
recognition, sensitivity to a wide range of analytes, relatively good
selectivity, multicomponent analysis as well as analyte recogni-
tion. The only limitation of this technique follows from the limited
sensitivity of the actually produced semiconductor gas sensors. It
is a common opinion that the concentration range of the explo-
sive smell to be discovered by these sensors is in the range
106 109 g/ml [4,5,6]. The distributed response of an array, mea-
suring the changes in electrical conductivity, is used to identify
the constituents of a vapor sample. The measured signals are then
analyzed by advanced signal processing methods, able to associate
this response with a smell specic to the particular explosive. To
provide the highest selectivity of recognized classes by an elec-
tronic nose, different measures of similarity have been tried in
the past. The most important among them are: the correlation,
Euclidean and Mahalanobis distances as well as KulbackLeibler
and KolmogorovSmirnov statistical measures [1,3,7,8].
However the application of conventional solution of electronic
nose based on one semiconductor array of sensors suffers from

0925-4005/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2011.10.071
 K. Brudzewski et al. / Sensors and Actuators B 161 (2012) 528533 529

Fig. 1. The general scheme of the differential nose used for recognition of explosive
materials.

some disadvantages, like the decreased sensitivity due to the small

concentration of smell or change of the baseline due to the variation
of temperature, humidity, and other environmental conditions. Fig. 2. The distribution of the mean values of differential signals of 12 pairs of
In this work, we present a novel approach to the problem of sensors at 100 measurements.

explosive detection, involving differential electronic nose com-

posed of two chemo sensor arrays [2] working in parallel. One of
them forms the measurement array and the second the reference
array. Both act in the same environmental conditions. The signals
measured by these two arrays are subtracted from each other, pro-
ducing a difference signal of greatly reduced interference effects
due to the changes in humidity or temperature of the environment.
Such system of gas measurement is more stable and resistive to
the changes of the environmental conditions, so its performance is
more stable and robust.
2. Design of experimental system
the ambient air was sucked with ow rate 0.5 SLPM by an inducting
pomp. The ambient temperature at the measurement was changing
from 15 C to 26 C and the humidity of air (RH) was changing from
18% to 31%. To provide stable values of the measured signals their
acquisition is done at the nal period of the measuring window (the
second half of it).
The corresponding signals registered by the appropriate sen-
sors of both arrays are subtracted from each other by using the
differential amplier, then converted by A/D converter to the digi-
tal form and nally delivered to the computer interface for further
processing, which leads to the recognition of smell.

The solution to the problem of explosive material recognition

3. Signal processing
proposed in the paper is based on the application of the differ-
ential nose [2]. The ow-air system for detection of the vapor
The rst point that should be checked in electronic nose is the
explosive compounds is shown schematically in Fig. 1. The most
independent behavior of all pairs of sensors forming the differential
characteristic point is the application of two sensor arrays instead
signals of the nose. Fig. 2 presents the distribution of the average
of one, usually applied in the conventional solutions. The streams
values of differential signals of 12 applied pairs of sensors at 100
of air are delivered to both chambers of gas sensor arrays from
measurements of the investigated explosives: TNT, PETN and RDX.
the odor acquisition place through the socket outlet. The mea-
As it is seen the responses of the individual sensors are different
surement channel contains inside the vapor of explosive material,
for the same explosive and form the patterns characteristic for the
while the reference one only the outside air, free of explosive smell.
particular explosive material. Moreover, we can observe the signif-
Both arrays provide simultaneous information of the actually mea-
icant change of the differential response of the same sensor pairs
sured odors (as with a traditional e-nose), but only differential
for different materials. To nd the statistical relationship between
proles of signals are stored and processed further. In the pre-
the sensor signals at different explosives we have calculated the
sented system both sensor arrays are identical and composed of
correlations between them. Table 1 illustrates the results of the
12 heated metal oxide gas sensors of Figaro series: 2xTGS2600-
correlations between the sensor signals corresponding to all three
B00, 2xTGS2602-C00, TGS2610-C00, TGS2610-D00, TGS2611-C00,
investigated explosive materials.
TGS2611-E00, 2xTGS2612-D00, 2xTGS2620-C00. We have applied
the sensors of series 26xx, known from their high stability of
operation and small size. Some sensors in both arrays have been Table 1
duplicated to compensate for their limited number of types. All The correlations of the sensor signals for all applied sensor pairs.
sensors have been wired in series with a potentiometer, used Sensor Corr(RDX, PETN) Corr(RDX, TNT) Corr(PETN, TNT)
to tune the level of the sensor output signal at clean air envi-
Sensor 1 0.0727 0.3005 0.0243
ronment. The duplicated sensors have been adjusted to work at
Sensor 2 0.1976 0.1039 0.2970
different loadings, hence their output signals are different. To pro- Sensor 3 0.8120 0.5568 0.5113
vide the information of temperature and humidity we have used Sensor 4 0.6050 0.5050 0.4992
additionally the temperature sensor LM35DH and humidity sensor Sensor 5 0.4680 0.3819 0.0059
HIH-3610-02. Sensor 6 0.1832 0.5830 0.1170
Sensor 7 0.1080 0.4592 0.2285
The measurement array senses the vapor of explosive material Sensor 8 0.8876 0.4918 0.5507
delivered to it through the socket outlet. The sample of about 1 g of Sensor 9 0.0300 0.5744 0.0394
the explosive materials was placed in cylindrical vial in the channel. Sensor 10 0.5722 0.6697 0.5091
The total volume of this vial was about 200 ml. The second array Sensor 11 0.0982 0.2278 0.2268
Sensor 12 0.0296 0.1980 0.2625
(the reference one) senses only the ambient air. In both channels
530 K. Brudzewski et al. / Sensors and Actuators B 161 (2012) 528533
Fig. 3. The PCA mapping of the signals of 12 sensors corresponding to three inves-
tigated explosives.
It is evident that the signals of all sensors corresponding to dif-
ferent explosives are weakly correlated. It means that the choice
of the sensors applied in the system is appropriate to differentiate
smells of the explosives. It provides good basis for the electronic
nose application. Fig. 3 illustrates the distribution of the vectors of
12 sensor signals corresponding to RDX, PETN and TXT mapped on
two most signicant principal components: PCA1 and PCA2 . Each
explosive material was represented by 1000 samples. It is evident
that the patterns of measured signals of the sensors separate the
explosives very well. The samples belonging to different explosives
form the individual clouds of data, separated from each other.
This observation conrms our good choice of sensors and points
to the ability of the proposed sensor array to recognize different
explosive smells. It means, that the only problem to be solved is
the computation technique that should be applied to separate the
patterns corresponding to the actual measurement. The distribu-
tion of these patterns suggests application of the simplest linear
technique.
First we tried to analyze the sum of all sensors corresponding
to different gases. Fig. 4 presents the distribution of these sums
of the crude differential signals of 12 sensors applied in the elec-
tronic nose for TNT, PETN and RDX corresponding to one session
of the measurements. The results depict 100 registrations acquired
within the time window of 30 s. All values of signals are expressed
Fig. 4. The distribution of the sum of the measured crude differential signals (in
volts) of 100 samples of all 12 sensors acquired within the time window of 30 s.
in volts. It is evident that the differences between the crude
differential signals corresponding to two different explosives are
very low.
The measured values of all samples are very close to each other.
For RDX the mean value was equal 0.0264 V with standard deviation
std = 0.0024 V, for TNT the mean was 0.0163 V at std = 0.0005 while
for PETN the mean value was equal 0.053 V with std = 0.00008. Tak-
ing into account some possible changes in the environment and
instability of the sensor characteristics it is evident, that the actu-
ally observed differences between two mean signals belonging to
different explosives (lower than 0.01 V) form not satisfactory basis
for taking the reliable decision. Therefore we have to apply addi-
tional processing of the signals leading to the greater enhancement
of this difference.
Among many different methods of signal processing the con-
volution and correlation play an important role as a measure of
similarity between two signals. In our case more appropriate is the
auto convolution, an operation convolving the signal with itself at
different delays (measured in number of samples). In our system
we will apply this procedure to enhance the difference between
the differential signals of the nose at different sniffed explosive
materials.
The measuring system registers samples of the sensor signals
at the sampling rate governed by the clock. Within the measuring
window we get the stream of p such samples for each sensor of
both arrays. The differential amplier generates the difference of
the corresponding sensor signals of both arrays, i.e.,
xi = xm xr (1)
for i = 1, 2,. . .,12, where the upper index m refers to measurement
and r to the reference array. At N = 12 sensors and p samples reg-
istered within the measurement window these samples form the
matrix X of the dimension p N. The signals gathered in the matrix
X represent numerically our recognition problem. Proper process-
ing of this matrix should enable us to extract the basic, reliable
features for the recognition of the smells corresponding to different
types of explosives.
The matrix X representing the differential signals is subject to
the 2-dimensional auto-convolution. This mathematical operation
for the matrix X is in general dened by the following equation
[9,11]:


s(n1 , n2 ) = x(k1 , k2 )x(n1 k1 , n2 k2 ) (2)
k1 =k2 =
where x(i, j) is the i,jth element of the matrix X and n1 , n2 are the
shift indexes, changing, respectively, p n1 p and N n2 N.
The values of s(n1 ,n2 ) form the resulting convolution matrix S.
The size of the matrix S in each dimension is equal to the dou-
ble dimension of the input matrix, minus one. It means that at
the assumed size p N of the original matrix X, the size of S is
equal (2p 1) (2N 1). Each column of this matrix represents
the cumulated information corresponding to the appropriate sen-
sor signals at different delays. In further processing we form the
sum of elements in each row, that is the cumulated signals coming
from all sensors. In this way the p delayed responses of N sen-
sors are represented by one column containing (2p 1) cumulated
results of the 2-dimensional convolution. The numerical experi-
ments performed for many different gas measurement processes
have conrmed that this kind of representation greatly enhances
the differences among different smells.
4. Experimental results
The experiments have been performed for the recognition of
three types of explosive materials represented by TNT, PETN and
 K. Brudzewski et al. / Sensors and Actuators B 161 (2012) 528533 531

RDX. All measurements have been done using the developed differ-
ential nose system. In each experiment we have used the sample of
1 g of the appropriate explosive. The measurements have been car-
ried out under the following experimental conditions: the volume
of the sample chamber was 200 ml, the ow rate of an ambient air
controlled by an inducting pump was kept constant and equal 0.5
SLPM per sensor array, humidity of the air changes were kept in the
range of (2851%), the ambient temperature was varying from 15 C
to 26 C. The signals corresponding to the appropriate sensors of
both arrays have been subtracted by the differential ampliers and
then converted to the digital form and transmitted to the computer
using 16-bit AD converter (two modules of ADAM-4017). These
signals were then subject to the 2-dimensional auto-convolution
using MATLAB platform [11].
Our recognition strategy of different types of explosive material
was as following. For each explosive material we made the mea-
surements lasting 30 s, registering p = 100 sample results for each
of 12 sensors. We have performed many such measuring sessions
at different days and at various environmental conditions (differ-
ent temperature, humidity, air pressure, etc.). As a result, for each
explosive we collected the measured data organized in the form Fig. 5. The shape of the representative prole vectors for three investigated explo-
sive materials: PETN, TNT and RDX for 199 delays.
of X matrix: one corresponding to TNT, the second to PETN and
the third to RDX. Each matrix X was subject to the 2-dimensional
convolution, producing the results in the form of the appropriate for the indices i, j = TNT, PETN and RDX and k changing from (p + 1)
S matrix, according to Eq. (2) at different delays. In further analy- to (p 1). The simpler one (and still sufciently accurate) is the
sis we consider the convolution results corresponding to the delay measure in the form of the maximum absolute difference between
shifts changing from 99 to 99 samples (199 samples together). For both proles, i.e.,
each measuring session we collected the independent convolution
results. dij = max{abs(si (k) sj (k))} (5)
According to the 2-dimensional convolution formula we get the This measure will be applied in this work. Table 2 presents the
convolution results containing 2N 1 elements (N number of sen- calculated maximum distances between the representative prole
sors) for each delay. Denoting them by sij we generate the matrix S vectors of these three investigated explosive materials. We can see
of 2p 1 rows and 2N 1 columns. Summing up the values of the that they are now much higher than the original distances existing
row elements (column wise) we get the set of proles s(i) corre- among crude differential signals presented in Fig. 4.
sponding to ith delay (ith row of S matrix) in the form They form a good basis for the recognition of the actual sample
under investigation. To recognize the actual single sample of the

N
explosive material we have to register the response of both sen-
s(i) = s(i, j) (3) sor arrays of the differential nose, form the differential signals and
j=N calculate the appropriate convolution according to the presented
procedure. Next we compare the actual convolution results with
The highest value corresponds to the delay equal zero. The larger the representative prole vector of each explosive material, calcu-
(from zero) is the delay distance, the smaller is the value of this lating the maximum difference of them (at zero delay), according
sum. On the basis of these results we can dene the representative to Eq. (5). The smallest value of dij indicates the membership of the
prole vector of the dimension 2p 1 for each explosive. To cre- investigated sample to the appropriate explosive material.
ate this prole vectors we have performed 10 measuring sessions Fig. 6 presents the graphical results of comparison of the set of 11
for each explosive. The measured differential signals were subject measurements done for TNT, PETN and RDX (33 measurement ses-
to the 2-dimensional auto convolution forming the corresponding sions together). The horizontal axis represents the time delay (each
prole vectors of the components s(i) dened by the relation (3) for sample corresponds to 0.3 s) and vertical axis the cumulated val-
i changing from (p + 1) to (p 1). On the basis of these results we ues of the convolved signals corresponding to the appropriate time
have calculated their mean, called the representative prole, sep- delay. The bold lines are the representative prole vectors of each
arately for TNT (vector sTNT ), PETN (vector sPETN ) and RDX (vector explosive material and the other thin lines represent the actually
sRDX ). measured samples of the appropriate material. All measured sam-
Fig. 5 presents the resulting representative prole vectors for the ples of RDX are grouped around the representative prole vector
above three investigated explosive materials: RDX, TNT and PETN. of RDX. The same is true for TNT and PETN. It is seen that they are
It is seen that the distances between the values corresponding to closest to their corresponding representative vector.
different explosives at xed delays are now very large and form the Table 3 presents the statistical results in the form of the dis-
reliable basis for recognition of the explosive material. tances of the actually investigated single samples representing TNT,
Different measures of the distances between these proles may
be applied in practice. One of them is the total summed measure
Table 2
representing the global mutual distance between the pairs of the The maximum distances dij between the representative vectors for TNT, PETN and
prole vectors dened as the sum of differences over all delays, i.e., RDX.

TNT PETN RDX


p1

dij = abs (si (k) sj (k))

TNT 0 3.42 6.12
(4) PETN 3.42 0 9.54
k=p+1 RDX 6.12 9.54 0
532 K. Brudzewski et al. / Sensors and Actuators B 161 (2012) 528533

In assessing the ability of our differential nose to the recognition

Fig. 6. The graphical presentation of the positions of the single measured samples
of TNT, PETN and RDX and their representative prole vectors.
Table 3
The statistical results of recognition at 11 independent measuring sessions of three
investigated explosives in the form of their mean distances and standard deviations
(mean std) from the representative proles.
TNT prole RDX prole PETN prole
TNT samples 0.52 0.35 6.13 0.65 3.41 0.64
RDX samples 6.24 2.53 1.82 1.67 9.67 2.52
PETN samples 3.41 0.09 9.53 0.09 0.075 0.05
PETN and RDX explosives from their representative prole vectors.
Each explosive material was represented by 100 samples measured
11 times at different environmental conditions and different days.
The amount of explosive material placed in the vial was also slightly
changing in these measuring sessions.
The results are given in the form of the mean distances between
the actually measured samples and the appropriate prototype pro-
les as well as the standard deviations of these results. It is evident
that the distances between the actual measurement results and the
appropriate prole vectors of different explosives are high enough
for undertaking the reliable recognizing decision.
The smallest value of the distance dij indicates the recognized
type of explosive material. Small value of mean distance to the
appropriate prole of many samples at small standard deviation
provides good and stable basis for the recognition of the appropri-
ate explosive.
of the explosives we should also take into account the background
of volatile organic compounds (VOC), the organic chemicals that
have a high vapor pressure at ordinary, room-temperature [10].
Very important is the presence of ethanol, used in production of
the explosives, which may strongly inuence the signals of sensor
arrays. The molecules of ethanol that are not originating from the
explosives may either induce the false detection or mask the true
vapor.
Since the TGS sensors are very sensitive to ethanol vapors, we
have made additional experiments checking the explosive recog-
nition ability of our system in the presence of ethanol in the
environment. The ethanol source was placed in the vicinity of
our measurement system. The concentration of it in the ambi-
ent air was changing with time within the limits from 20 to
8 ppm.
Fig. 7 presents the 3-dimensional plot of the PCA mapping of
the differential sensor signals on three most important principal
components in the case of pure air (Fig. 7a) and presence of ethanol
(Fig. 7b) in the air. In spite of some differences of the plots the
separation of patterns representing different explosive materials is
still visible.
We have performed the dened earlier signal processing of the
differential signals measured in the presence of ethanol and com-
pared their proles with the representative proles determined
for pure air (without ethanol). Table 4 presents the calculated
maximum distances between the prole vectors of these three
investigated explosive materials measured in the presence of
ethanol and their representative vectors acquired in the pure
air.
It is evident that the presence of ethanol vapor did not change
the nal recognition results of the explosives. The minimum dis-
tance of the actually measured prole (with the presence of
ethanol) to the representative proles of the explosives, points
uniquely to the proper type of explosive. In each case the recog-
nition was perfect. These results show that in spite of the presence
of ethanol, our system was able to recognize properly each of the
explosives.
On the basis of results of the performed experiments we
may conclude, that the observed distances of the actually mea-
sured proles for TNT, PETN and RDX samples to the dened
representative proles provide sufciently safe tolerance margin
to avoid the misrecognition of the explosive material. Espe-
cially stable are the characteristics of RDX, for which we have
observed very good repetition of results at many measure-
ments In all investigated cases we have got perfect recognition
of all samples of the explosive materials (100% of recognition
accuracy).

Fig. 7. The 3-dimensional PCA mapping of the sensor signals to three most important principal components in the case of lack (a) and presence (b) of ethanol in the ambient
air.
 K. Brudzewski et al. / Sensors and Actuators B 161 (2012) 528533
Table 4
The maximum distances dij between the representative proles of TNT, PETN, RDX and the prole vectors of these explosives in the presence of ethanol.
Representative prole of TNT
Prole of TNT in presence of ethanol 2.83
Prole of PETN in presence of ethanol 2.23
Prole of RDX in presence of ethanol 10.45
5. Conclusions
The electronic noses detecting explosives are still at various
stages of development and a lot of new solutions must be tested
before being eld-operational. This paper has proposed the appli-
cation of two sensor arrays working in parallel, in order to increase
the sensitivity and stability of the nose at different environmental
conditions. The appropriate sensor signals of both arrays are sub-
tracted from each other forming the differential signals, which are
further processed to form the output signal capable to recognize the
smell of different explosives. Application of sensors working in dif-
ferential mode has made the system less susceptible to the change
of environmental conditions, since these changes are compensated
in the differential signal.
The experiments have been performed for three families of
explosives: the TNT, PETN and RDX. They have shown that the dif-
ferential nose is able to recognize the smells coming from these
families of explosives. The recognition is based on the maximum
distance of the actually acquired (convolved) differential output
signal of the electronic nose from the average of convolved output
signals of the particular type of the explosive materials existing
in the knowledge base (so called representative prole vectors).
The experiments performed for many measuring sessions of TNT,
RDX and PETN have shown perfect performance of the explosive
recognizing system based on the differential nose principle.
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Biographies
Kazimierz Brudzewski was born in Poland in 1943. He received the PhD in solid-
state physics from Warsaw University of Technology in 1974, after which he joined
the Staff of the Department of Chemistry. He habilitated in thin lms physics in
1981. His present position is the Head of the Sensor Technique Laboratory. His work
encompasses many aspects of thin solid lms, including sensor technique, electronic
noses and application of the articial neural networks.
Stanislaw Osowski was born in Poland in 1948. He received the Ph.D. and Dr.Sc.
degrees in electrical engineering from Warsaw University of Technology in 1975
and 1981, respectively. At present he is a Professor at the Electrical Engineering
Faculty of this University. His main interest is in signal processing, articial neural
networks and their applications.
Wojciech Pawlowski was born in Poland in 1950. He received the Ph.D. degrees in
chemical engineering from Warsaw University of Technology. At present he is an
Assistant Professor (Adiunkt) at the Department of Chemistry of this University. His
main interest is in explosive materials.