FLAVOUR AND FRAGRANCE JOURNAL

Flavour Fra`r[ J[ 1999^ 04] 104Ð111

Detection of perfumes in diesel fuels with semiconductor

and mass-spectrometry based electronic noses
Roger Feldhoff,1 Claude-Alain Saby2 and Philippe Bernadet1
1
Elf-Aquitaine, Groupement de Recherches de Lacq, B.P. 34, 64170 Lacq, France
2
Elf Antar France, Centre de Recherches d’Elf Solaize, B.P. 22, 69360 Saint-Symphorien d’Ozon, France

Received 5 June 0888

Revised 0 February 1999
Accepted 0 February 1999

ABSTRACT] The gas!phase of two diesel fuels scented with perfume mixtures were examined with a FOX 3999
electronic nose "Alpha!M[O[S[\ France# and a Smart Nose GA "LDZ Laboratory\ Switzerland#[ The _rst system
uses chemical gas sensors\ the second a mass spectrometer[
The data of both instruments were evaluated by principal component analysis "PCA# and linear discriminant
analysis "LDA#[ The LDA results obtained allowed the detection of a much lower perfume concentration with
the mass spectrometry data than with the chemical sensor data[ Copyright Þ 1999 John Wiley + Sons\ Ltd[

KEY WORDS] diesel fuel^ gas!phase^ headspace^ volatile compounds^ detection limit^ perfume^ electronic nose^
chemical sensors^ mass spectrometry^ principal component analysis^ discriminant function analysis

Introduction gas phase is normally analysed by gas!chromatography

The aim of this article is to assess the usefulness of
electronic noses as a complementary tool to odour
panels[ Electronic noses can certainly not replace the
human nose because they do not respond to the same
molecules[ On the other hand\ they are much faster\
more repeatable and less expensive than expert panels[
Potential applications of these devices can be product
or quality control in the chemical industry\ in particular
for health damaging products[
The _rst study done in our laboratory describes
the distinction of diesel fuels coming from di}erent
re_neries[0 Chemical sensors and two mass spectrometer
based electronic noses were used and compared[ The
results obtained with both techniques were similar[
Strong correlations between the mass spectral data and
the chemical sensor responses were observed[ The mass
spectrometers showed a better reproducibility and were
much more practical for this qualitative distinction of
diesel fuels[
The goal of this study is to _nd out in which con!
centrations a perfume mixture can be detected in a
complex matrix like a diesel fuel[ The results obtained
with chemical sensors and mass spectrometers shall be
compared[
The liquid phase of oil and oil derivatives are mostly
analysed by supercritical ~uid chromatography\1 mass
spectrometry2 or ~uorescent indicator absorption[3 The
 Correspondence to] R[ Feldho}\ Elf!Aquitaine\ Groupement de Recherches
de Lacq\ B[P[ 23\ 53069 Lacq\ France[
"GC# or gas chromatography coupled with mass
spectrometry "GC!MS#[
Electronic noses could equally be used to measure
changes of the gas phase of chemical products[ The
advantages of electronic noses over classic GC are their
simpler use and higher speed[ The greatest disadvantage
is that chemical compounds can not be analytically
identi_ed[
Electronic noses have been proposed for quality
control of foodstu}4Ð6 or "alcoholic# beverages[7Ð09 They
were also applied to industrial food product control[00
Other papers give a more general overview about
electronic nose technology and applications[01\02 Further
studies\ one of them carried out in our laboratory\
applied an electronic nose to perfumes[03\04 There are
two articles which describe the application of an elec!
tronic nose to fuels[05\06 The _rst one discusses the quali!
tative distinction of several automotive fuels "with
di}erent octane values#[05 The second one concentrates
on forensic and law enforcement applications[06
Experimental Conditions
Since chemical sensors and mass spectrometry are of a
very di}erent nature it was not possible to use the same
working conditions for both machines[ However\ to
compare the analytical potential of these techniques
it seems to be more appropriate to optimise working

Copyright Þ 1999 John Wiley + Sons\ Ltd[

105 R[ FELDHOFF\ C[!A[ SABY AND P[ BERNADET
conditions for both instruments independently[ This is
what was done in this study[
Chemical Sensors
The chemical sensor based instrument used was a FOX
3999 electronic nose "Alpha!M[O[S[\ Toulouse\
France#[ It was equipped with 07 semiconductor
sensors[ The samples were passed by a HS499 auto!
sampler "CTC Analytics AG# with a capacity of 49
samples[ To provide a constant ~ux of dry air through
the electronic nose\ a humidi_er "air condition unit
ACU\ model 0886\ Alpha!M[O[S[# was used[ The air
condition unit was supplied with synthetic air "nitro!
gen:oxygen R79#[ Its air ~ux was set to 299 ml:min\ the
relative humidity was regulated between 16[1) and
18[4)\ the temperature varied between 38[6>C and
49[1>C[ The dry air vector gas was passed via a 0 l bu}er
bottle before entering the electronic nose[ The FOX
3999 instrument was set to 149 ml:min vector gas con!
sumption[ A third exit tube of the bu}er bottle allowed
the super~uous air to escape[ The whole setup was
mounted in an air!controlled laboratory with an ambi!
ent temperature of 10>C[ Careful instrument main!
tenance was necessary to obtain reproducible results
"for more details see reference ð0Ł#[
The samples "09 ml gas vials _lled with 099 ml of diesel
fuel# were passed in arbitrary order[ The vials were
heated to 24>C by the autosampler "incubation time 29
min with agitation#[ The temperature of the injection
syringe was 39>C[ The syringe was _lled twice before
taking 399 ml of the sample headspace and injecting it
into the FOX instrument[ Syringe _ll speed and injec!
tion speed were 099 ml:s and 0499 ml:s\ respectively[
After each injection the syringe was baked out for 3 min
at 49>C[ It was then ~ushed with nitrogen "N 49# for
5 ]29 min[ The delay time between two injections was 0 h
29 min[ This comparatively long interval was necessary
because the return of some of the gas sensors to their
initial values was extremely slow[ The volatile com!
pounds contained in the headspace obviously caused a
long desorption process[ This is probably related to the
viscous nature of diesel fuel with long!chained com!
pounds "09Ð19 carbon atoms#[
The 07 sensors of the FOX electronic nose are listed
in Table 0[ We only used "doped# metal!oxide sensors
Table 1. Metal-oxide sensors of the three chambers (A,
B, C) of the FOX 4000 electronic nose
Position Chamber A Chamber B Chamber C
0 T29:0 P29:0 SY:LG
1 P09:0 P39:1 SY:G
2 P09:1 P29:1 SY:AA
3 P39:0 P69:0 SY:Gh
4 T69:1 T39:0 SY:gCTl
5 PA1 TA1 SY:gCT
Copyright Þ 1999 John Wiley + Sons\ Ltd[
because they have a higher long!term stability and are
less sensitive to humidity ~uctuations than their con!
ducting polymer!based homologues[ The sensor signals
were recorded for 599 s with an acquisition point each
second[
Mass Spectrometer
The second instrument used\ a Smart Nose GA 199\
was based on a mass!spectrometer[ The corresponding
measurements were carried out by LDZ Laboratory\
CH!1963 Marin!Epagnier\ Switzerland[ The system|s
detection unit consisted of a Balzers quadrupole mass
spectrometer with 089 channels "from 09 to 088 amu#[
The samples were 19 drops "about 079 mg# of diesel fuel
_lled in 09 ml vials[ The injection unit was a CTC
Headspace Autosampler PAL[ The samples were incu!
bated at 49>C for 4 min "with agitation#[ The syringe
and injector temperatures were 099>C and 019>C respec!
tively[ After each injection of 1[4 ml of sample head!
space\ the syringe was purged for 6 min and the injector
for 09 min with nitrogen "9[4 bar#[ The acquisition time
per sample was 09 min[ For data examination three
scans per sample were averaged[ Each diesel type was
measured four times[
Samples
Most car drivers _nd the smell of diesel fuel unpleasant[
This circumstance leads many petrol companies to add
perfumes to their products[ The perfumes mask the
odour of heavily smelling volatile compounds[
The samples used were two di}erent diesel fuels] F91
"a winter diesel from the {elf|!re_nery at Feyzin# and
G00 "a summer diesel from the re_nery at Grandpuits#[
These two diesel fuels were scented in di}erent con!
centrations with either an {elf| perfume mixture or with
a complex additive[ The additive is a mixture of a deter!
gent\ an anti!foam\ an anti!corrosion protection and 7
g:099 g of the perfume[ The perfume concentration and
coding of these samples are listed in Tables 1 and 2
Even at the lowest additive concentration used
"sample F91A9979# a signi_cant odour di}erence was
observed to the non!scented sample[ This was con_rmed
by an odour panel consisting of eight persons[ The
scented sample was described as more pleasant by the
panellists[ Odour descriptions corresponding to bad
smells obtained a lower weight[
The odour di}erences between the same two samples
were equally con_rmed by gas!chromatography com!
bined with "human nose# sni.ng "GC!OLF#[ The odour
pro_le obtained by headspace injection showed clear
di}erences "not shown#[ On the other hand\ the pure
GC data "not shown# did not allow for any qualitative
distinction between them[ There might be small di}er!
ences in some peaks which could not be resolved due
Flavour Fra`r[ J[ 1999^ 04] 104Ð111
 DIESEL FUELS SCENTED WITH PERFUME MIXTURES 106

Table 2. F02 Diesel samples with different perfume and additive concentrations
Final Samples scented with the additive Samples scented with the pure perfume
perfume
concentration ðml:lŁ Code Quantity added ðml:lŁ Code Quantity added ðml:lŁ

9 F91 9 F91 9
79 F91A9979 0999 F91P9979 79
059 F91A9059 1999 F91P9059 059
219 F91A9219 3999 F91P9219 219
539 F91A9539 7999 F91P9539 539
0179 F91A0179 05 999 F91P0179 0179
09 999 F91A0) 014 999 F91P0) 09 999

Table 3. G11 diesel samples with different perfume and additive concentrations
Final Samples scented with the additive Samples scented with the pure perfume
perfume
concentration ðml:lŁ Code Quantity added ðml:lŁ Code Quantity added ðml:lŁ
9 G00 9 G00 9
79 G00A9979 0999 G00P9979 79
059 G00A9059 1999 G00P9059 059
219 G00A9219 3999 G00P9219 219
539 G00A9539 7999 G00P9539 539
859 G00A9859 01 999 G00P9859 859
0179 G00A0179 05 999 G00P0179 0179
0819 G00A0819 13 999 G00P0819 0819
1459 G00A1459 21 999 G00P1459 1459

to the low quantitative reproducibility of the manual
injection method used[ The perfume consisted of many
di}erent compounds and its total concentration was
only 79 ppm in this sample[ The GC!peaks were too
small to be detected or they were hidden by the numer!
ous GC!peaks from the diesel itself[
Results and Discussion
Chemical Sensor Results with PCA
For data examination\ we used DRmax:R9\ which is the
maximum change of the sensor|s electrical resistance
divided by the initial resistance[ This value gives the
most stable results with respect to sensor baseline vari!
ations[
A principal component score plot "PCs 0\ 2# for the
measurements done with diesel F91 is shown in Figure
0[ PCs 0 and 2 were chosen for this representation
because PC1 did not contribute much to the separation
of the di}erently perfumed samples[ The importance of
the _rst three principal components are 78[8\ 2[3 and
0[7)\ respectively[ According to the small importance
of PC2 with respect to PC0\ the data!distribution is
nearly one!dimensional[ PC0 expresses the di}erences
in additive concentration whereas PC2 contains infor!
mation about the diesel|s pure perfume content[ Only
three groups can be separated] samples with 0) of the
additive\ samples with 0) of the pure perfume and a
rest group with lower perfume contents[ Within this rest
group\ the samples with the pure perfume seem to form
a separate cloud that touches a second cloud containing
the pure diesel fuel and the diesel with additive[ The
samples A0179 are all found at the right border of the
additive cluster but there is still no distinct separation
from the main cloud at this perfume concentration[
Figure 1 shows the corresponding results for G00[
Again PCs 0 and 2 were used[ The relative weights of
the _rst three principal components are PC0 83[3)\
PC1 1[0) and PC2 0[1)[ Apart from samples A0179\
A0819 and A1459 all other samples form a big cloud[
PC0 and PC2 both increase with additive concentration[
In PC2\ one might equally suspect a slight concentration
in~uence of the perfume "see samples P1459 at the upper
border of the main cloud#[ PC1\ again\ did not contain
much useful information for the distinction of the
di}erent samples[
In Figure 1\ two populations of data points can be
observed] a diagonal line with positive gradient\ starting
from value 9[009 on the x!axis\ can be imagined to split
the data into two groups[ This can best be seen on the
samples with higher additive concentrations[ The reason
for this phenomenon was a spontaneous baseline shift
of the chemical sensors during the experiment[ This
baseline shift probably occurred due to the insu.cient
temperature control of the instrument[
Chemical Sensor Results with LDA
How can the data model be optimized< One method to
improve the separation is linear discriminant analysis

Copyright Þ 1999 John Wiley + Sons\ Ltd[ Flavour Fra`r[ J[ 1999^ 04] 104Ð111
107 R[ FELDHOFF\ C[!A[ SABY AND P[ BERNADET

Figure 1. Principal component score plot for the (perfumed) diesel F02 as obtained with the FOX 4000 instrument (all
sensors used). F02 pure, P F02 with perfume, A F02 with (perfume containing) additive

Figure 2. Principal component score plot for the (perfumed) diesel G11 as obtained with the FOX 4000 instrument (all
sensors used). G11 pure, P G11 with perfume, A G11 with (perfume containing) additive

"LDA#[07\08\19 However\ the stability of LDA models
strongly depends on a careful feature selection[0
To select the most important sensors\ we looked at
the sensors contributing to the PCA models[ These are
shown in Figures 2 and 3 for F91 and G00\ respectively[
Since PC1 did not contribute to the separation of the
di}erent samples\ we concentrated on PCs 0 and 2[ We
assume that PC0 mainly contains information about
the additive and PC2 about the perfume[ PC0 shows
very similar patterns in both _gures\ with strong con!
tributions from B1 and C1!3[ The similarities for PC2
are less distinct[
We then developed a LDA model only built on the
sensors important for PCs 0 and 2[ For this\ we chose
those sensors which in both PCA models have a load
higher than 0[4[ According to this threshold value\ the

Copyright Þ 1999 John Wiley + Sons\ Ltd[ Flavour Fra`r[ J[ 1999^ 04] 104Ð111
 DIESEL FUELS SCENTED WITH PERFUME MIXTURES 108

Figure 3. Loads of the first three principal component vectors for (perfumed) diesel F02 as obtained with the FOX
4000 instrument

Figure 4. Loads of the first three principal component vectors for (perfumed) diesel G11 as obtained with the FOX
4000 instrument

sensors retained from PC0 are A5\ B0\ B1 and C1!C3[
The main contributors to PC2 are sensors A0\ A3!5\
B0!2 and C1\ C2[ The union of these two groups\ thus\
contains sensors A0\ A3!5\ B0!2 and C1!3[ LDA models
based on these sensors were computed for both\ F91
and G00[ In both cases there were software warnings
that the matrix was close to singular[ This shows that
the observed di}erences between samples are quite small
and are close to the instrument|s detection limits[
The corresponding discriminant function score plot
for F91 is shown in Figure 4[ The inner!class variances
are smaller than obtained with PCA[ However\ the sep!
aration of single groups is no better than before[ There
are again two clouds\ one contains only samples with
perfume and the other only samples with additive[ The
pure diesel is found just in the middle between these
two clouds[ DF0 "70[6) of information# describes the
additive content and DF1 "04[9) of information# the

Copyright Þ 1999 John Wiley + Sons\ Ltd[ Flavour Fra`r[ J[ 1999^ 04] 104Ð111
119 R[ FELDHOFF\ C[!A[ SABY AND P[ BERNADET

Figure 5. Linear discriminant score plot of (perfumed) diesel data as obtained with the FOX 4000 instrument (sensors
1, 4–9, 14–16 used). F02 pure, P F02 with perfume, A F02 with (perfume containing) additive

perfume content[ In the case of the samples with additive
there is a tendency towards a concentration dependence
for sample concentrations above 219 ppm[ The lowest
additive concentration "well separated# could be sug!
gested to be about 0179 ppm[ For the pure perfume it
is not possible to de_ne a precise detection limit[ It
should be considerably higher than 1999 ppm but still
below 09 999 ppm "0)#[
Also in the case of G00 "Figure 5#\ the inner!group
variance is much smaller with DFA than with PCA[
The sample separation is much better now[ Not only
the samples with high additive concentrations but also
with high perfume content can now be distinguished
from the weaker perfumed samples[ Starting from a
main cloud containing weaker perfumed samples\ the
additive concentration increases with DF0 "importance

Figure 6. Linear discriminant score plot of (perfumed) diesel data as obtained with the FOX 4000 instrument (sensors
1, 4–9, 14–16 used). G11 pure, P G11 with perfume, A G11 with (perfume containing) additive

Copyright Þ 1999 John Wiley + Sons\ Ltd[ Flavour Fra`r[ J[ 1999^ 04] 104Ð111

41[4)#\ the pure perfume concentration with DF1
"importance 39[1)#[ The lowest concentrations "well
separated# are 0179 ppm in the case of the additive and
between 0179 ppm and 0819 ppm in the case of the
perfume[
It is remarkable that the behaviour of the two diesels
is quite di}erent[ In the case of F91\ the samples with
low perfume and low additive concentrations form two
di}erent clouds[ In the case of G00 there is a "linear#
concentration dependence in both cases[ The detection
limits for the additive are about the same with F91 and
G00 "about 0179 ppm#[ In the case of the pure perfume\
the detection limit is much higher with F91 "signi_cantly
more than 1999 ppm# than with G00 "0179Ð0819 ppm#[
This observation is underlined by the fact that the
importance of DF1 is much bigger in the case of G00
"39[1)# than in the case of F91 "04[9)#[ A reason for
this di}erence in behaviour might be that F91 is a winter
diesel "W# and G00 is a summer diesel "S#[ Another\
maybe more probably reason\ may be the di}erent
chemical composition of the two fuels due to their
di}erent origins[ In an earlier study we found that the
sample origin plays a more important role on the chemi!
cal composition than the fuel type "see reference ð0Ł#[
Signi_cant di}erences in nitrogen content between the
samples from Feyzin "079Ð149 ppm# and Grandpuits
"about 49 ppm# were found[
Normally\ LDA models must be veri_ed "e[g[ by
leave!one!out cross!correlation#[ In this case this was
not done because the computed model "{matrix close to
singular|# did not allow reliable predictions[ Another
reason was that the data base was not su.ciently large
enough[ However\ the obtained LDA maps show
Figure 7. Linear discriminant score plot for (perfumed) diesel data as obtained with the Smart Nose instrument (masses
73, 80, 87, 88, 93, 94, 101, 108, 109, 122, 136 used). F02 pure, P F02 with perfume
Copyright Þ 1999 John Wiley + Sons\ Ltd[
DIESEL FUELS SCENTED WITH PERFUME MIXTURES 110
reasonable results and give an idea about the possi!
bilities and the limits of chemical sensor based electronic
noses[ Because of the closeness of the discussed
measurements to the instruments detection limits we did
not continue to use this kind of electronic noses for
this application[ Another reason was that "spontaneous#
instrument drifts were observed[
Mass Spectrometry Results
The F91 samples were also investigated with a Smart
Nose "mass spectrometer based# electronic nose[ The
whole dataset "09 to 088 amu# was normalized on mass
39[ A PCA was then performed on masses from 55 to
062\ which were the channels with the most important
information "see also reference ð0Ł#[ The result of the
PCA "not shown# was poor[ No sample discrimination
was possible[
Then a feature selection by subsequent elimination
of less important masses was performed[ The retained
masses were 62\ 79\ 76\ 77\ 82\ 83\ 090\ 097\ 098\ 011
and 025[ After range!scaling\ a LDA was performed[
The results are shown in Figure 6[ The sample with 0)
perfume was left out to obtain a more convenient axis
scale[ The distribution is nearly one!dimensional with
relative importances of 86[1) for DF0 and only 1[2)
for DF1[ There is a separation of all of the groups now[
There seem to be two di}erent phenomena] the _rst is
expressed by DF0 and increases linearly with perfume
concentration[ The second is expressed by DF1 and
obtains saturation at a perfume concentration of about
059 ppm[
Presently it is not known how well the long term
Flavour Fra`r[ J[ 1999^ 04] 104Ð111
111 R[ FELDHOFF\ C[!A[ SABY AND P[ BERNADET
Table 4. Comparison of the parameters used and the performance of the two systems with respect to the
identification of perfumed diesel samples
System parameter or property
Detection principle
Injection technology
Sample volume
Incubation temperature
Incubation time
Headspace injection volume
Time delay between two injections
Analytical information used
Measurement repeatability of individual samples
Detection limits found with F91 for perfume:additive
Detection limits found with G00 for perfume:additive
drift of mass spectrometer based electronic noses can
be mastered[ It is\ therefore\ not clear whether both of
these parameters would be stable over a longer time
period[ If one only uses DF0 "86[1)#\ the perfume
detection limit may be ½219 ppm[ The sample with
219 ppm can be distinguished from the pure diesel by
Mahalanobis Distance Analysis[
Conclusion
The measurements carried out show that perfume detec!
tion in diesel fuels is di.cult with both types of elec!
tronic noses] the most important system parameters
used and the observations made are summarized in
Table 3[ The measurement repeatability of the mass
spectrometer is much better than that of the chemical
sensors[ It is also obvious that the mass spectral data
lead to a much lower "pure# perfume detection limit
"½299 ppm# than the chemical sensor data "Ł1999
ppm#[
With sensor selection and LDA it was possible to
make a dependence of the chemical sensor responses
from the perfume concentration visible[ However\ the
measurement repeatability of the sensors was not
su.cient to build a stable and reliable LDA model[
The measurement repeatability of the mass spec!
trometer was much better[ This is the main reason why
the perfume detection limit obtained with mass spec!
trometry was signi_cantly lower than that obtained with
chemical sensor measurements[ After selection of 00
masses\ a LDA model was computed[ Unfortunately\
there were not enough data to do a _nal evaluation of
the stability of this LDA model[
It is important to mention that this technique can only
be used to monitor di}erences between two samples "e[g[
a pure and a perfumed one# but not to give analytical
information about the perfume content of an unknown
sample[
Copyright Þ 1999 John Wiley + Sons\ Ltd[
FOX 3999 Smart Nose
Chemical sensors Mass spectrometer
Syringe injection Syringe injection
9[0 ml 19 drops\ ½9[1 ml
24>C 49>C
29 min 4 min
099 ml 1499 ml
0[4 h 09 min
07 sensor signals Mass spectra "09Ð088 amu#
− ¦
Ł1999 ml:l: ½ 0179 ml:l ½219 ml:l: not tested
0179Ð0819 ml:l:½0179 ml:l not tested
Acknowled`ements * We wish to thank Dr Francžois Hartmann\ Dr
Laurent Germanaud\ Dr Franck Eydoux "Centre de Recherches d|Elf
Solaize# and Prof Dr P[ McLeod "Ecole Pratiques des Hautes Etudes\
Massy# for support and productive discussions[ We further thank Dr
Zesiger "LDZ Laboratory\ Switzerland# for his cooperation[ Thanks
for their kind help and professional work are equally due to the
members of the odour panel of the Groupement de Recherches de
Lacq[
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Flavour Fra`r[ J[ 1999^ 04] 104Ð111