Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine
The sensitivity of sensor assembly based on piezoquartz resonators (PQR) with the chemical coatings of the specified type relatively to the saturated vapours of several lowest alcohols is investigated. As the chemical coatings, some complex compounds of d-transition metals with stearate anion (St⁻)...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2006
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| Цитувати: | Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine / A.P. Filippov, P.E. Strizhak, D.I. Denisyuk, T.G. Serebry, T.S. Ivaschenko // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2006. — Т. 9, № 2. — С. 87-91. — Бібліогр.: 7 назв. — англ. |
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irk-123456789-1214392017-06-15T03:04:53Z Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine Filippov, A.P. Strizhak, P.E. Denisyuk, D.I. Serebry, T.G. Ivaschenko, T.S. The sensitivity of sensor assembly based on piezoquartz resonators (PQR) with the chemical coatings of the specified type relatively to the saturated vapours of several lowest alcohols is investigated. As the chemical coatings, some complex compounds of d-transition metals with stearate anion (St⁻) and octadecylamine (ODA) of the general formula M(ODA)NSt₂ were used, where M²⁺ are ions of d-transition metals Cu(II), Co(II), Ni(II), and N was equal 0, 2, 4, and 6. The sensor images for each of all alcohols investigated by us has the unique character that can be used for discrimination between individual alcohols by using the set of coatings of PQR sensors applied in this work. 2006 Article Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine / A.P. Filippov, P.E. Strizhak, D.I. Denisyuk, T.G. Serebry, T.S. Ivaschenko // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2006. — Т. 9, № 2. — С. 87-91. — Бібліогр.: 7 назв. — англ. 1560-8034 PACS 07.07.Df http://dspace.nbuv.gov.ua/handle/123456789/121439 en Semiconductor Physics Quantum Electronics & Optoelectronics Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
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| description |
The sensitivity of sensor assembly based on piezoquartz resonators (PQR) with the chemical coatings of the specified type relatively to the saturated vapours of several lowest alcohols is investigated. As the chemical coatings, some complex compounds of d-transition metals with stearate anion (St⁻) and octadecylamine (ODA) of the general formula M(ODA)NSt₂ were used, where M²⁺ are ions of d-transition metals Cu(II), Co(II), Ni(II), and N was equal 0, 2, 4, and 6. The sensor images for each of all alcohols investigated by us has the unique character that can be used for discrimination between individual alcohols by using the set of coatings of PQR sensors applied in this work. |
| format |
Article |
| author |
Filippov, A.P. Strizhak, P.E. Denisyuk, D.I. Serebry, T.G. Ivaschenko, T.S. |
| spellingShingle |
Filippov, A.P. Strizhak, P.E. Denisyuk, D.I. Serebry, T.G. Ivaschenko, T.S. Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine Semiconductor Physics Quantum Electronics & Optoelectronics |
| author_facet |
Filippov, A.P. Strizhak, P.E. Denisyuk, D.I. Serebry, T.G. Ivaschenko, T.S. |
| author_sort |
Filippov, A.P. |
| title |
Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine |
| title_short |
Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine |
| title_full |
Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine |
| title_fullStr |
Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine |
| title_full_unstemmed |
Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine |
| title_sort |
discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine |
| publisher |
Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| publishDate |
2006 |
| url |
http://dspace.nbuv.gov.ua/handle/123456789/121439 |
| citation_txt |
Discrimination of the saturated vapours of alcohols by the responses of assembly of piezoquartz sensors covered with metal stearates and their complexes with octadecylamine / A.P. Filippov, P.E. Strizhak, D.I. Denisyuk, T.G. Serebry, T.S. Ivaschenko // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2006. — Т. 9, № 2. — С. 87-91. — Бібліогр.: 7 назв. — англ. |
| series |
Semiconductor Physics Quantum Electronics & Optoelectronics |
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2025-07-08T19:54:08Z |
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2025-07-08T19:54:08Z |
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| fulltext |
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2006. V. 9, N 2. P. 87-91.
© 2006, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
87
PACS 07.07.Df
Discrimination of the saturated vapours of alcohols by the responses
of assembly of piezoquartz sensors covered with metal stearates
and their complexes with octadecylamine
A.P. Filippov, P.E. Strizhak, D.I. Denisyuk, T.G. Serebry, T.S. Ivaschenko
L.V. Pysarzhevsky Institute of Physical Chemistry, NAS of Ukraine
31, prospect Nauky, 03028 Kyiv, Ukraine
E-mail: pstrizhak@hotmail.com
Abstract. The sensitivity of sensor assembly based on piezoquartz resonators (PQR)
with the chemical coatings of the specified type relatively to the saturated vapours of
several lowest alcohols is investigated. As the chemical coatings, some complex
compounds of d-transition metals with stearate anion (St-) and octadecylamine (ODA) of
the general formula M(ODA)NSt2 were used, where M2+ are ions of d-transition metals
Cu(II), Co(II), Ni(II), and N was equal 0, 2, 4, and 6. The sensor images for each of all
alcohols investigated by us has the unique character that can be used for discrimination
between individual alcohols by using the set of coatings of PQR sensors applied in this
work.
Keywords: piezoquartz sensor, alcohols, d-transition metal complex.
Manuscript received 01.03.06; accepted for publication 29.03.06.
1. Introduction
Expansion of assortment of alcoholic drinks in the
consumer market especially last years is accompanied by
the growth of release under the guise of known
commodity marks of obvious fakes or production of
obviously poor quality. The wide circulation was
obtained with shadow business on manufacturing strong
alcoholic drinks from the poor-quality and non-
certificated raw material, cases of poisonings with drinks
of this kind are frequent. Organoleptic parameters at
assortment identification of drinks possess a low degree
of reliability more often, and they usually become
covering for falsification. Therefore, the need for
development of objective express trains – techniques of
quality assurance of specified production with the help
of display chemical reactions as well as physical and
chemical methods of the analysis grows continuously.
Among the perspective principles of such control there
can become the identification of a product smell using
the multisensor devices, for example, assembly from
several piezoquartz resonators (PQR) with sensitive
chemical coatings, the so-called “electronic nose” (EN).
For the development of such devices with a reference to
the above mentioned problem, a necessary stage is
research of sensitivity and selectivity of multisensor
assembly in relation to different components of a
controllable product. Among them, there can be both
substances inherent to it (i.e., describing its assortment
an accessory) and unusual (i.e., characteristic
falsifications for means).
The most full and authentic analysis of quality and
authenticity of various grades of vodka or cognacs could
be provided by known methods of gas and liquid
chromatography as well as other tool methods of the
chemical analysis with use of computer systems and
databases. However, such analysis demands the
expensive equipment, presence of the highly skilled
attendants and can be carried out only in stationary
laboratories. It limits an opportunity of wide application
of these means for mass quality assurance of specified
production on manufacturing and in trade enterprises.
For such purposes the most suitable can be the portable
analyzer of smells such as EN in which the assembly of
sensors based on PQR with the sensitive chemical
coatings put on them is used. Development of such
devices is impossible without creation of the sensitive
chemical coatings possessing even partial selectivity in
relation to various alcohols.
A number of attempts to create such devices are
described in the literature with use of gas
chromatographic stationary phases, polymers, propolis
and other substances of the various nature as sensitive
coatings [1-3].
So, in the work [3] by development of approaches
to create EN for testing cognac and coffee aroma as
chemical coatings for PQR sensors sensitive to alcohols,
the following adsorbents have been recommended: PEG-
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2006. V. 9, N 2. P. 87-91.
© 2006, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
88
2000, dinonylphtalate, methysilicon oil, Triton X-100,
polyethylene glycole adipinate and polystyrene. Among
them, the first three adsorbents represent viscous liquids
that results in attenuation of a volume acoustic wave
both with increase in thickness of the adsorbent film and
with the weights of alcohol adsorbed by this film. It
results in the fact that these sensors with such coatings
give a nonlinear dependence of PQR frequency leaving
(Δf) on the analyte vapour concentration. Moreover, this
dependence passes through the peak when achieving the
certain degree of saturation of a sorbent film with
analyte what demands special receptions for application
of such sensors, for example, record "chrono-frequency-
gram" that is registration of changes Δf with time [3].
In our opinion, assembly of the sensors, capable to
distinguish organic substances of different chemical
nature, and, especially, substances of the same class
(alcohols) in presence of water vapours, it is expedient to
create with use of the solid chemical coatings having,
basically, the hydrophobic nature. Such coatings in the
sensor assembly should differ among themselves not
only in relation to various polarity of molecules of
different alcohols, but also in relation to a structure of
the hydrocarbonic radical in the molecule of the given
alcohol.
Discrimination ability of a sorbent concerning a
structure of a hydrocarbonic radical can be appreciably
caused by the shape of hydrophobic cavities in the
structure of the sorbent film in which the given
hydrocarbonic radical can be inserted more or less
complementarily in relation to points of the cavity,
capable to carry out weak cooperative interactions with
the adsorbate molecule.
It is known that the structure of hydrophobic micro-
pores can be generated by long chain hydrocarbonic tails
of surface-active substances (SAS) organized in
Lengmuir-Blodgett (LB) films on a surface of any solid
substrate [4], or included into a matrix of mesoporous
silica [5]. Pure SAS themselves at usual temperature are
liquid substances or have low temperature of fusion.
SAS molecules fixed on a surface of a solid substrate as
LB film form a rigid enough microporous structure
which can be used with success for creation of sensitive
chemical coatings on metallic electrodes of PQR with
the mentioned above properties [4]. However, the
techniques of LB films drawing demands use of the
complex equipment and is labour-consuming. LB film
consisting of one or several monolayers though possess
exclusive speed and convertibility of the response, but
because of very small thickness of a layer have no big
sorbtion capacity and do not give sufficient sensitivity.
Preparation of multilayered LB films with the purpose to
increase of their sensitivity demands is a work of time.
Besides, when that much increasing in quantity of
monolayers, the degree of orderliness of LB films
gradually decreases, and the condition of SAS molecules
in them comes close to that is observed in usual bulk
solid or liquid phases of corresponding SAS at the given
temperature.
As is known, salts of metals with ionogenic SAS
have much higher temperatures of fusion than an initial
SAS. Thus they are well dissolved in organic solvents,
and can be deposited on PQR electrodes by a way of
simple application or by pulverization of solutions of
corresponding SAS and subsequent drying the obtained
coating. As was shown from our researches with the help
of a method of the X-ray phase analysis (XRРА), the
obtained by these means solid films possess the ordered
periodic structure irrespective of their thickness.
Recently we have developed methods of synthesis of
some salts and complex compounds of d-transition
metals with stearate anion (St-) and octadecylamine
(ODA) of general formula M(ODA)NSt2, where M2+ are
the ions of d-transition metals Cu(II), Co(II), Ni(II) and
others, and N can vary from 0 up to 6 [6]. These
compounds were investigated as chemical coatings for
PQR sensors sensitive to vapours of hydrocarbons and
other volatile organic substances.
In this work, studied was the sensitivity of PQR
sensors with the chemical coatings of the specified type
relative to the saturated vapours of some of the lowest
alcohols. Due to the hydrophobic nature of these coatings,
in our opinion, less others are subject to interfering
influence of water vapours and can serve as the good
sensitive coatings reacting to vapours of volatile organic
substances on the basis of water vapours.
2. Experimental
In present work the following alcohols were investigated
as analytes: methanol, ethanol, propanol, iso-propanol,
butanol-1, butanol-2, iso-butanol and iso-pentanol. All
the analytes had qualification “chemical pure” or “pure
for a chromatography” and were used without additional
refining.
For manufacturing the sensors the piezoquartz
resonators manufactured by enterprise “UKRPIEZO”
(Cherkassy, Ukraine) were used. They were made of
АТ-cut quartz plates and had nickel-silver electrodes and
initial frequency of 10 MHz.
The following compounds were used as covering
materials for PQR sensors: CuSt2 (1), Cu(ODA)2St2 (2),
Cu(ODA)4St2 (3), Cu(ODA)6St2 (4), Ni(ODA)6St2 (5),
Co(ODA)6St2 (6).
Conditions of synthesis of the compounds and their
deposition on PQR electrodes were described earlier [7].
The mass of the coating corresponding to the change of
frequency of every PQR was (−Δfcoat) = (7.0 ± 0.5) кHz.
In the work, there used was the experimental setup
described earlier [6]. It was consisted of a power unit of
a direct current, the generator, a frequency meter, a
personal computer, and also the tight glass chamber with
thermostating water jacket and a neck with polished
glass joint where the glass plug fitting was inserted. On
the internal end of the plug the contacts for PQR were
tightly inserted, and on its external part the portable
generator was fixed.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2006. V. 9, N 2. P. 87-91.
© 2006, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
89
Table 1. Physical and chemical characteristics of the studied alcohols.
Alcohol Mol. mass,
Dalton
tboil
(760 mm Hg), °C
Рsat (25 °С),
hPa
Сsat (25 °С), mg/l ΔH evap, kJ/mol
methanol 32.04 64.7 168.3178 217.60 38.49
ethanol 46.07 78.4 78.4233 145.78 43.27
propanol 60.10 97.3 27.1416 65.82 45.31
iso-propanol 60.10 82.2 59.9426 145.36 44.23
butanol-1 74.12 117.8 8.1557 24.39 46.39
butanol-2 74.12 99.6 24.1558 72.24 50.23
iso-butanol 74.12 107.9 13.7751 41.20 45.67
iso-pentanol 88.15 131.3 4.04598 14.39 58.19
Table 2. The values of responses of PQR sensors obtained in atmosphere of saturated vapours of the corresponding
alcohols at (25 ± 0.5) ºС. Covering materials for the PQR sensors: 1 – CuSt2, 2 – Cu(ODA)2St2, 3 – Cu(ODA)4St2, 4 –
Cu(ODA)6St2, 5 – Ni(ODA)6St2, 6 – Co(ODA)6St2.
Number of coating / Value of the response (–Δfan, Hz) Alcohol
1 2 3 4 5 6
methanol 495 409 976 713 659 629
ethanol 1467 523 2099 953 1066 1855
propanol 1884 969 2781 1285 1864 2797
iso-propanol 1807 868 1965 1371 1459 2737
butanol-1 2686 1221 2733 1568 2456 2789
butanol-2 1780 1087 1904 1376 2169 1933
iso-butanol 2319 1170 2807 1413 2119 2757
iso-pentanol 2744 1607 2851 2000 2873 3775
The sensor response was measured as a frequency
change of PQR with the corresponding coating, when it
was introduced in the chamber with an atmosphere of air
saturated with vapours of corresponding alcohol at
(25±0.5) °C, liquid phase of which was present at the
bottom of the chamber. The PQR frequency was
preliminary measured in an atmosphere of pure air at the
same temperature and relative humidity. The value of
the response, i.e., decreasing the PQR frequency in an
atmosphere saturated with an analyte vapour (–Δfan) in
comparison with its frequency in an atmosphere of pure
air, was measured after an establishment of equilibrium
(a constancy of frequency) that was reached no more
than in 3-4 minutes after mounting PQR into the
chamber. After extraction of the PQR from the chamber,
its frequency in the atmosphere of pure air completely
came back to the initial value approximately for the
same period of time. For every analyte, it was executed 3
measurements of responses on PQR sensor with the
same coating. Results of these measurements differed
among themselves no more than by 10 % were averaged
and further used for construction of vector diagrams
characteristic for every analyte.
3. Results and discussion
In Table 1, some physical and chemical characteristics
of the investigated alcohols are presented: molecular
weight, temperature of boiling at normal atmospheric
pressure, partial pressure and concentration of saturated
vapour of corresponding alcohol at 25 °С, and also
molar enthalpy of evaporation.
Table 2 gives the values of responses (–Δfan, Hz)
obtained for PQR sensors with the mentioned above
coatings in the atmosphere of saturated vapours of the
corresponding alcohols at (25 ± 0.5) ºС.
In the figure, the vector diagrams of the response
group of the 6 PQR sensors for saturated vapours for
each of the investigated alcohols are represented. These
diagrams are the figures drawn connecting the direct
lines of the ends of these six vectors, coordinates start
with the general beginning and are directed at identical
corners from each other. Number of a vector
corresponds to the mentioned above number of the
coating, and the length of a vector corresponds to a
value of the corresponding PQR sensor response (−Δfan
in Hz), obtained in saturated vapours of the given
analyte. Each of these figures has the characteristic
type and corresponds to a sensor (frequency) image for
given analyte on given set of PQR sensors.
It is clearly seen in the figure, that the sensor
images (i.e., the picture of relative lengths of response
vectors) for each of all alcohols investigated by us has
the unique character that can be used, at least, for
identification of individual alcohols by using the set of
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2006. V. 9, N 2. P. 87-91.
© 2006, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
90
0
1000
2000
3000
1
2
3
4
5
6
0
1000
2000
3000
1
2
3
4
5
6
a. Methanol b. Ethanol
0
1000
2000
3000
1
2
3
4
5
6
0
1000
2000
3000
1
2
3
4
5
6
c. Propanol d. Iso-propanol
0
1000
2000
3000
1
2
3
4
5
6
0
1000
2000
3000
1
2
3
4
5
6
e. Butanol-1 f. Butanol-2
0
1000
2000
3000
1
2
3
4
5
6
0
1000
2000
3000
1
2
3
4
5
6
g. Iso-butanol h. Iso-pentanol
Fig. 1. Sensor images of the saturated vapours of the lowest alcohols at T = (25 ± 0.5) ºC. Covering materials for PQR sensors:
1 − CuSt2, 2 − Cu(ODA)2St2, 3 − Cu(ODA)4St2, 4 − Cu(ODA)6St2, 5 − Ni(ODA)6St2, 6 − Co(ODA)6St2.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2006. V. 9, N 2. P. 87-91.
© 2006, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
91
coatings of PQR sensors applied in this work. It is
interesting to note that besides the distinctions between
alcohols on relative values of responses on different
PQR, between various alcohols, in general, it is also
observed the distinction on average absolute size of
responses of all the PQR sensors. If to compare data of
Table 1 to those of Table 2, in some cases it is possible
even to notice the tendency of increase in average
absolute size of responses of all the PQR sensors on
transition from alcohol with higher partial pressure of
saturated vapour (for example, methanol) to that with the
smaller value Рsat (iso-amyl alcohol) at the same
temperature. That is, at the same temperature all the
investigated coatings give, on the average, the greater
response in a case of saturated vapours of less volatile
iso-amyl alcohol (tboil = 131.3 °С) than in the case of
more volatile methanol (tboil = 64.7 °С). To be truth, by
comparison of sensor images of iso-propanol (tboil =
82.2 °С) and butanol-2 (tboil = 99.6 °С) such tendency is
not observed. It is obvious that, in absence of sharp
selectivity at the same concentration of analytes in a gas
phase, the sorption of more volatile analyte by a sensor
coating, in general, should be less than that of less
volatile analyte. On the other hand, the concentration of
saturated vapours at the same temperature for the former
analyte is always higher than for the latter. Thus, when
comparing the results of sorption for saturated vapours
of different analytes at the same temperature, it is
necessary to take into account two abovementioned
factors that possess opposite action, but generally do not
compensate each other. The parity of these factors can
change with temperature what it is necessary to be taken
into account when drawing up the database suitable for
use of the multisensor assembly both in identification of
vapours of individual analytes and the analysis of their
mixtures (i.e., complex smells).
Acknowledgements
The work is partially supported by the scientific program
of the National Academy of Sciences of Ukraine “Sensor
systems and technologies” (grant 2C).
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