Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography
Influence of modifying pentasyl group synthetic zeolites (Silicalite-1 and Silicalite-2) with metal cations capable to specific interactions on the separation ability of the chromatographic column has been studied.
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Інститут хімії поверхні ім. О.О. Чуйка НАН України
2010
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nasplib_isofts_kiev_ua-123456789-289952025-02-09T14:58:35Z Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography Поєднання молекулярно-ситових і комплексоутворюючих властивостей насадок в газовій хроматографії Сочетание молекулярно-ситовых и комплексообразующих свойств насадок в газовой хроматографии Eprikashvili, L. Pirtskhalava, N. Andronikashvili, T. Kordzakhia, T. Zautashvili, M. Dzagania, M. Функціоналізовані матеріали, одержані золь-гель і темплатним методами Influence of modifying pentasyl group synthetic zeolites (Silicalite-1 and Silicalite-2) with metal cations capable to specific interactions on the separation ability of the chromatographic column has been studied. Вивчено вплив модифікування синтетичних цеолітів сімейства пентасілів (Сілікаліту-1 і Сілікаліту-2) катіонами металів, здатних до специфічних взаємодій, на розділювальну здатність хроматографічної колонки. Изучено влияние модифицирования синтетических цеолитов семейства пентасилов (Силикалита-1 и Силикалита-2) катионами металлов, способными к специфическим взаимодействиям, на разделительную способность хроматографической колонки. 2010 Article Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography / L. Eprikashvili, N. Pirtskhalava, T. Andronikashvili, T. Kordzakhia, M. Zautashvili, M. Dzagania // Хімія, фізика та технологія поверхні. — 2010. — Т. 1, № 3. — С. 292-295. — Бібліогр.: 15 назв. — англ. 2079-1704 https://nasplib.isofts.kiev.ua/handle/123456789/28995 543.544 en Хімія, фізика та технологія поверхні application/pdf Інститут хімії поверхні ім. О.О. Чуйка НАН України |
| institution |
Digital Library of Periodicals of National Academy of Sciences of Ukraine |
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DSpace DC |
| language |
English |
| topic |
Функціоналізовані матеріали, одержані золь-гель і темплатним методами Функціоналізовані матеріали, одержані золь-гель і темплатним методами |
| spellingShingle |
Функціоналізовані матеріали, одержані золь-гель і темплатним методами Функціоналізовані матеріали, одержані золь-гель і темплатним методами Eprikashvili, L. Pirtskhalava, N. Andronikashvili, T. Kordzakhia, T. Zautashvili, M. Dzagania, M. Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography Хімія, фізика та технологія поверхні |
| description |
Influence of modifying pentasyl group synthetic zeolites (Silicalite-1 and Silicalite-2) with metal cations capable to specific interactions on the separation ability of the chromatographic column has been studied. |
| format |
Article |
| author |
Eprikashvili, L. Pirtskhalava, N. Andronikashvili, T. Kordzakhia, T. Zautashvili, M. Dzagania, M. |
| author_facet |
Eprikashvili, L. Pirtskhalava, N. Andronikashvili, T. Kordzakhia, T. Zautashvili, M. Dzagania, M. |
| author_sort |
Eprikashvili, L. |
| title |
Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography |
| title_short |
Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography |
| title_full |
Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography |
| title_fullStr |
Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography |
| title_full_unstemmed |
Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography |
| title_sort |
combining molecular sieve and complexing properties of the column packing in gas chromatography |
| publisher |
Інститут хімії поверхні ім. О.О. Чуйка НАН України |
| publishDate |
2010 |
| topic_facet |
Функціоналізовані матеріали, одержані золь-гель і темплатним методами |
| url |
https://nasplib.isofts.kiev.ua/handle/123456789/28995 |
| citation_txt |
Combining Molecular Sieve and Complexing Properties of the Column Packing in Gas Chromatography / L. Eprikashvili, N. Pirtskhalava, T. Andronikashvili, T. Kordzakhia, M. Zautashvili, M. Dzagania // Хімія, фізика та технологія поверхні. — 2010. — Т. 1, № 3. — С. 292-295. — Бібліогр.: 15 назв. — англ. |
| series |
Хімія, фізика та технологія поверхні |
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Хімія, фізика та технологія поверхні. 2010. Т. 1. № 3. С. 292–295
_____________________________________________________________________________________________
292 ХФТП 2010. Т. 1. № 3
UDC 543.544
COMBINING MOLECULAR SIEVE AND COMPLEXING
PROPERTIES OF THE COLUMN PACKING
IN GAS CHROMATOGRAPHY
L. Eprikashvili, N. Pirtskhalava, T. Andronikashvili, T. Kordzakhia,
M. Zautashvili, M. Dzagania
Melikishvili Institute of Physical and Organic Chemistry of Georgia
5 Jikia Street, Tbilisi 0186, Georgia, physorgchem@pochta.ru
Influence of modifying pentasyl group synthetic zeolites (Silicalite-1 and Silicalite-2) with metal cations
capable to specific interactions on the separation ability of the chromatographic column has been studied.
INTRODUCTION
Zeolites belong to the selective sorbents which
strongly adsorb some compounds (normal chained
hydrocarbons) but do not adsorb others (aromatic,
cyclic) depending on the configuration of the ad-
sorbate molecule. The selectivity of zeolites is due
to their molecular sieve properties [1]. The use of
zeolites in gas chromatography ensures the separa-
tion of a complex mixture of oil origin [2].
Mixtures of meta-, ortho- and para-isomers
of different hydrocarbons are difficult to separate.
For their separation, such sorbents as Benton-34
and liquid crystal phases are known to be used [3, 4].
The selectivity of adsorbents is probably due
to their structural properties. Zeolite Silikalite also
exhibits increased selectivity to para-isomers. Be-
cause of its molecular sieve properties, it can retain
linear molecules of para-isomers and does not ad-
sorb ortho- and meta-isomers [5–8].
In this paper, we present the results of studying a
selective adsorbent that combines molecular sieve
properties with complexation properties, namely, a
zeolite (Silicalite) modified with metal cations capable
of forming complexes with benzene hydrocarbons.
EXPERIMENTAL
Two samples of Silicalite: Silicalite-1 (analog
of ZSM-5) and Silicalite-2 (analog of ZSM-11)
from the pentasyl group have been investigated
[9]. These zeolites are characterized by an ideal
unit cell of the following composition:
Nan(Al nSi96-nO192)~16H2O n~3 [10].
The adsorbents studied are high-silica zeo-
lites. In contrast to conventional zeolites, they
exhibit hydrophobic properties.
The structures of both zeolites are almost identi-
cal: ten-membered rings form two systems of inter-
secting channels lying in perpendicular planes. The
main difference between them is as follows: in Sili-
calite-1, the two channel systems bearing oxygen
rings of the size 0.51–0.56 nm are of both round –
shape and ellipsoid configuration whereas all rings in
Silikalite-2 possess ellipsoid configurations of the
size 0.54x0.56 nm [10]. Barrer in [10] believed that
even such a small difference in zeolite structures
could strongly affect their adsorption properties.
In our experiments, powders of Silikalite-1 and
Silikalite-2 (the Silikalite sample was synthesized at the
Center for porous Materials of Manchester and kindly
provided by Dr. R.J. Paisted) were modified with cad-
mium, thallium, and silver cations by ion exchange [11].
These cations can form unstable complexes
with some benzene compounds. In the course of
modification, the initial sodium forms of Silikalites
were treated three times with a 0.1 M solution of
corresponding metal nitrates. After each treatment,
the powder was washed with distilled water to re-
move excess sodium cations and then dried at
150°C for four to six hours. In the chromatography
column, zeolite was used in the surface-layer ver-
sion [12] that is a powder of dispersity of 25–60 µm
applied onto a solid support, celite-545, grains
60–80 mesh using the procedure proposed by Bom-
bauch [13]. The zeolite and solid support (1:2) were
mixed in a rotating porcelain cylinder. In the result-
ing adsorbent, the fraction of zeolite was ~27–29%
relative to the mass of the solid support.
The experiments were conducted on LKhM-
8MD Model 3 chromatograph using a column of
0.5 m in length and 3 mm in inside diameter. The
adsorbent packed in the column was thermally
activated by heating the column to 250°C in a
Combining Molecular Sieve and Complexing Properties of the Column Packing
_____________________________________________________________________________________________
ХФТП 2010. Т. 1. № 3 293
flow of a carrier gas (nitrogen) for 4–6 h. Column
temperature in the experiments was maintained at
230°C under isothermal conditions. The flow rate
of the carrier gas (nitrogen) was of 50 mL/min. A
flame ionization detector was used.
Model test mixtures consisted of the following
isomers: (1) meta-, ortho-, and para-xylenes; (2)
meta-, ortho-, and para-chlorotoluenes; (3) meta-,
ortho-, and para-dichlorobenzenes; (4) para-xylene,
para-chlortoluene, and para-dichlorobenzene. We
determined parameters characterizing the process
of chromatographic separation [14].
RESULTS AND DISCUSSION
Table 1 presents relative retention times of all the
studied compounds and corresponding asymmetry
coefficients of chromatographic peaks on both the
initials (sodium) forms of Silikalites and cation-
exchanger forms. As can be seen in Table 1, selectiv-
ity to para-isomers for all the studied compounds
was much higher them that to ortho- and meta-
isomers of the same triad. The retention times of
these isomers were almost equal. In going to cation-
exchanger forms, the retention times of ortho-, meta-,
and para-isomers increased in the order
Na<Cd<Tl<Ag, depending on the nature of the
cation incorporated into the Silikalite. The increase
was more pronounced for para-isomers and less pro-
nounced for ortho- and meta-isomers. This effect was
enhanced as the molecular mass of compounds was
increased. The asymmetry coefficients for ortho- and
meta-isomers insignificantly changed depending on
the isomery and the type of the cation-modified form;
a noticeable increase was observed for para-isomers.
According to the tabular data, relative reten-
tion times of the components on Silicalite-2 are
higher as compared to those on Silicalite-1 on
average by 170% and they are higher on both on
the initial (sodium) and cation (Cd+2, Tl+, and
Ag+) modified forms; as for the asymmetry coef-
ficients, they are higher, i.e. Кас→1.
By comparing retention times, we calculated
the increase in selectivity of the retention of para-
isomers compared to ortho-isomers cation-exchanger
forms of Silikalites (Table 2).The data in Table 2
indicate that, for all isomers, selectivity increases in
the order Cd<Tl<Ag depending on the cation nature
in comparison with initial (sodium) forms.
As was shown in our earlier paper [15], the in-
troduction of Cd and Ag cations into type X zeo-
lites significantly increased the retention volumes
for unsaturated hydrocarbons in comparison to
those for saturated ones. This effect was more pro-
nounced for silver- than for cadmium-containing
zeolite and be explained by the formation of two
complexes differing in stability. Thus, the interac-
tion of AgX with ethylene proceeds as overlapping
of two orbitals, the occupied π orbital of ethylene
with the vacant 5sp orbital of the silver ion and the
occupied 4d orbital of silver with the vacant π*
orbital of ethylene. In the case of CdX, interaction
proceeds as overlapping of only π and 5sp orbitals.
It is likely that, for the studied isomeric benzene
derivatives, π bonds the benzene rings of isomers
also interact with corresponding orbitals of Cd, Tl,
and Ag cations to form complexes differing in stabil-
ity (it increases in the above order) which results in
an increase in the retention volumes of all isomers.
A significant increase in the selectivity of the
adsorbent to para-isomers is due to the molecular
sieve properties of the zeolite which more
strongly adsorbs these isomers because of their
configuration. As a result, the rate of molecular
diffusion, which is also determined by the nature
of the radical at the benzene ring, decreases.
The data in Table 2 also indicate that the se-
lectivities of thallium- and silver-containing
Silikalits to para-isomers are very high and al-
most equal. This can be explained by the fact that
the physical and chemical properties of Tl + and
Ag + cations are similar [12].
Thus, we can conclude that the selectivity of
cation-modified Silikalites to para-isomers is deter-
mined by two factors: (1) the effect of molecular sieves
and (2) the ability of analytes to form complexes with
cadmium, thallium, and silver cations whereas only
the complexation effect is responsible for the adsorb-
ent selectivity to ortho- and para-isomers.
As follows from aforesaid, cation-modified
Silikalites, in particular, those containing thallium
and silver ions can be attributed to adsorbents
selective to para-isomers.
The values of the criterion of uniformity of
separation ∆ [14] of a model ternary mixture of
para-isomers on the studied adsorbents are pre-
sented in Table 3.
It can be seen that the sharpness of the sepa-
ration of the model mixture increases in the above
order depending on the cation nature. Both in-
crease in the retention times of the individual
components and more symmetrical peaks (Ta-
ble 1) on Silicalite-2 compared to those on Sili-
calite-1 define higher values of the criterion of
uniformity on Silicalite-2 (Table 3).
L. Eprikashvili, N. Pirtskhalava, T. Andronikashvili et al.
_____________________________________________________________________________________________
294 ХФТП 2010. Т. 1. № 3
Table 1. Relative retention times (t /
R) of some benzene derivatives and asymmetry coefficients of chromatographic
peaks (Kas) of corresponding compounds [14] (column temperature 230°C)
Adsorbent
initial (so-
dium) form
of Silikalite-1
applied onto
celite-545
initial (so-
dium) form
of Silikalite-2
applied onto
celite-545
cadmium
form of
Silikalite-1
applied onto
celite-545
cadmium
form of
Silikalite-2
applied onto
celite-545
thallium
form of
Silikalite-1
applied onto
celite-545
thallium
form of
Silikalite-2
applied onto
celite-545
silver
form of
Silikalite-1
applied onto
celite-545
silver
form of
Silikalite-2
applied onto
celite-545
Compound
t/
R Kas t/
R Kas t/
R Kas t/
R Kas t/
R Kas t/
R Kas t/
R Kas t/
R Kas
benzene 1.00 0.77 1.00 0.82 1.00 0.72 1.00 0.80 1.00 0.67 1.00 0.78 1.00 0.64 1.00 0.76
o-xylene 0.37 0.77 1.12 0.80 0.34 0.75 1.15 0.77 0.23 0.73 1.17 0.75 0.24 0.70 1.22 0.73
m-xylene 0.43 0.75 1.17 0.78 0.39 0.70 1.25 0.75 0.25 0.67 1.27 0.73 0.27 0.65 1.29 0.70
p-xylene 0.89 0.70 2.23 0.75 1.14 0.67 2.70 0.73 0.89 0.65 2.87 0.70 0.89 0.63 2.89 0.67
o-
chlorotoluene
0.43 0.75 1.28 0.77 0.39 0.73 1.30 0.75 0.29 0.70 1.39 0.73 0.30 0.67 1.41 0.70
m-
chlorotoluene
0.49 0.73 1.39 0.75 0.41 0.70 1.41 0.73 0.35 0.67 1.52 0.70 0.34 0.64 1.56 0.67
p-
chlorotoluene
1.31 0.67 2.89 0.73 1.48 0.65 3.45 0.70 1.72 0.64 5.83 0.67 1.72 0.60 5.89 0.65
o-
dichlorobenzene
0.54 0.70 1.56 0.74 0.64 0.67 1.58 0.70 0.40 0.63 1.65 0.67 0.43 0.61 1.78 0.65
m-
dichlorobenzene
0.49 0.67 1.50 0.70 0.59 0.65 1.58 0.67 0.37 0.60 1.61 0.65 0.38 0.57 1.71 0.63
p-
dichlorobenzene
1.94 0.65 4.06 0.68 1.70 0.63 4.75 0.65 2.63 0.57 8.87 0.63 2.55 0.55 8.96 0.60
Table 2. Increase in selectivity of the sorbent (%) p-isomers on the o-isomers of the corresponding triads in all the
modified samples of the sorbent
Compounds
Silikalite-1
+ Cd2+ -
Celite-545
Silikalite-2
+ Cd2+ -
Celite-545
Silikalite-1
+ Tl+ -
Celite-545
Silikalite-2
+ Tl+ -
Celite-545
Silikalite-1
+ Ag+-
Celite-545
Silikalite-2
+ Ag+-
Celite-545
p-xylene/
o-xylene
5.5 35 34.9 59 38.4 72
p-chlorotoluene/
o-chlorotoluene 29.3 39 37.4 194 38.8 236
p-dichlorobenzene/
o-dichlorobenzene 40.6 56 49.3 311 52.7 323
Table 3. Criterion (∆) of uniformity of the separation of a ternary model mixture of para-isomers on selective ad-
sorbents (column temperature 230°C)
Model
mixture
Initial (sodium)
form of
Silicalite-1
applied onto
celite-545
Initial (sodium)
form of
Silicalite-2
applied onto
celite-545
Cadmium
form of
Silikalite-1
applied onto
celite-545
Cadmium
form of
Silikalite-2
applied onto
celite-545
Thallium
form of
Silicalite-1
applied onto
celite-545
Thallium
form of
Silicalite-2
applied onto
celite-545
Silver
form of
Silikalite-1
applied onto
celite-545
Silver
form of
Silikalite-2
applied onto
celite-545
p-xylene–
p-chloro-
toluene–
p-dichloro-
benzene
0.24 0.27 0.37 0.40 0.44 0.47 0.56 0.58
Combining Molecular Sieve and Complexing Properties of the Column Packing
_____________________________________________________________________________________________
ХФТП 2010. Т. 1. № 3 295
CONCLUSION
After modification of corresponding stationary
phases, the developed adsorbent can be successfully
used in gas chromatography for the separation and
analysis of mixtures of ortho-, meta-, and para-
isomers of aromatic organic compounds.
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Received 18.05.2010, accepted 17.08.2010
Поєднання молекулярно-ситових і комплексоутворюючих властивостей насадок
в газовій хроматографії
Л. Епрікашвілі, Н. Пірцхалава, Т. Андронікашвілі, Т. Кордзахія,
М. Зауташвілі, М. Дзаганія
Інститут фізичної та органічної хімії ім. П. Мелікішвілі
вул. Джикія 5, Тбілісі 0186, Грузія, physorgchem@pochta.ru
Вивчено вплив модифікування синтетичних цеолітів сімейства пентасілів (Сілікаліту-1 і Сілікаліту-2) ка-
тіонами металів, здатних до специфічних взаємодій, на розділювальну здатність хроматографічної колонки.
Сочетание молекулярно-ситовых и комплексообразующих свойств насадок
в газовой хроматографии
Л.Эприкашвили, Н.Пирцхалава, Т.Андроникашвили, Т.Кордзахия,
М.Зауташвили, М.Дзагания
Институт физической и органической химии им. П. Меликишвили
ул. Джикия 5, Тбилиси 0186, Грузия, physorgchem@pochta.ru
Изучено влияние модифицирования синтетических цеолитов семейства пентасилов (Силикалита-1 и
Силикалита-2) катионами металлов, способными к специфическим взаимодействиям, на разделительную
способность хроматографической колонки.
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