1070-4272/02/7511-1795$27.00C2002 MAIK [Nauka/Interperiodica]
Russian Journal of Applied Chemistry, Vol. 75, No. 11, 2002, pp. 1795!1798. Translated from Zhurnal Prikladnoi Khimii, Vol. 75, No. 11,
2002, pp. 1830!1833.
Original Russian Text Copyright + 2002 by Kartsova, Makarov.
AND ION-EXCHANGE PROCESSES
A Mixed Phase C
for Gas Chromatography
L. A. Kartsova and A. A. Makarov
St. Petersburg State University, St. Petersburg, Russia
Received April 24, 2002
Abstract-Stationary phases for gas chromatography were prepared: 10 wt % fullerene C
on Inerton N-AW
(deposition from saturated toluene solution) and a mixed phase C
+ dibenzo-24-crown-8. These phases were
tested in a wide temperature range (403280oC) with selected organic compounds containing various func-
tional groups and with their mixtures.
Active recent efforts were aimed at searching for
new selective chromatographic phases allowing sep-
aration in one chromatographic run of multicompo-
nent mixtures of compounds differing in the nature of
functional groups, polarity, and boiling point.
Development of an electric-arc procedure for pre-
paring fullerenes in a fairly high yield stimulated
active studies of the chemical and physicochemical
properties of the new modification of carbon. Chro-
matographic studies of interactions between fullerenes
and organic compounds furnish useful information
concerning both the physicochemical properties of
fullerenes themselves and their possible use as chro-
The high hydrophobicity of C
with its thermal stability, resistance to oxidation, and
capability for donor3acceptor interactions make this
substance promising as a stationary phase for gas
The selectivity range in analysis of multicompo-
nent mixtures can be extended by using mixed phases.
Combining fullerenes with crown ethers will not only
affect the physicochemical characteristics of the car-
bonaceous stationary phases (solubility, hydrophobic-
ity, capability for various specific interactions with
functional groups of components of complex mixtures
being separated), but also furnish new data on com-
plexation with macrocycles.
Stationary phases were prepared from fullerenes
(Astrin Joint-Stock Company, St.
Petersburg) and dibenzo-24-crown-8 (DB-24-C-8,
Reaktiv-Servis Scientific and Production Complex,
Limited Liability Company, Moscow).
tested as stationary phase for gas
chromatography was applied onto Inerton N-AW sup-
port (grain size 0.2030.315 mm) in an amount of
10 wt % from toluene. A toluene solution of fullerene
was added to Inerton N-AW placed in a porcelain cup
in an amount fully covering the solid (0.5-cm layer of
the liquid over the solid); the cup was placed on a
water bath and carefully stirred until the solvent was
fully evaporated. The mass obtained after the solvent
evaporation was dried in the air thermostat of a Tsvet-
500M gas chromatograph at 100oC for 3 h. Then it
was sieved through standard sieves, and the 0.203
0.25-mm fraction was used as packing for a 3000 0
2-mm glass column. The packed column was condi-
tioned in a carrier gas flow (N
, 30 ml min
wise heating from 70 to 270oC).
The mixed C
+ DB-24-C-8 phase was prepared
as follows. Fullerene was applied onto Inerton N-AW
(0.203 0.25 mm) as described above, after which
10 wt % DB-24-DC-8 was applied from a chloroform
solution (at the reverse application order, i.e., first
DB-24-C-8 from chloroform and then C
ene, the characteristics of the resulting sorbent were
similar). After complete evaporation of the solvents,
the packing was dried in the air thermostat of a Tsvet-
500M gas chromatograph at 70oC for 3 h. Then it was
used as packing for a 3000 0 2-mm glass column. The
packed column was conditioned in a carrier gas flow
, 30 ml min
; programmed heating from 80 to
200oC and keeping at 200oC for 5 h).
Experiments were performed with the participation of