YU-ISSN 0352-5139
J.Serb.Chem.Soc. Vol. 68, No 3(2003)
CONTENTS
Macromolecules
B. Dunji}, J. Djonlagi}, S. Vuka{inovi}, M.Sepulchre, M. O. Sepulchre and N. Spassky: Rheokinetic study
of crosslinking of a,w-dihydroxy oligo(alkylene maleate)s with a trisisocyanate
147
Physical Chemistry
M. M. A~anski: Retention behaviour of some estradiol derivatives on alumina in normal phase
chromatrography
163
V. Manovi}, B. Grubor, M. Ili} and B. Jovan~i}evi}: Sulfur retention by ash during coal combustion. Part
II. A model of the process
171
H. Hubicka and D. Kolodynska: Separation of Y(dcta)- complexes from Nd(dcta)- and Sm(dcta)complexes on polyacrylate anion-exchangers (Short communication)
183
Electrochemistry
B. N. Grgur, N. M. Markovi} and P. N. Ross Jr.: Electrochemical oxidation of carbon monoxide: from
platinum single crystals to low temperature fuel cells catalysts. Part II. Electrooxidation of H2, CO and
H2/CO mixtures on well characterized PtMo alloy
191
S. Stankovi}, B. Grgur, N. Krstaji} and M. Vojnovi}: Kinetics of the zinc anodic dissolution reaction in
near neutral EDTA solutions
207
Analytical Chemistry
Z. M. Grahovac, S. S. Miti} and E. T. Pecev: Kinetic determination of ultramicro amounts of Cu(II) ion in
solution
219
Environmental Chemistry
T. [olevi}, B. Jovan~i}evi}, M. Vrvi} and H. Wehner: Oil pollutants in alluvial sediments – influence of
the intensity of contact with ground waters on the effect of microorganisms
227
Organic Chemistry
N. Djapi}, Z. Djarmati, S. Filip and R. M. Jankov: A stilbene from the heartwood of Maclura pomifera
(Note)
235
J.Serb.Chem.Soc. 68(3)147–162(2003)
UDC 678.664+547.476.2:543.23
JSCS – 3030
Original scientific paper
Rheokinetic study of crosslinking of a,w-dihydroxy oligo(alkylene maleate)s with a trisisocyanate
BRANKO DUNJI]1, JASNA DJONLAGI]1#, SLAVKO VUKA[INOVI]1, MAURICE SEPULCHRE2,
MARIE-ODILE SEPULCHRE2 and NICOLAS SPASSKY2
1Faculty of Technology and Metallurgy, Karnegijeva 4, YU-11000 Belgrade, Serbia and Montenegro and
2Laboratoire de Chimie Macromoléculaire, Université Pierre et Marie Curie, 4, Place Jussieu, 75005 Paris,
France
(Received 19 June, revised 4 December 2002)
Abstract: The crosslinking reaction of three series of a,w-dihydroxy oligo(alkylene maleate)s with a
trifunctional isocyanate was followed by dynamic mechanical analysis and FTIR spectroscopy. The
evaluation of rheological parameters, such as storage G’ and loss modulus G", was recorded. A typical G’
versus time curve has a characteristic “S” shape, indicating autoacceleration of the crosslinking reaction.
The whole curing process starting from G’ equal G" or the beginning of gelation is described by a second order phenomenological rheokinetic equation which takes into account the autoacceleration effect, the latter
being a consequence of the superposition of both the chemical reaction and phase segregation. It appears
that the crosslinking reaction rate depends on the concentration of the functional groups, i.e., on the
molecular weight of the polyester prepolymer and on the length of the aliphatic sequence in the repeating
unit or the segmental mobility. The crosslinking rate decreases in the order: poly(octamethylene maleate) >
poly(hexamethylene maleate) > poly(butylene maleate).
Keywords: hydroxyl terminated polymaleates, polyurethane, rheokinetic analysis.
REFERENCES
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7. B. Dunji}, M. O. Sepulchre, M. Sepulchre, N. Spassky, J. Djonlagi}, Makromol. Chem. Phys. 199
(1998) 1051
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J.Serb.Chem.Soc. 68 (3)163–170(2003)
UDC 549.73+577.175.6+661.183.7:543.544
JSCS – 3031
Original scientific paper
Retention behaviour of some estradiol derivatives on alumina in normal phase chromatography
MARIJANA M. A^ANSKI
Department of General and Inorganic Chemistry, Faculty of Technology, University of Novi Sad, Bulevar
Cara Lazara 1, YU-21000 Novi Sad, Serbia and Montenegro (e-mail: marijana@tehnol.ns.ac.yu)
(Received 24 September, revised 8 November 2002)
Abstract: The retention constants of variously substituted estradiol derivatives were measured as a function
of the composition of various binary mobile phases in order to study the relationship between chemical
structure and retention behaviour in TLC on alumina. The slopes and intercepts of the linear relationships
between the retention constant RM and the logarithm of the volume fraction of the polar mobile phase
component were calculated and are discussed in relation to the characteristics of the solute and mobile
phase. The RF values and relative retention DRM of the compounds depend largely on the retention
behaviour of their substituents. The results obtained in this investigation are compared with the results of
the same derivatives obtained in previous investigations on silica gel.
Keywords: thin layer chromatography, alumina, non-aqueous binary mobile phases, estradiol derivatives,
Soczewinski equation.
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J.Serb.Chem.Soc. 68(3)171–182(2003)
UDC 662.61/.62+66–948.2+546.22:66.011
JSCS – 3032
Original scientific paper
Sulfur retention by ash during coal combustion. Part II. A model of the process
VASILIJE MANOVI]1, BORISLAV GRUBOR2, MLADEN ILI]2 and BRANIMIR JOVAN^I]EVI]3,4
1Mining and Geology Faculty, University of Belgrade, Dju{ina 7, 11000 Belgrade, 2Institute for Nuclear
Sciences - Vin~a, P. O. Box 522, 11001 Belgrade (e-mail: grub@rt270.vin.bg.ac.yu), 3Faculty of
Chemistry, University of Belgrade, P. O. Box 158, 11001 Belgrade and 4ICTM - Center of Chemistry, P.
O. Box 473, 11001 Belgrade, Serbia and Montenegro
(Received 29 August, revised 18 November 2002)
Abstract: An overall model for sulfur self-retention in ash during coal particle combustion is developed in
this paper. It is assumed that sulfur retention during char combustion occurs due to the reaction between
SO2 and CaO in the form of uniformly distributed non-porous grains. Parametric analysis shows that the
process of sulfur self-retention is limited by solid difussion through the non-porous product layer formed on
the CaO grains and that the most important coal characteristics which influence sulfur self-retention are
coal rank, content of sulfur forms, molar Ca/S ratio and particle radius. A comparison with the
experimentally obtained values in a FB reactor showed that the model can adequately predict the kinetics of
the process, the levels of the obtained values of the SSR efficiencies, as well as the influence of
temperature and coal particle size.
Keywords: coal combustion, sulfur retention by ash, modelling.
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J.Serb.Shem.Soc. 68(3)183–190(2003)
UDC 546.65+547.391.1:620.168.3
JSCS – 3033
Short communication
SHORT COMMUNICATION
Separation of Y(dcta)– complexes from Nd(dcta)– and Sm(dcta)– complexes on polyacrylate anionexchangers
HALINA HUBICKA* and DOROTA KOºODY¼SKA
Department of Inorganic Chemistry, Faculty of Chemistry, Maria Curie-Sklodowska University, Maria
Curie-Sklodowska Sq. 3, 20-031 Lublin, Poland
(Received 20 September, revised 4 December 2002)
Abstract: The formation of anion rare earth element complexes with aminopolycarboxylic acids gives new
possibilities for the separation of these elements on anion-exchangers. The higher affinity of the Nd(dcta)and Sm(dcta)- complexes for the anion-exchangers compared to Y(dcta)- complexes indicates the
possibility of yttrium purification as a macrocomponent from the former by frontal analysis. The weakly
basic polyacrylate gel anion-exchanger Amberlite IRA 68 was more effective in the purification of Y(III)
from Nd(III) and Sm(III) complexes with DCTA than the strongly basic anion-exchangers of this type.
Keywords: rare earth elements, polyacrylate anion-exchangers, DCTA.
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J.Serb.Chem.Soc. 68(3)191–205(2003)
UDC 66.087.3:546.263.3–34+546.92
JSCS – 3034
Original scientific paper
Electrochemical oxidation of carbon monoxide:
from platinum single crystals to low temperature fuel
catalysts. Part II: Electrooxidation of H2, CO and H2/CO
mixtures on well characterized PtMo alloy
BRANIMIR N. GRGUR1, , NENAD M. MARKOVI]2 and PHILIP N. ROSS JR.2
1Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11001 Belgrade, Serbia
and Montenegro and 2Lawrence Berkeley National Laboratory, 1 Cyclotron Road, MS 2-100, Berkeley,
CA 94720, USA
(Received 5 November 2002)
Abstract: The oxidation of hydrogen and hydrogen–carbon monoxide mixture has been investigated on
well-characterized metallurgically prepared platinum–molybdenum (PtMo) alloys. It was concluded that
the optimum surface concentration of molybdenum is near 23 mol.%. Based on experimentally determined
parameters and simulations, the mechanism of the oxidation of CO/H2 mixtures is discussed.
Keywords: fuel cell, anode, platinum, molybdenum, hydrogen, carbon monoxide.
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J.Serb.Chem.Soc. 68(3)207–218(2003)
UDC 546.47+532.73:543.559
JSCS – 3035
Original scientific paper
Kinetics of the zinc anodic dissolution reaction in near neutral EDTA solutions
SLAVKA STANKOVI], BRANIMIR GRGUR, NEDELJKO KRSTAJI]# and MILAN VOJNOVI]#
Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade,
Serbia and Montenegro
(Received 8 October, revised 11 November 2002)
Abstract: Polarization curves of the anodic dissolution reaction of zinc were determined in EDTA solutions
of different total molar concentrations (0.05, 0.10, 0.15 and 0.20 mol dm-3), the pH values of which were
systematically varied (pH 3.0 – 10.0). The Tafel slopes of the anodic polarization curves are close to 40 mV
dec-1 at lower current densities (10-5 – 5´10-4 A cm-2), while at higher current densities (5´10-4 – 10-2 A
cm-2) the slopes are in the range of 60 – 120 mV dec-1. The order of the anodic reaction determined from
the anodic polarization curves at lower current densities are: z+ (H+) » – 1/2 for pH < 8 and z+(H+) » 1 for
pH > 8, while z+(H4Y) » 1 for all pH values of the examined EDTA solutions. On the basis of these
results, two mechanisms of the zinc anodic dissolution reaction are proposed: at pH < 8 and at pH > 8. In
both cases the relevant EDTA species directly participate as reactants in the anodic reaction. The
dependences of the corrosion potential on pH and on total molar EDTA concentration indicate that the
relevant EDTA species take part as reactants in both the cathodic (hydrogen evolution) and anodic (zinc
dissolution) reactions of the zinc corrosion process.
Keywords: zinc, EDTA, anodic dissolution, kinetics, mechanisms.
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J.Serb.Chem.Soc. 68(3)219–226(2003)
UDC 543.23+54.063:546.56+541.8
JSCS – 3036
Original scientific paper
Kinetic determination of ultramicro amounts of Cu(II) ion in solution
Z. M. GRAHOVAC, S. S. MITI] and E. T. PECEV
Faculty of Natural Sciences and Mathematics, Department of Chemistry, University of Ni{, Vi{egradska
33, 18000 Ni{, Serbia and Montenegro
(Received 19 September, revised 26 November 2002)
Abstract: A new kinetic method is described for the determination of ultramicro amounts of Cu(II) based
on its catalytic effect on the oxidation of trisodium-2-hydroxy-1-(4-sulphonato-1-naphthylazo)naphthalene6,8-disulphonato (red artificial color PONCEAU 4R) by hydrogen peroxide in borate buffer (B.B.) The
detection limit given by Perez-Bendito is 0.8 ng/cm3, but the detection limit that we experimentaly
determined is 3.8 ng/cm3. The relative error ranges between 7.77 and 2.09 % for the concentration interval
3.8 to 50.1 ng/cm3. Kinetic equations are proposed for the investigated process. The effects of certain
foreign ions upon the reaction rate were determined for an assessment of the selectivity of the method. The
method was applied for the determination of Cu(II) ions in samples of alloy.
Keywords: kinetic method, copper(II) determination, PONCEAU 4R, samples of alloy.
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J.Serb.Chem.Soc. 68(3)227–234(2003)
UDC 504.054:553.068.2:628+579.24
JSCS – 3037
Original scientific paper
Oil pollutants in alluvial sediments – influence of the intensity of contact with ground waters on the effect
of microorganisms
T. [OLEVI]1,2, B. JOVAN^I]EVI]1,2 , M. VRVI]1,2# and H. WEHNER3
1Faculty of Chemistry, University of Belgrade, P. O. Box 158, 11001 Belgrade, 2ICTM, Chemistry
Centre, P. O. Box 815, 11001 Belgrade, Serbia and Montenegro and 3Federal Institute for Geosciences and
Natural Resources, P. O. Box 510153, Hannover, Germany
(Received 4 October, revised 3 November 2002)
Abstract: The influence of the intensity of interaction between oil pollutants and ground waters in alluvial
sediments on the effect of microbial activity was investigated in this work. The study was based on a
comparison of detailed analyses of two fractions of an oil pollutant originating from a Danube alluvial
formation near the Pan~evo Oil Refinery: fraction 1, separated from the aqueous layer by decantation,
presumed to have been in less intensive interaction with water, and fraction 2, isolated from the aqueous
emulsion by extraction with chloroform, presumed to have been in stronger interaction with water. Both
fractions were shown to originate from the same type of oil pollutant. Nevertheless, significant
compositional differences between the two fractions were observed. A significantly pronounced
domination of even carbon number homologues of C18–C24 n-alkanes in fraction 2, atypical for crude oil
pollutants, compared to the corresponding distribution observed in fraction 1, suggested a more intense
activity, i.e., a much better effect of microorganisms in direct contact with the oil pollutant within the
aqueous environment. The identification of even carbon number C14–C18 n-alcohols and C14–C18 fatty
acids, as well as cholesterol, in fraction 2, suggested that microorganisms of the algal type in nonphotosynthetic conditions were most probably responsible for the mentioned microbial processes.
Keywords: oil pollutants, alluvial ground waters, microbial activity, n-alkanes, n-alcohols, cholesterol, fatty
acids.
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UDC 547.636.2:633.913.2
JSCS – 3038
Note
NOTE
A stilbene from the heartwood of Maclura pomifera
NINA DJAPI]1, ZOLTAN DJARMATI2, SNE@ANA FILIP2 and RATKO M. JANKOV3,
1Tehnical Faculty “Mihajlo Pupin”, University of Novi Sad, Djure Djakovi}a b. b., 23000 Zrenjanin, 2BioEcological Centre, Petra Drap{ina 15, 23000 Zrenjanin and 3Chemical Faculty, University of Belgrade,
Studentski trg 16, 11000 Belgrade, Serbia and Montenegro
(Received 1 July, revised 3 December 2002)
Abstract: Dried heartwood powder of Maclura pomifera, Moraceae, was extracted with acetone. Silica gel
column chromatography (CC) of the crude extract yielded 2',3',4',5'-tetrahydroxystilbene (oxyresveratrol).
Keywords: Maclura pomifera, Moraceae, heartwood, oxyresveratrol.
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