J. Serb. Chem. Soc. 63(6) 395 (1998)

IN MEMORIAM
Hans-Joachim Neumann

On March 5th, 1997, Prof. Dr. habit. H. J. Neumann died in Clausthal at the age of 66.
H. J. Neumann studied chemistry at the TH Braunschweig. At the same university he received his doctorate in 1959. In 1969 he qualified as University Teacher for Chemical Engineering. In his 35 years of scientific research work he worked on many aspects of chemistry, mainly petroleum chemistry. Since 1976 H.-J. Neumann was an honorary professor at the Technical University, Clausthal. He distinguished himself especially in the field of the composition of bitumens. His research work on bitumen began in 1970 with the results of correlations between chemical composition and practical relevant properties such as rheology, aging and adhesion.
For the bitumen industry Prof. Dr. Neumann was an important consultant and partner in handling research work. His knowledge not only dissipated in the form of lectures, but also in 100 publications now available to the scientific community.
Besides his research and education work he was further engaged in the education of chemists and engineers. He authored the book "Bitumen and Its Application". He has dedicated his knowledge and experience to the education of young scientists in all parts of the world. More than 45 dissertations were completed under his guidance. Most of these were done at the German Petroleum Institute (Institut f?r Erd”l - und Erdgasforschung, IFE). His efforts, outstanding research work, and knowledge led to the national and international fame of the IFE.
Prof. H. J. Neumann was the principal investigator of the joint research project "Synthetic Oil and Petrochemicals from Oil Shale and Polymer-Modified Bitumens", which was carried out by the Faculty of Technology and Metallurgy, Belgrade, the Highway Institute, Belgrade and the German Petroleum Institute, Clausthal-Zellerfeld. He was a co-mentor of two Ph. D. dissertations at the University of Belgrade and helped more than ten students of the Faculty of Technology and Metallurgy, University of Belgrade, to do important experimental measurements in his Institute. In 1990 H. J. Neumann, as the first German scientist, was elected an honorary member from abroad of the Serbian Chemical Society and for many years he was a member of the Editorial Board from abroad of the Journal of the Serbian Chemical Society.
We mourn an outstanding scientists and friend. We will miss his scientific experience and help.

Iradj Rahiman and Jovan Jovanovic 



J. Serb. Chem. Soc. 63(6) 397-418 (1998)
UDC 622.24/497.1/:665.51
JSCS-2544
Review paper

REVIEW
Organic geochemical investigation of crude oils. The southeastern part of the Pannonian Basin in Yugoslavia

BRANIMIR S. JOVANCICEVIC*,**, PREDRAG S. POLIC*,** and DRAGOMIR K. VITOROVIC**

*Faculty of Chemistry, University of Belgrade, P. O. Box 158, YU-11001 Belgrade and
**Centre of Chemistry ICTM, Njegoseva 12, Belgrade, Yugoslavia

(Received 13 January 1998)

1. Introduction
2. Organic geochemical characterisation of crude oils
3. Choice of parameters
4. Crude oils from the southeastern part of the Pannonian Basin
4.1. General characteristics
4.2. Biodegradation
4.3. Origin
4.4. Maturity
5. Conclusions

Key words: organic geochemistry, crude oils, correlation parameters, Pannonian Basin.




J. Serb. Chem. Soc. 63(6) 419-431 (1998)
UDC 665.45.002:66.094.3
JSCS-2515
Original scientific paper

Kerogen diversity demonstrated by oxidation.
III. Type I-II kerogens

DRAGOMIR VITOROVIC, ANDRE AMBLES*, SNEZANA BAJC, OLGA CVETKOVIC and
PREDRAG POLIC**

Centre of Chemistry, Institute of Chemistry, Technology and Metallurgy,
Njegoseva 12, YU-11000 Belgrade, Yugoslavia,
*Department of Chemistry, Faculty of Science, University of Poitiers, France, and
**Faculty of Chemistry, University of Belgrade, P.O.Box 158, YU-11001 Belgrade, Yugoslavia

(Received 9 February 1998)
A parallel study of intermediate type I-II kerogens from shales of various geographic origin (Timahdit and S. Pyongan shales and Estonian Kukersite) is described in this paper. An optimised multistep alkaline permanganate degradation method was used for their structural characterisation and differentiation. In addition to the proportions of the three main types of acidic oxidation products, as the basis for classification and characterisation, experimentally based supplementary fourth parameters were also introduced, aimed at improving the kerogen structural interpretations. Striking differences in the distribution of various kinds of aliphatic and aromatic acids enabled the advanced structural differentiation of seemingly similar kerogens.

Key words: kerogen, type I-II; structural characterisation; alkaline permanganate degradation; oxidation products.




J. Serb. Chem. Soc. 63(6) 433-437 (1998)
UDC 547.387:66.094.1:66.097.3
JSCS-2546
Original scientific paper

Reduction of some rigid ketones with thermally activated Al(OH)3 and 2-propanol as hydrogen donor

JOZE FORSEK

Faculty of Chemistry, University of Belgrade, Studentski trg 12-16, P. O. Box 158, and
Center for Chemistry, ICTM, Njegoseva 12, YU-11000 Belgrade, Yugoslavia

(Received 30 December 1997)
The reduction of some rigid ketones, 5a-cholestan-3-one (1), 4-tert-butylcyclohexanone (4), 5a-cholestane-3,6-dione (7) and 5a-androstane-3,17-dione (10), with thermally activated Al(OH)3 in refluxing 2-propanol as the hydrogen donor has been investigated. The reduction afforded predominantly alcohols 3 and 6, as the result of a stereoselective reduction of ketones 1 and 4, and alcohols 9 and 12, as the result of both a stereoselective and regioselective reduction of ketones 7 and 10.

Key words: reduction, rigid ketones, activated Al(OH)3, 2-propanol.




J. Serb. Chem. Soc. 63(6) 439-443 (1998)
UDC 547.857.1:547.455.562.7:542.9
JSCS-2547
Original scientific paper

Stereoselective reduction of the C4 carbonyl group of methyl 2,3,6-tri-O-methyl-a-D-xylo-hexopyranosid-4-ulose.
Synthesis of methyl 2,3,6-tri-O-methyl-a-D-galactopyranoside

DAVID YEAGLEY and MOMCILO MILJKOVIC
Department of Biochemistry and Molecular Biology, The M. S. Hershey Medical Center,
The Pennsylvania State University, Hershey, PA 17033, USA

(Received 17 February 1998)
Reduction of methyl 2,3,6-tri-O-methyl-a-D-xylo-hexopyranosid-4-ulose with lithium tri-sec-butylborohydride gave methyl 2,3,6-tri-O-methyl-a-D-galactopyranoside as the only detectable product. Reduciton of 1 by lithium aluminum hydride gave a mixture of corresponding D-gluco- and D-galacto-derivatives in 3:4 ratio.

Key words: synthesis, stereoselective reduction, methyl 2,3,6-tri-O-methyl-a-D-galactopyranoside.




J. Serb. Chem .Soc. 63(6) 445-453 (1998)
UDC 547.424.1:547.51
JSCS-2548
Original scientific paper

Substituted oxetanes in polymer synthesis.
III. Polyesters based on 3,3-bis(chloromethyl)oxetane and various dicarboxylates.
The influence of the chemical structure upon thermal behaviour

VICTOR BULACOVSCHI and VIOLETA TOADER

Technical University "Gh. Asachi" Iasi, Macromolecular Department,
Bd. Copou 11A, Iasi, RO-6600, Romania

(Received 26 November 1997, revised 23 February 1998)
This paper presents some aspects regarding the synthesis and thermal behaviour of polyesters, based on 3,3-bis(chloromethyl)oxetane (BCMO) and various dicarboxylates. In order to explain the different behaviour of the reaction systems, the reactivity of the dicarboxylate anions in the nucleophilic replacement of the chlorine atom was estimated using an AM1 programme. The polymers were characterized by 1H-NMR and DSC. Almost all the studied polyesters show good thermal stability. The lop-sides connection of the structural units to the main chain lowers the transition temperatures.

Key words: polymer synthesis, polyesters, oxetanes, thermal behaviour.




J. Serb. Chem. Soc. 63(6) 455-466 (1998)
UDC 678.742:543.4
JSCS-2549
Original scientific paper

Optical microscopy analysis of the morphology of isotactic polypropylene

ANITA GROZDANOV and GORDANA BOGOEVA-GACEVA

University "St. Cyril and Methodius", Faculty of Technology and Metallurgy,
Rugjer Boskovic 16, Skopje, Macedonia

(Received 16 July 1997, revised 16 February 1998)
The melt nucleation and crystallization, as well as the morphology of isotactic polypropylene, i-PP, used as a matrix in long fibre reinforced composites, were analysed by polarizing optical microscopy (POM). The investigations were carried out dynamically and isothermally in the temperature regime (Tc = 116-136°C) with a cooling rate of 5 K min-1. It was found that the nucleation density of i-PP decreases with increasing Tc, and, for the studied range of crystallization temperatures, an induction period ranging from 3 s to 25 min was determined. The growth rate of the spherulities was determined (4.7 - 0.14 µm/min) at different Tc values (119 - 136°C), and the crystallization energy parameters were calculated. The value for the fold surface free energy, se, was 0.64×10-5 J cm-2, and the lamellae thickness changed in the range from 436 to 642 nm, depending on the Tc.

Key words: i-PP, crystallization, morphology, nucleation, polarizing optical microscopy.




J. Serb. Chem. Soc. 63 (6) 467-474 (1998)
UDC 546.562/547.962.3:541.573
JSCS-2550
Original scientific paper

Application of differential pulse polarography to the study of the binding of Cu(II)-ions to albumin

JASMINA VIDIC, DESANKA SUZNJEVIC and DUSAN VUCELIC*

Institute of General and Physical Chemistry, Studentski trg 12-16/V, YU-11001 Belgrade and
*Faculty of Physical Chemistry, Studentski trg 12-16, YU-11001 Belgrade, Yugoslavia

(Received 6 October 1997, revised 23 January 1998)
The formation of the complex between copper(II)-ions and serum albumin has been studied by differential pulse polarography (d.p.p.) using 100 mM KCl/10 mM NaHCO3 solution, pH 7.8 and 50 mM citrate buffer/100 mM KCl/10 mM NaHCO3, pH 6.0, as the supporting electrolytes. It was found that the presence of citrate, as a strong chelator of copper, causes a decrease in the number of Cu(II)-ions bound to albumin. Unspecifically bound Cu(II)-ions could be removed during the time of incubation from both buffers studied. It has been demonstrated that d.p.p., with a working dropping mercury electrode, can be a useful technique for studying protein-metal interactions directly in solution.

Key words: bovine serum albumin, copper(II) complex, differential pulse polarography.




J. Serb. Chem. Soc. 63(6) 475-480 (1998)
UDC 577.18:543.544.2/.8
JSCS-2551
Original scientific paper

Determination of sodium fusidate in dosage forms by high performance liquid chromatography

SOTE VLADIMIROV, LJILJANA IVANISEVIC*, DANICA AGBABA, JASMINA BRBORIC and
DOBRILA ZIVANOV-STAKIC

Department of Pharmaceutical Chemistry and Drug Analysis, Faculty of Pharmacy, P. O. Box 146, 11152 Belgrade, and
*Department of Pharmacy, Vojvode Stepe 458, Belgrade, Yugoslavia

(Received 20 November 1997, revised 6 January 1998)
A simple HPLC procedure, suitable for the determination of sodium fusidate (SF) in dosage forms, was developed. The method involves using a UV detector (208 nm) in the presence of basic buffered media (pH 7.25) under reversed-phase conditions (Supelcosil® LC18TM, 3 mm particles). The linear regression between the concentration of SF and the peak area, y =  -4.4566 + 8.9238 x with a coefficient of correlation r = 0.9985, was confirmed for SF in the concentration range from 25 µg ml-1 to 150 µg ml-1. The detection limit of SF was 12.5 µg ml-1. The HPLC method was applied for the determination of SF in dosage forms: Stanicid® coated tablets, Stanicid® ointment and Stanicid® sterile gauze dressing. The concentrations and statistical parameters of sodium fusidate for all the investigated dosage forms were satisfactory and ranged from 100.41 to 105.39% (the R. S. D. ranged from 1.51 to 2.75%).

Key words: Rp-HPLC, UV-detection, sodium fusidate, raw material, dosage forms.




J. Serb. Chem. Soc. 63(6)481-487(1998)
UDC 577.164.1:543.2
JSCS-2552
Original scientific paper

Kinetic determination of pyridoxine hydrochloride in pharmaceutical samples

S. S. MITIC, G. Z. MILETIC, S. M.MILETIC and D. A. KOSTIC

Department of Chemistry, Faculty of Philosophy, University of Nis, YU-18000 Nis, Yugoslavia

(Received 22 November 1997, revised 23 January 1998)
A kinetic method is described for the determination of pyridoxine hydrochloride based on its inhibiting effect on the Mn(II) catalysis of the oxidation of malachite green with potassium periodate. The sensitivity of the method is 0.2 mg cm-3. The relative error ranges between 3.5 and 11.0% for the concentration interval 2.0 to 0.2 mg cm-3. Kinetic equations are proposed for the investigated process .The effects of certain foreign ions upon the reaction rate were determined for the assessment of the selectivity of the method. The method was applied to determine pyridoxine hydrochloride in pharmaceutical samples.

Key words: kinetic method, pyridoxine hydrochloride determination, malachite green oxidation, pharmaceutical samples.


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