1070-4272/02/7505-0840$27.00C2002 MAIK [Nauka/Interperiodica]
Russian Journal of Applied Chemistry, Vol. 75, No. 5, 2002, pp. 840 !845. Translated from Zhurnal Prikladnoi Khimii, Vol. 75, No. 5,
2002, pp. 858!863.
Original Russian Text Copyright + 2002 by Begak, Syroezhko, Fedorov.
OF FOSSIL FUEL
Trace Contaminants in Tars and Bitumens from West-Siberian
and Yarega Crude Oils
O. Yu. Begak, A. M. Syroezhko, and V. V. Fedorov
Mendeleev Research Institute of Metrology, Federal State Unitary Enterprise, St. Petersburg, Russia
St. Petersburg State Technological Institute, St. Petersburg, Russia
Received January 28, 2002
Abstract-The trace contaminant levels were determined for ten tar samples and six bitumen samples avail-
able from Kirishi, Yaroslavl, and Ukhta refineries, as well as from Neste (Finland).
High quality of road bitumens
is of decisive im-
portance for lengthening the lifetime of asphalt con-
crete pavement . In recent years the quality of tar
used as raw material for bitumen preparation was
stabilized. Also, bitumen production (Kirishi refinery)
widely utilizes bitumen compounding with tars and
vacuum gas oils, which significantly improves the
performance characteristics of commercial road bi-
tumens. BDUS 70/100 and BDUS 100/130 (produced
by the KINEF Limited Liability Company) bitumens
substantially exceed in quality BND 40/60, BND
60/90, and BND 90/130 bitumens that were previous-
ly produced by this enterprise. However, the possibili-
ties for improving the bitumen quality at the enter-
prise are not exhausted.
As known, bitumens with close group and chemi-
cal compositions obtained from the same raw material
often differ in the thermal stability (penetration P
and ductility D
sharply decrease after heat treat-
ment). The above parameters strongly depend on the
amount and composition of the impurity metals and
nonmetals both in the initial tars and commercial
products. This study was devoted to elucidation of
this dependence in the case of raw materials available
from the above-listed refineries.
Ten samples of BDUS 70/100 and BDUS 60/90
bitumens and tars from bitumen installations at the
The major suppliers of oxidized road bitumens in Northwest
Russia are Kirishi, Yaroslavl, and Ukhta refineries. The two
first-named enterprises are engaged in processing of the com-
mercial mixture of West-Siberian crude oils, and Ukhta
refinery, in processing of high-resin heavy Yarega crude oil.
Also, bitumens are supplied by Nafta, Finland.
The KINEF Limited Liability Company has undertaken major
reconstruction of the vacuum block of the AVT-6 installation.
KINEF Limited Liability Company and bitumen sam-
ples from Yaroslavl refinery were taken on May 173
24, 2001. Bitumens from the Ukhta refinery and Neste
were prepared in September 1999 and were stored for
two years in closed reservoirs under laboratory condi-
tions, at room temperatures.
All the tar and bitumen samples (Tables 1, 2) were
studied by a common scheme: (a) determination of the
acid numbers, ANs, mg KOH g
; (b) determination
of the content of trace contaminants by mass spec-
trometry with ionization in inductively coupled plasma
(ICP-MS) on a CG Plasma Quad Turbo Plus (Eng-
land) instrument: Weighed portions (753100 mg) of
tars and bitumens were degraded by a 1 : 2 mixture
of concentrated boiling nitric and hydrochloric acids
for 3 h on a sand bath, and the trace contaminants
were transferred to the aqueous phase, which was fol-
lowed by multielement analysis of the resulting solu-
tions; (c) deasphalting of tars and bitumens by cold or
hot precipitation (in a Soxhlet apparatus); (d) separa-
tion of the recovered malthenes into polar and non-
polar components using dimethylformamide (DMF);
(e) exhaustive deasphalting of polar and nonpolar
components of tars and their corresponding bitumens;
(f) chromatographic separation of polar and nonpolar
components of tars and bitumens into group com-
ponents and IR,
H NMR, and
C NMR studies; and
(g) elemental analysis and X-ray diffraction study of
the initial tars and bitumens, malthenes, asphaltenes,
and polar and nonpolar components.
The entire complex of investigations was aimed
at revealing the most significant differences in quality
standard and substandard bitumens and tars.
We found (Table 1) that, on storage for 6 months
under laboratory conditions, tars get harder, and their
penetration significantly decreases, for example, ap-