ISSN 1070-4272, Russian Journal of Applied Chemistry, 2007, Vol. 80, No. 1, pp. 131!138. + Pleiades Publishing, Ltd., 2007.
Original Russian Text + V.V. Platonov, A.A. Khadartsev, A.Yu. Shvykin, D.V. Prokopchenkov, V.A. Proskuryakov, T.V. Chestnova, 2007, published
in Zhurnal Prikladnoi Khimii, 2007, Vol. 80, No. 1, pp. 132!139.
AND POLYMERIC MATERIALS
Chemical Composition of Oxidative Degradation Products
of the Organic Matter of Shungite Rock
from the Zazhogino Deposit (Karelia, Trans-Onega Region)
V. V. Platonov, A. A. Khadartsev, A. Yu. Shvykin, D. V. Prokopchenkov,
V. A. Proskuryakov, and T. V. Chestnova
Leo Tolstoy State Pedagogical University, Tula, Russia
Tula State University, Tula, Russia
St. Petersburg State Technological Institute (Technical University), St. Petersburg, Russia
Received April 25, 2006
Abstract-Oxidative degradation of the organic matter of shungite rock from the Zazhogino deposit (Kare-
lia, trans-Onega region) with various reagents was performed. The composition of the products obtained was
studied by IR Fourier spectroscopy and gas chromatography3mass spectrometry. The set of the compounds
identified reflects the structure and origin of the macromolecular network and mobile phase of shungite.
Oxidative degradation is relatively widely used for
determining the features of chemical composition and
structural organization of macromolecules of various
caustobioliths . In this study we examined the
chemical composition of the organic matter (OM)
of shungite rock (SR) from the Zazhogino deposit
(Karelia, trans-Onega region) by oxidative degradation
with various reagents.
The starting shungite rock ground in a ball mill to
a particle size of 70390 mm was charged into a Teflon
vessel and thoroughly stirred for 6 h at 20oC with
40% HF. The resulting slurry was allowed to settle,
and the solid phase was repeatedly washed with water
to pH ~7 by decanting, vacuum-filtered on a B1uchner
funnel, and dried to constant weight at 100oC, after
which the OM content in SR was determined by ther-
mal gravimetric analysis of the resulting OM-enriched
product. According to the elemental analysis, treat-
ment of the initial SR with aqueous HF increased the
OM content from 30.21 to 82.00 wt %. The elemental
composition of SR OM (wt % daf) is as follows:
C 95.45, H 0.30, N 0.60, and O + S 3.65.
Oxidation of SR OM with an alkaline solution of
ammonium peroxodisulfate was performed as follows.
A 100-ml three-necked flask with a power-driven stir-
rer and a thermometer was charged with 10 g of the
enriched SR and 50 ml of 16 wt % aqueous NaOH.
The resulting suspension was heated to 60oC with
vigorous stirring, after which 5 g of dry (NH
was added in small portions through the third neck.
In so doing, intense foaming was observed because of
the release of ammonia and oxygen. After 1 h, the
temperature was raised to 90oC, an additional5gof
was added, and the mixture was stirred
at 90oC for 2 h, after which the third portion (5 g) of
was added. Then the mixture was stirred
at 90oC for 3 h more, cooled to room temperature, and
vacuum-filtered through a glass frit no. 4; the residue
of the enriched SR was washed with distilled water to
neutral reaction, dried in a vacuum oven to constant
weight, and weighed. The weight of the solid obtained
was 8.50 g.
The brown filtrate was combined with wash waters
and extracted in a separating funnel with CH
(4 0 50 ml). The combined extracts were dried over
, and the solvent was distilled off
on a water bath. The residue was dissolved in a small
amount of chloroform, the solution was quantitatively
transferred into a weighed bottle, and the solvent was
evaporated in an oven at 70oC. The resulting extract
was dried in a vacuum oven to constant weight. The
yield of the CH
extract was 0.04 wt % relative to