SCIENTIFIC ABSTRACT MATYSKA, BA. - MATYUKHIN, N.YA.

• Document Type: CREST
• Collection: Scientific Abstracts
• Document Number (FOIA) /ESDN (CREST): CIA-RDP86-00513R001033010018-4
• Release Decision: RIF
• Original Classification: S
• Document Page Count: 100
• Document Creation Date: November 2, 2016
• Document Release Date: June 14, 2000
• Sequence Number: 18
• Publication Date: December 31, 1967
• Content Type: SCIENTIFIC ABSTRACT

Z/ODq/6o/ooe/ojLi/ooj/ooi
E112/E153
Analytical Control of Isoprene Rectification
Two types of isoprene from different sources were investigated:
1) Soviet material, with 96% isoprene content, and 2) Czecho-
slovak material, prepared from isobutylene and formaldehyde, with
13% isoprene. The different distillation fractions were analysed
by mass spectrography, infrared spectroscopy and gas chromato-
graphy, using thermoconductivity cells for detection. A
chromatogram of sample B (Czechoslovak), e.g. first sample of
condensate from stIll-head. is shown ItFig.l), revealing 8 peaks
and identified as follows: 1) isobutylene, not isolated in
pure state but found in one fraction in an amount of 15%
together-with 85ao' 3-methylbutene-1; 2) and 3), peaks
appertaining to butene-I and butene-2 (confirmation of structure
through mass spectrography); 4) 3-miethylbutene-I (this compound
was isolated from one fraction in 99.5 purity and identified
spectroscopically by comparison with data in the literature;
5) 2-methylbutene-I (this compound was identified by comparison
with literature data. It was obtainod by fractional distillation
Xn approximately 80% purity. It was also obtained by preparative
Cavd=k*

Z/ ooq/6o/ooo/oi1/ool/ooi
E1.12/E153
Analytical Control of Isoprene Rectification
gas chromatography, and both samples proved identical);
6) isoprene: standard prepared by fractional distillation in
99.98% purity and by preparative chromatographic method (ethyl
cyclopentanecarboxylate as stationary phase); 7) 2-methylbutene-2
prepared by fractional dititillation in 98% purity (identified by
method used for 3-methylbutene-1; compound prepared for
identification purpose also by preparative gas chromatography).
Chromatogram of sample A (Soviet isoprene) revealed similar
characteristics. A special peak 0b) was noticed, the identity
of which was not yet determined. Results of practical
distillation tests were as follows. Sample A was distilled over
a low-efficiency column with reflux ratio 13:1. Pentene
contents were reduced from 4 to 1.256, and isoprene of 98.8% purity
and in yields of 80% was collected. Using a more efficient column
with reflux ratio 40:1 equilibrium was established after 2 hours
and isoprene of 99.98% purity was obtained in poor yields.
Attempts to improve yields by the addition of azeotropic agents
(methanol, water) failed. Distillation of sample B was undertaken
Car4=54&

Z/009/60/000/011/001/001
MVE153
Analytical Control of Isoprene Rectification
over a column with reflux ratio 4:1. The concentration of
isoprene in the middle fraction was doubled and the distillate
contained only four components: 3-methylbutene-1; 2-methyl-
butene-1; isoprene; 2-methylbutene-2. A further fractionation
over a column with reflux ratio 25:1 yielded further fraction,
from which only those containing 2-methylbutene-1, isoprene and
2-methylbutene-2 were collected. Distillation of the three
combined fractions over a column with reflux ratio 40:1 gave a
two-component mixture in which the pentene concentration amounted
to only 13%. By azeotrcopic distillation with acetone,
conversion into high-gracte isoprene could be achieved. It is
claimed that yields were satisfactory. Acknowledgements are
made to Doctor J. Pech, director, V16SK Gottwaldov for useful
advice and for supplying some of the raw materials.
There are 6 figures, 4 tables and 16 references (including several
patents to one reference): 11 English, 4 Czech and 1 Soviet.
ASSOCIATION: Ustav fyzikAlni chemie CS", Praha (Institute for
Card:ZIQ% Physical Chemistry, 6S" Prague)
SUBMITTED: June 6, i!)6o

S/081 62/000/024/033/073
B144/B186
AUTHORSo PoWek, J., Matyska. B.
TITLEs Chromatographic fractionation,of polychloroprene
PERIODICALs Beferativnyy zburnali Khimiya,'~no. 24, 1962, 25'9-26o,
abstract 20266 (Collect. Czechoel. Commune, v. 27, no. 4.
1962, 616 - 822 [Ger.; summary in Russ.])
TEXT: It was established that polymers can be separated chromatographi-
-:ally into fracttons having similar molecular we.ight even on adsorbents
such as 0powdered glass and NaGl. The chromatography was performed at
19 - 23 C in columns (44.0&2.8 or 58.0o2.8 cm) filled with powdered glass
having a granulation of 0.01 or 0.02 cm or with NaCl powder of