ORIG. RUSSIAN: EXPERIMENTAL PRODUCTION OF STABLE ISOTOPES

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP88-00904R000100110033-3
• Release Decision: RIPPUB
• Original Classification: U
• Document Page Count: 20
• Document Creation Date: December 22, 2016
• Document Release Date: August 26, 2009
• Sequence Number: 33
• Publication Date: May 1, 1964
• Content Type: STUDY

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Third United Nations
International Conference
on the Peaceful Uses
of Atomic Energy
Confidential until official release during Conference
EXPERIMENTAL PRODUCTION OF STABLE ISOTOPES
I.G.Gverdtziteli, T.A.Gagooa, G.N.Muskhelishvilt
U.V.Nikolaev, E.D.Oziashvili, G.A.Thevzadze
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Introduction
To develops works on stable isotopes application a r;ilot,
plant producing boron, nitrogen, oxigen, carbon, noon, :irgor
krypton and other isotopes has been organized in Tbil iasi ..
Isotope separation is carried out by means of dist.illrition,
chemical, exchange and mass-diffusion methods. Experimental
production technological cycle also includes the preparation
of initial products to feed boron isotopes separating devices
and the synthesis of a number of compounds on th a bass of
boron, nitrogen, oxigen and other isotopes.
The basic building of the pilot plant is a fifteen-sto-
rey tower of the 63 metres height. Column type separating de-
vices are placed on its verticals. Mass-diffusion cascades
and auxiliary equipment are situated on its floors. The suffi-
cient height of the tower permits to set columns of cascade
one above another; in such a way as to realize material trans-
port between columns through the special dosing devices with-
out piping pump application. It's evident that such a system
of f lux distribution appreciably increases separating equip-
ment operation reliabilit y. The four-storey building adjoins
upon the towor part. There are placed there: a control-room
where all the separating processes automatic control systems
are concentrated; initial products producing devices; enriched
raw material treatment devices and isotopic composition and
chemical analysis control laboratories too.
A general sight of the production building with its
tower part is given in the figure I.
Production Cycle Obtaining Compounds on the Boron-IO
and Boron-II Bases.
Technological process general diagram which shows an
interrelation between separate cycles is performed in the
figure 2. The technological process includes:
.iUU
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I. Production of boron trif luoride BF3 and its dimethyl
ether complex (CH;1)) 6 ?BF;~;
2. Boron isotope separation by distillation BF.; and
exchange distillation (CH,,),,O?BF;{ methods.
3. Converting of the enriched feed into the elemental
boron, boron acid and other compounds
Boron trifluoride is obtained by acidic method (adjust-
ment I) from the reaction:
6KBF4+B203 + 6H2SO4 = 8BF3+6KHSO4+ 3H20.
Tho purity of BFI was 99%. The major impurities are: SO,,,
and SiP,1. A part of the boron trifluoride is gone to feed
columns, separating boron isotopes by low-temperature dis-
tillation--BF,, (adjustment 4), the rest of BF,, is supplied
to the device 2 to obtain its dimethyl ether complex. Herne
dimetbyl ether of industrial production is used; the purity
of which is 99, 8~b. The waste of the BF 3 producing process
is neutralized in the apparatus 3 and is canted off. To pro-
duce boron isotopes ( B'J and B 11 ) a number of devices is
equipped; they consist of the three separating cascades to
obtain boron oy the exchange distillation method of the
compound (CH ;5) 2 0 ? BF,5 /192/ and columns , separating boron
isotopes by BF,,, distillation method. /3,4,5/
I. Cascade device wits 25kg boron eutput ., ye arly with
B1~ 855 concentration consists of the two colu"Ns 5 and 6.
The diameters of the first and second cascade columns are
128 and 70 mm; the length of the packed part is 21, 7 and 22m
accordingly. The B 10 concentration in the lower part of the
first column is 50% and in the waste; it is 8%.
2. The column 7 with 50 kg boron output yearly with
B 40% ' concentration has a packed part length of 22,,7m and
a diameter of I28mn. B10 concentration in the waste it 8%.
3. The column 8 is megat for 90kgboron_yearly pro-
duct-ion with B11- 991 concentration. The length of its
packed part is 23m, and the diameter of the column is 128mm.
The Bt~-vonc ntrs Lion in the waste in 18, 85P.
3_
M
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When developing separating devices an appreciable atten-
tion was paid not only to thy, 7:,t" r *f existing packing sys.
tam efficiency, but to the creation of new ones too. Considering
that column, with large diumaters (more than 30anm) actually
eammot be pro-flooded, new paackings have been developed which have
relatively high efficioacy and do not require any pro-fliedi*g.
Packing system , used 1la. exchange dirstillatioi columns
consists of triangular helice layers with the height of each
layer of an order of Icy, and capillary gaskets, which are
strips of a twice beat metal gauze /6/. Over each helice laayec
6...6 gaskets are placed. The witth of each gasket is 5 mm, tbs.;)
length is rather loss th.aa the column diameter.
The offic.ieccy of this packing system has been determiued
at the complex distillation in the columns with diameters k?,
74 and I28mm, The KETP values obtained are shown on the fl# k.
4.Tn BFi dJ stillatlag columns a cap-type packing is applied-0/',
The elements of this packing are caps with four sharp to)tb;
made of metal gauze. They are produced by pressing the
of double gauze through the round hole. Pro-floodisag i i
jd o'
required.
The figure 5 represeitts the depeadance of efficiency
on reflux density when operating without pre-flooding for
cap-type packing and for triangular helices with gaskets
aad without them.
The HFTP values have been obtained in the column
with the diameter of 94 mm by means of benzene-carbon tetra-
chloride standard mixture.
The curves in figure 5 show that H 'P as well as
pressure drop values are mirilum for the cap-type packing.
Enriched products (CH .j) 2O . B10P3 and (CHg) 20 . B11 F 3
are converted in elemental boron ( apparatus 9,10) . The
latex: it produced by the fused salt electrolysis of potassium
eh zor id't .aCL and potassium fluohorate KBFz1 ;/I/. The
u+,. - outlet is 804. The purity of the elemental boron
98%. Besides the broad ? usin g of B1oF3 in neutron-
?~J
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waste-flux from the chemical-exchange device.
In connection with the fact, that the low-temperature
distillation process technologically is rather complicated,
than chemical-exchange process, initially the chemical-exc-
hange device is provided. afterwards, the main part of N"
production will be carried out by nitric oxide distillation
method.
The chemical-exchanges cascade device diagram for pro-
dueixg 4,5kg of 99?% nitrogen *early is given in the fi-
gure 6.
The diameters of the first (2) and second (3) columns
are 120 and 26mm; THE lengths of the column packing part
are 17,0 and 17, 8m. Packing system of the first column
represents triangular helices (dimensions of the element:
295 X 2, 5mm) and gauze gasket layers, placed at every other
centimetre. The packing of the second column is represented
by triangular helices with element dimensions 2,3 x 2,3mm.
The ref luxes of th4 I and 2 colnmas are 400 and I6cm /mix.
of IOmolar nitric acid accordingly.
The concentration at the transition point from the I
column to the second Ck1, and, successively, the eolnaan
lengths are determined to minimize equilibrium time of the
cascade. The calculation results in the farm of coacentration-
obtailing time C K 2 = 98% N dependanc a at the end of the
second column on the concentration CK,. value at the and of
the first cols * are given in the figure 7. The calculation
is dome for the two values of the first column equitilent
theoretical stage height h1= 12 and 20cm.
As it can be seen from the figure 7, the curve, charac-
terizing this dependance , has sloping minimum in the range of
-values Crt 10-30 %- When reducing C K1 below 5% the adjustment
time sharply rises.
N'~ heavy isotope is produced in the form of nitric oxide,
nitric acid, free nitrogen and ammonia-
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and nitric acid HN"O is intended-
.Ammnonia, responding high requests of purity, is obtained
by calcium nitride hydrolysis. The process consists of -three
stages:
I.Deoxidation of ties nitric oxide to the free nitrogen
(apparatus 9) ;
2. Calcium nitride syathe sis (apparatus 10) ;
3. Calcium nitride hydrolysis (appatus II).
Ammonia's purity in the obtained product is 99,9/'0'. The
ur,a.j or impurities are: N2, H,,, H.,,O.The product outlet is 957o.
On the base of nitric oxide, enriched nitrogen N"-S and
o xi sea 0'g isotopes, the production of heavy oxigen water H .,0
.lass-diffusion.
To produce a whole number of highly enriched isotopes,
needed in sm.a.il amounts, and for the separating small amounts
of material, ~t construction of cascades with 120 mass-diffusion
elements and 30 mass-diffusion columns is conjectured. These
devices being used for 41ong time in laboratory conditions,
showed high reliability and st -~.bility of operation /15,I1-3/.The
main kinds of isotope products obt;.Hi ned in mass-diffusion
devices will be neon isotopes Ne-', carbon isotope
C , argon isotopes A"' , A' , krypton isotope Kr'~ and others.
As an original raw material natural isotopic mixture will be
used mainly. In mass-;.Ii ('fusion cascades reenrichment of the iso-
topes, produced by ch-anieal exchange and distillatiol method
up to the highest coznce:n'c-~ations will be carried out. The output
of each device, calculated by Ne with concentration 95-?98," is
nearly 200gr yearly.
Isotope and Chemical Composition Control of
Production .
Isotopic composition of uh }:curds on the boron isotope
base is measured by two ;n6 t i method and
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nuclear-magnetic resonance -Besides, the samples from the devices
of complex-exchange distillation in the form of (CH ) .. O . BF3 are
measured by nuclear-magnetic resonance method; while the samples
from the boron trifluoride distillation device in the form of BF.i
are measured by means of mass-spectrometer method.
Compound isotopic composition on the base of N 's is measured
by mass-spectrometer method in a form of compounds: NO and N.j18/
The Durity of final products B it', B B'~Fi , (CH`s) 0 ? BI0F,5 ,
(CH3 ),,O-B Fand also the purity of feed materials (initial p'-o-
ducts) is controlled by chemical methods.
Technological Process Automatic Control System-
Automatic control system of the enterprise must provide with
optimum regulation of all the technological processes.
optimization must take place by means of such parameters, as
the concentration of the valuable isotope in final product is,
as the maximum output is, as economy is and so on.
These functions must be performed by the controlling elect-
ron computer, which operates together with automatic optimizer
and electron model of separating columns.
.terpri se automatic control system functional scheme is
given in the figure 8-
The automatic regulation of separating devices and initial
and final products producing devices is carried out by correspon-
ding control panels with the help of sensing elements D, which
controls the technological proce,6ss, and by means of actuating
mechanisms.
The enterprise general control is carried ou* by the electron
computer. It interrogates the sensing elements, after this the
c1.ata enter the automatic optimizer and together with controlling
aachi.ne and electron model adjiustrnent , the programme is worked
out. The realization of this programme is done by means of co-
inraar.d ing device, which send:', necessary commands to the corresponding
panel of ;:utoma tic regulation.
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ToO control the technological processes and automatic ad-
justment system operation serves dispatcher board- Moreover, by
means of dispatcer board the is troduction of additional data
and change of the device operation is performed.
The total system of the enterprise automatic regulation is
realized in two stages. The first stage -- formation of separate
devices automatic control panels -- includes the development
of special sensing elements and actuating mechanisms. The second
stage -- formation of an automatic optimizer , electron model
and commanding device, which together with the controlling elec-
tron computer will make a thorough automation of the enterprise,
At present the first stage of the automation is already
realized -- the panels of isotope-separating processes automatic
control are formed. Regulation of these processes is carried on
by device hydrodynamic parameters. This caused the need of some
questions' solvation,which are connected with the measurement;
ai- regulation of aggressive fluid small fluxes and rela-
tively small gas fluxes; the need of regulating reaction zone
place in the devices, operating by chemical-exchange method, etc.
The expenditure-meters of small fluxes f fluids and gasses are
developed; there are developed sl.Acial actuating mechanism for
precise regulating of fluxes, saturated by gasses dissolved in
them, and other devices. A particular. -.ttention is paid to the
reliability and accuracy of regulation . Electron regulators
are entirely without contacts and collected on the transistors
and magnetic elements.
Fluid flux regulators , operating at continuous,inter-
mittent and quasi-continuous regimes, and also gas flux regula-
tors , secure the control with an error not exceeding ?I,5>,
and the major part of the error is due to the expenditure-meters
(the error of the regulators themselves are no more than + 0900.
The reaction zone situation regulation in the reactors is
done by self-tuned regulators, which automatically choose a nece-
ssary regime for the operation. This provides with the keeping
the reaction zone at the assigned place of roactor at aminimum
number of regulations.
Circulation regulators in distillation columns provide with
keeping the circulation in dependance upon the level of fluid in
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the evaporator ; that permits to carry on the separating pro-
cesses at small hold-ups and entirely excludes the possibility
of evaporator overheating.
Other parameter regulators provide with the control with
an error not exceeding Io /18/.
Separating process automatic regulation system includes
emergency and warning signal system. Involving a particular
importance of signal device reliability a system with thorough
self-checking is developed.
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Cap LIo11n
F:L1;. 1: -- A oiiora1 .L:';f1-1; o.l' n.r'o(lu(;.i.i : I).t i I.dI VI i.Llr r:1 Louver p 1.1- t;.
Cycle ;mf,.:.uro of obt i.rii.ri ; compoia.nci.:, on Lire 1;-1U
~r1cl 1':l:.I b"So"
c1.CV:LCC.
2) BL'' Complex lvVi t;i1 d:imc~ LIB Jl G U.o:v cl.cv_i.Co.
')) WardLo itC'llW.r.'f1.1 j Cer'.
~I) BF-. 1DroducLion device: 85',.'; B1:0 by ctl_:n L L1.1r1tio.n.
5,6) the first and the second cascade columns producing 85%
BIu Ii complex-exchange distillation,
7) 99% B producing column by complex-exchange distillation.
8) 40% BIO producing column by complex-exchange distillation.
9) Tetrafluorideborate potassium producing apparatus.
10) Electrolytic cell.
II) Boren acid producing apparatus.
Fig.3 -- Boron isotope enrichment factor dependence on temperature
at BF distillation.
I - enrichment factor E.103, 2 - pressure, atm. 3 - temperature,
o0 K.
Fig.4 -- Equivalent theoretical stage height dependance on column
diameter for packing consisting of triangular helice and
capillary gasket segments.
I - ETSH, cm, 2 - diameter, cm.
Fig-5 -- Efficiency of different packings at non-pre-flooding
operation.
0 - segments of triangular helices 3o O x 2,4
;
- the same packing with capillary gaskets;
x - cap-type packing 4,5/2,8 of double gauze (dashed
curves relate to pressure drops)
I - ETSH, 2 - reflux density, ca/cm 2.min, 3 - pressure drop
mm Hg/m
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Fig.6 -- Producing cycle scheme of compounds labelled by NI5
I - Nitrogen oxide absorber.
2,3) The I and 2 columns to produce N15 by chemical exchange.
40) Phase-returning system
6) Nitric oxide purifying apparatus.
7, 8) The I and 2 columns producing N15 and 008 by
distillation.
9) Nitric oxide deoxidation apparatus,
IO,II) Apparatus for calcium nitride synthesis and hydrolysis.
12) Water and nitric acid producing system from nitric oxide.
Fig.7 -- Concentration Ck2 98% N15 at the end of the column 2 obtai-
ning time dependance upon the concentration value at the
transition point Ck at the height h1 = 20 and 12 on of the
I column stage
I - days, 2 - molar fractions.
Fig.8 Enterprise automatic control system functional diagram.
I - from control panel and sensing elements, 2 - from
control panel, 3 - unit of interrogation of sensing elements,
4 - automatic optimizer, 5 - electron model, 6 - controlling
machine, 7 - dispatcher board, 8 - commanding device,
9 - to control panels, 10 - to the unit of sensing elements
interrogation, II - separation umLit No.I, 12 - control panel
No It 13 - from sensing elements of separation unit No 2,
14 - control panel No 2, 15 - to the actuating mechanizms
of separation unit No 2, 16 - from sensing elements of
separation unit it 17 - control panel i, 18 - to actuating
mechanisms of unit it J - sensing element 9K - sensing
element of isotope concentration, BM - actuating mechanism.
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Table I
D& tce 'aZarneteZ3 Z`o Pioa~uce Bozon
sotopes
devcce
exc~iczr7~ 5 tj
c~c.s'ti'~t'c
d T&
Zion
8F3
.99/; B1
~fe&ces
3X30/"
~ eCice r
3,2X2,9M~,
titan
ifeC(cer
3,5 X-30Mr,