AN ABSORPTION METHOD FOR THE EXTRACTION OF KRYPTON AND XENON

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP82-00039R000100100055-0
• Release Decision: RIPPUB
• Original Classification: C
• Document Page Count: 20
• Document Creation Date: January 4, 2017
• Sequence Number: 55
• Publication Date: January 27, 1951
• Content Type: REPORT

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Sourco = Ruas~c~n mon~l~,y norf od~.oal~ Obahoh K'hlm~ Vol IX~ No 18,
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~~AFt T~l~ F!~'PR~AOT~Qt~~ Q~ K~CP'~i~ A"~1'0 XF~1aN
A~1 A~~oRPT~bN NI~T~IQp
Pam
V. 0~ ~'aotovck~y,
1n~a of faro raooo,
A11�Un~,o~1 ~loatrA"Toch In~t
~u~u~~~tad 19 Marah 1939
~ tOr~ r~.r~~l xo~t~a~ k1~V@ ire xo��nt
ThA 'r~tx'4p~i 0011I~Ol~~~tt~ 0~ ~ftA ~ ~~1~ ~o~ ~l~a~r 1~~~~~1 atD~a
rra ao u~ raid tr~~m~~~ndou~ pr~ct~~.c~~1 impo~~t~ ,
yAa ~
?k~�t ~no~tc~o~o, 1ow h~a~ c~n~k~~c~t;tv~ty~
wb~~a ,
~ �~ccku~oloI' off' ~~~~~~~a~~or~~ o~ w1~~,ah
Tkj@ rol~n~kf~~,1~a ~;ro~rt~~ o~ ~k~~ o0 oro rinc~pa~ly broad, ~tr~ �~~0 1~~u1
tklo hJ~~ro~on n~f~ ~tro~on infl~aotr~ r�r� uloitoo ~'o~r ob~~a~nin~ krypton
~~c ~L~vo or�a~cd tho p ~
~'nc~~an o~ ook~n~, ~ ~ ~ ~ ua~~~~t~oo, ~n~l tt~io k~~c boon w~doly rQ~
SKr) an~1 xonor~ ~X) �~~;~i~~.cat? q
~'~:octa~l ;tai pr~c~~:coo uoofa zbroo~~
~ct:~on off' ~r anal X From air (k~IOT~~: A K1eo"~
In tha procooo off' tho oxGr tl~e i~oun~~o o~ tho proccn~ ropor~~ oqr
car�J. ~lon o~ th~,� procoeo ~s outia~d� iri amo~~ta o~ 0.1 ~~0 0~ 3~? c,nc1 to"
p
pan io obtain�cl w1~~ck~ cot~~a~nc Kr and X oo tk~~:o oKy~!cn, ~~tk�~ict~ wQ ro~nr
~ ~ ~~xturoc off' ark f
~othor w~tk~ ~n~~~~!~~;tic~t~t n~'~m,
' a rortcnntrr~#~c, cryrt~~r~~knr~ ]:OGb"~OG~? ~,-~rnr~;a ac? i,~ttG t
�~cco~~~ co
to :t.n t1=~o o~~ou~t~{
Kr nn~t X r1c �I',lio ak~r~~,~~,~k ~~~1 i~o~,
' cor~cean~r~hc ~:nN~o ~,~~re Kr panel X ro~rosnnt~ a
Tk~a r~~r~CA~~I t l'1~r 4~' ~lt.~o
~tm~ ~a cot~co~.v~til,~,ti ~Eo u~� thrj m�~~kio~1 n:t urn
ccrl~o~~o tnchnralor?,;~a~1 l~ro~?1 ~ r~.nr:l cubot~cl~~cn~~ty o~par~ting krypton and
~n~r k7;rcl~~a~;cn ~~rL~h ~hn c~n~;on�'J~n~�~ 110T~s Wo aro devc'~op~.n~ ~I, mo~~l~ocl of
on' from tho c~~ml~uot~,on prorlv:ctc ~ ~o~thod o~ c~boe~aont r~'~otiltia-
~ce~ 14 tho ~
~~k~1o t;~o~ I~; occm~ t7oc~~~~b~~o to o`~o o~ obt~na ?~,n,~ a l~~u~.c~ phr~ac dt~-
,ti1.on o.~ ~k~n c�nnon~~~x~~to w:l~h tlta ~~ua~
r'iohorl ~.n k{~~ ~~d X)~
~ t~s~y~ia_j1~; ~~r~.ct~y pr~at~c~~. ~~~ni ~p a~~
Tho prdonn~~ ~,nvns~~.~~,aL.~a~~ ~ ,rncoao~.~~~ o
.t ~ l~~ `1.3:`~~:E~~y x?r~rl ~tlc o~t~mu~n co~~dlt~.o~~g ~nr _llc~ rod
cc~r~,h~:r~ ~,l~n poo.~~.
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h~ aa~, o~ ob~a~,ni~~ tho~o
~ the nd~Qrp~ion ma~l~or~ w~.th ~ ~
t~~a cAr~aontxa~t ~
a~o~ (Kr ~d '~I~a p~'o ~a~ d~.~at~~y
aoib~a to ~~o~ too Q9~~~ aonoontr~ o
prir~aip~~ ~u'i~~ Po ~,~h Dome
umn thrau~lr nn ~,~p~r~tuo ~~~1od
~@ d~s$.~~~,~~i~An 0~ W~~hing RQ~
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fax the ~urpQOO A~ a~~o4t
' ~~~cor~ont (~o~ivatod earb�r~, e~~io~ ~
ka,nd o~ ~ ton ~d
h�boi~,i.n~~ haav~ oam~onontc k~`A
tantion by ~~loarptiAn a~ the hiG
i~~ ra to k~pton~ a~-
c aooount wo w11~ razor only`
a~~on (P10T~s ~n `~ha ract off' 'phi
~ io~bla to
to kton aro d@~'inite~y app
thAU~h ConQ~u~~.0~~ rQ~~~i~t~~; t~~
ca ~~~ra~~-o~~ a~` ~a~oouc ~?~~uroc
anAn) ~ ~ a~~r~.'lar iar~t~aod ~o~ ~thc ~ oh
. ~ ~ cc1 c?~~ ~~~a walk-1Gnow~ rai~.ti~at~ rrh
acl of ~r~c~~ic~nr~~~ ~~~oo~~~t~o~~ io boc+ ,
r>:~ot~~
. ~ ~~i~~ ~ir~t~o the ao~~~or~or~ts a~ t~~a
~ ~ ba o~~r~tior~so~ in t1~~a ~o~.~~~~,~~g n~at~~?or
scr
o . ~rc~ri o�>.a~~ ot1?or cc for ~s their p
% u~ x~xt,uro ~~o ~,Q ac~~cr~a~,ocl c1i~~ r ,e
~,oNoo atomic, woi~~~t)
. ~j - bA~~~~~~; ~,oin~, o~~i~,ioc?~: ~~,a~,~:~or~~,~~r~~
icsl p~io~c~1 ec ( ~~~~~~ura~ T}pis
d oifi~~~atic?r is t,o oc~~~ar~r~i,e �uo~~ a
conoo~`?od~ thr~ ou~ioz ~ri
. ~ ~~,in a p~asoo~~c mixture, i~~ cleo con~-
vt~ ~~r~le ~'or ru,~,~ ~it~~`~~~ocl o~ set ar ~
r~~~,cti ~
~1,ic~ol~~~e to ~`~1`~� c~e~sor~y~ifyrt m~thod~
~~iota],y aP~
cl a ii=v~oti~,Ectir~t~o on t~~a aclsorpt~otti
.,a.po~la ac~cl ax~tiremel~ :~nte~ o~t1 C
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. t, an carr~.ed out by K� Petard and K�
era ase� by aotivc~ted carbon hove a
o~ r ~
� ~iir~atf or1 below. We rr111, note ,
1ti whose ~rorks we sha].a~ stilbn~t ~,o e,~a
ire ~
ha method of f r~~Ct`:>; r~rigl adsorpt~ d~~ o
ars anc~ W. Lom~~.~, C'~, ] s1~c>~,au~, su ugg,~~4~ ar~~� ~~n~
-r~,dtitia~ hea hg ex'~exi.
cep ~ the ~
g ,~rac~?i by �ra~~~"g~ T
Th be carr~,ed ~s~~~ ~em'~ 6 ohm
Quad a C
s4x'~'~~�n sh adsorb'�n~ a hers ~'d
de o~ the ~e
Y: e~acua~~,nri ~ ati~s o~
Y~ ~ ~h� ~hg in~c s~ g
`F`A r ork and
ncs o~ ou ~
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1~
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kn tk~at tho p~~sonao o~ ano oo~~~o o as an �~'#'oot or? tha ammount off' ad-
s4rp~~Qn off' anotx~or oanc~aonant)~ adoorbont (aativato~i aarbpn~ oii~aa
dot us attom~t to oluaids~to the in,~'],uQn~o of esoh of the faotore er~u-
rr~rat~od~ T'raotic~~ ail�orpt~ior~ is in oooar~oo thA p~~ooing of a ~aoooua m~x-
t~~ro oantinuc~usly thro~lgh a~~ ac~oorbont and ~uk~aoyuoxltly doaorbing tho acl-
AorbQCl portion ot~ tho gAO~ ~~'rctm tk~o onginAOr~ng and praduo~tic~n point of
viow this mot~~A~l is o~ctren~�~~ a~~traotive, oir~oe with a �uitablo systo~~~ for
awitohin~~ ov@~t tha linos it i� poaeib~:c to proc~uoo a oo~~tir~uouo flow of gas
with an in�ignifia~t c~uant~~t~? of adsorb�nt~ ~or~evor, o~~oh a procooa of
c~r-
n~j~io adaorptic~n oan load to a son�iderabl~ 1,oae of kryptan, for tha highor`
~~�ic l~o~li~~g paint o#' a oomponent and tho lowQt~ thQ tQmparature of tha ad-
sorbent, tho longor thQ timQ neo�osary� to r�~oh adsorptiean �qu~,l~,briiun~
2n tho ~�r~vestigation of tho aesorption of rare gases ~5~ we had the
opportunity to satisfy ourselves that in a given Comp�raturo r~~n~;� ttie ad-
sorption equilibi~um for helium anc~ neon is reached vary 9u~.alrly~, wliil� ~'or
hQ~~vy raro gases the process oontinues for a long timQ, `this circwnstanc�
in tha use of dynand,c fractional adsorpt~.an ragti~irgs a very low velocity of `
gas flow, sand this iq negativel~r rafleot�tl iY~ the dimensions of the adsorp-
tion a~:~paratus~
Thare i,s no doubt that from the po~.nt of view of reducing losses of
krypton it is preferable ~~o use tha method off' fractional desorptian~ the
given adgorber ~s saturated up to a certain pressure with the conc�ntrate,
and then the process of fraational deaorpt~.on is acoomplish�d wt t~~ a vacuum
pump. such a method, when the correct thermal oond~tians are c~~osen, not
only perm~.ts all the ox~rgen and argon to be separated from the adsorbent, but
r
also permits the residual gas (Kr and X) to be t~!:ta~.ned in the pure form,
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w~,thout substent3al losses,
' ~ ~ The praotioaJ, uestian arises as the whether the recess of fr~.ct3,onal
q p
~1 desorption should be oarried out by the gradual heating o� the adsorbent or
bar the evaouation of the adsorbent at a constant temperatut~e~ The expert-
~ sees of our work and the investigations of K. Peters and K. weld. ~6~'' show `
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 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100055-0
o~do~ tQ Q~~'ao~ivo~.y s~~~ra~a the ~a~oou~ r~~tu~ cud o~tai~
~~ypto~
d xor~o~ in too aura ~'or~n tho a~~orbe~ ~l~ou~,d ~o ovaauated the ~oloc~od
~deorptia~ pro~euro (~oa bo~.ow) down to ~ ~it~~~ ~,ow prec~ur@ ~d th@ ro-
ei~~u~ ~~o sop rated by hoa~ir~~ tho ~~lsor~ont~
Tt~o to~~paraturo Bator is off' deoisivo inportanAo ~'or effective ~Q~ara-
t;~on o~' the ~aosou~ ~,xtu~~e by the adsorption ~thod~ ~nvosti~atior~ on sd-
oorptian of uses s~~oris that within ~ spsoi~'ied temperature interval t~~e ad-
sorption takos placo r@versibly (not in tho t~,arr~odynam~,o scnao oi' thA wok),
i~o~, thA cutwos off' adsorption anal desorption fury ooir~aid�~ WQ oanduoted
si~~~ilar o~cpori~?onta with h@~ium anal ?~eon at the tompordturo of lic~id nitro-
gen; ~'or holi~~n tho adsorption anal doao~?ption ou~~ras w�re fully ooinoi~lont,
but for noon Choy oho~rQd an insi~~nii'ia~t c~iver~enoQ~
Tho fact that tl~o process takos such a course dopriveD us of th� oppor-
t~u~ity to saparatQ the individual fractions in thoir puro form in th� de-
sorption ~7~~ ~�~owev�r, ae the researches of K. Vetere and K. Well 6
s~iawc~c~, t~ioro is for each tae a eo-c~led ori~,ica1 temperature of adsorption;
bo]=ow this tor~perature the adsorption ~jr~ desorption prooasser~ do not pro-
oe�d reveraib],y~ This ar~.tioal ten~parature of adsorption has a phyeioal
si~nii'iaanoe which c~~,f
f�rs 1~,t~;~,Q ~ron~ th� ordinary cr~.tical ~~en~paratur� of
a liven has
The facts stated above pernd,t a very important practise/ conclusion to
be reachedt if the process of adsorption of a ~aseous~ctv.re is carried
out at a temperature lower than the oritica~ temperature of one has and
higher thAn that of a~~ot~tar, i,hen in the subsequent desorption pure i'raetions
a
wil]. be oapablo of 'be~.n~ s�paY'ated in a single operation :j
Thus K. Peters shored that at a tQ erature of *~22 �
~ ~ (the cr~.tical
temperature of neon is �228. y a neon�he~.~.um m~,xtura coti~ld be completely
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separated without the formation oi' intermediate fra.ct~,ons contain~g neon
L
and helium in various proport~.ons,
1
Thg considerations cited have a direct relation to the mixture we are
interested iry (the concentrate consisting of 0 , Ar, and Kr ~ In the
~ 2 ) g3.ven
case wo d~,spose of a e~,Leab~.e temperature interval the c
i ( ritical temperature
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+ ~ I ,m. p n Arif t,~r ~
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' ~

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of kypton ~o �63~ While
thoeo of ~Ygen ~d argon + ~spaotive
which a f~oil~tstao tho ae
and p+u~ati~ of taa
~ to a etil~. groater oxtont
of ~conon) ~n a atato� ~n tho ~
when is otated ~t of
abovo ~t is oloar that t~~o proooea of
+~QOrptior of the s~.
taste wi~a which Ka aro oonaoxnad must b
0 oarriod out in the temporaturo ~N
Larval boated boloH the oritioal t�
~aperature of kr~ton a~ �o~what abovo
~o oritioal tamporatwroo of 0 and ~r�
~ zt moot b� noted hoNOVer~ that un~
~tQ the or~n~y at'~'~?i0~, tel~~~~'a~,t~+o
tho oritioal t�n~poraturo of adeo
tion~ of a g~Yer~ gae ie o ~
n moans a fixedi onob~ ti
g gaan ty~ but depends
on a conies of aa~plex faotors~ the ohnraater
of the aurFaae of the adeor-
bent~ the method off' its treatment and
, tho nature of tho other comporiastr of
the gaseous m~xture�
Thus K. Peters ['e,~' ir~troduoeo an intone
o~ et3ng example, Tha inveatiga�
tip ref�rrod to euooaeded in deaorbin at '
g 0 the 3~hole quantit~r of adsorbed
Prime, while in the Following exper~anQnt t~~ere
wse adsorb�d the same qua.
City of
propane ad well ae a oerta~ asst
~ ity of butane. tt appeared that
in th� subsequent d�eorption th� whole
ga~tit~ of propanQ was separated not
at 0� ~ but at -10� ~ and even at �20'
gene the more vo~,atile oomponent (pre
pie) was die~~lacod from the adeo tia
~ n surflaoa b~ the less volatile, and
this naturaa~r resulted ire a shift of the
oritioal ten~er$ture of ad~aorption
oS propa~ae~
In the oase with which xe are concerned it
ehov~,d be expoeted that the
adsorbed krypton w~,d contrfbute to the
c~eplaoemen~~ of ~r and 0 from the
adsorption su~+Faoe and would t ~
hereby faoilitate the ddsorption of thes�
In the separatian off' a gasee~
gaseous mixture by the fxaotional oondensation
or fraotional evaporation methods the va or
p tensi ens of the component s of the
mi~ctus~ are of b ash, c impor~;anae ~ 8 analo
Y when the gaseous mlxtti~e is be-
ing separated by adsorpt~on~ the pressures
aver the adsorbent (the unadeorbed
phase) which correspond to a v�
6i n value of adsorption (isostero) should
be
compared for a sari�a of temperatur�e and
tho components of interest to us.
In Table
4 are cited the respective dat$
From our exper~,megts for adM
sorption values equal to 2~ 6, 9, ar~d lz
ou cm of gae.
It is evident that the stet
gre the ratio of the pressures ~ the unadw
Sorbed phase~F the o
omponents ~ioh are of interest to us the m
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ry ! 1 wlr~ ? f
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w~~~~~
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i~ r 1 t.} ~ t~ ~ 4
i ~ pfi r !i t~ r
r 1 e^r p~d , t r{
ii t i
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'ski 1
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~~V~~'~~~a ~~S Q~~rt~~.~~~~~ fq~' f~'~A~~,4~~ d~sor~tior~l ~k~~~ i~~e~~ ~8
aa~~ad by uo too ~,aat aoz~ o* ~~b~a
dot us Hots that sear aa~,au~ations worn oared out by Aators aid
k~~ We11 b for the rasa of the adsorption of ~Cr, and Ar ~y aotivatad
oarbor~s irr pr~,no~.plo an ann~a~ot~e d~~.roatian of t~l~ pro~o$s was shy
Ao io ovic~ent frn~~n the data oitar~, ~oc~orin~ o~~ the �~om~arat ar~d rem
duotion off' tho nude o"~' adsorption per unit oi' adsorbont ir~prove th@
condit~~ons for thQ soparr~~ien of tho gasoaus rn~,xturo, burl in tk~s oaao tho
rooiprooai in~'`lucnaQ o:~ tho aor~ponont� of tho miacturo on tho adsorption
proaoso wao not takon intc aAOOUn~~ hortQVOr, irr adaptic~~ tho pros�as for
pro~~uot~.on onA shou~~l not prooaed along tho 1~:nQ of the rim~rm laworir~~ o~f
ternpQra~uro an~~ v~aQasivo ~.nbreasin~ of tho quantity of adsorbent, for this
wild, lea~~ to ~ a~trem� rotardatior~ of the d�sorption prooeas, to oxoeasiv�
loading of thQ adsorb�nt frith adsorbed 0 acrd Ar, and to a oonaiderabl� in-
2
o~~eaee off' thQ inaotivo spac� in thQ ~~~pa,ra�~us, a1a. of which is undesirable
far operation w'~th rich valuable geese as krypton arrd x�non~
We assu~~� the�b t13� opt~~mum ~tarnperature far the proooss of adsorption
and su~~sequQnt desorption rmtist be taken ae -120 to -130�
~'he influence of pressure on the ra~~io o~f the oomponents in the ad~
corbod p~rasa is preson�~ed in Tahle which we compiled from oxp�rim�nta7.
t~~t~~
~al~lo ~ was made up for a t�inparat~re of -100� ~ As is evident frorY~
tho data c~~ fed, loWC~ring off' the teinperatt~ra increases the r�~,ative quantity
of krypton in the adsorbed phasA; it must be expected that ~rhen the mixture
is adsorbed the ratio of the components in tyre adsorbed phase givos more
favora~~la indices for l{rypton with an increase off' pr�ss~ro~
~n F3,~ure ~ are shown the isobars of adsorption oi' Kr, Ar, and 02.
From these curves, bes~.dos the temperature dependence of the amount o� ad-
so Lion it 3.s possible to obtain data on the ratio of components in the
~ ~
adsorbed phase for a liven isobar (800, X00, 200, ~0 mm ~Ig) and for a given
' '
temperature� '
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 Declassified in Part -Sanitized Co A roved for Release 2012/05/25 :CIA-RDP82-000398000100100055-0
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