TONIC EXCHANGE IN FRESH AND AGED HYDROSOLS OF ARSENIC SULFIDE

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP82-00039R000100100030-7
• Release Decision: RIPPUB
• Original Classification: C
• Document Page Count: 16
• Document Creation Date: January 4, 2017
• Sequence Number: 30
• Publication Date: January 10, 1951
• Content Type: REPORT

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BIND ACS ~n~090I~`` 4r ARS~'NIC SULF~E
Titl�s IO~LC EXC1~Ari4E IN ~N
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bimonthly ~eriodic~l, ~arch~iAp~i1
gourca: Kolloi Zhurnal, R~�~ian
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ONTO F~C~I~ TN ~D AGLD HTDA080L8
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Or NIO BCL~D~
8y A~ N~ Khari~a
ionio exobange playa an important past in the etruotural
As we know,
er of mioellea and, in oonneotion therewith,
ohange of a binary elootrio lay
olloid solutions ~ T n the bi story of ba1~ a oentury
in the stability o~ o
it is orsible to Find very dif=erent viewpoints
of study of this problea~ p
lee overning ionic exchange in sole of areenio eulfido~ On ~nY
on ru g
es offal that o! the equivalenQe of ionic exchange, authors
problems, Pe ~
� o!`ten contradict each other This impelled us to take up again
ll 1e.7
io~io exchange in the As 5 sole ~ while taking into account
the study o! 2 3
terial already aolleated on this aub~eot ~ 1n spite of the opin-
all the ma
t a we showed in our article 119)
n of various authors 120, l? e
io
ous said discovered in As 8 sots can never play the part of a
that arsen 2 3
As 0 in water have a high pN value (of the
strong said ~ 8olutione oT 2 3
aid content in them cannot be determined neither
order o~ ~�b)� The tats/ a
b otentiometrio titration north alkali solutions
by oondt~otometria nor y p
h t acidification of aged sole (and the
and hence reference to the feat t a
ultrafiltrates) depends on arsenous said, contradicts .
acidity of their
N
the data obtained by us on the properties of arsenous aaid~ Seaause o
rooesses
insi nifiaanoe of the aaidia properties of As20 solutions, the p
a~ ~r ~,r.
the 6 3
Y'd
~t
.min arsenite precipitates, for exas?ple by the equations ~NArO~ ~
for for g
~ x
~8a Aso 2~tC1, ~aeem rather improbable to ue, since it would be fie:
~8aC12 ( 2)2
ve weak areenaus said could, to an appreciable
r dif f fault to admit that a ry
low value ~e 3, displs,ae a strong hydroohloria aaid~
degree, and at the
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Declassified in Part -Sanitized Copy Approved for Release 2012J05/25 :CIA-RDP82-000398000100100030-7

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l~or the additioa at ~ o~~ of a
Our oaperi~ont aonfi~ed our opini~on~ A
1 to 100 0~ of a solution of ohea~
O.l N solution of BaC~, CaC~ and g0 g
io~tl a Ar 0 ~~0 m�~l~l~ hot tho e~gh~et turbidity war dirooverod~
23
Still lore oou~d arsonite preaipitater be forded is aoid iattrmiooller
dr of AR ~ rols~ 1lhat strong aoida appear in aging AsgA rolr~ Wbet
fluff g ~ wh ~
~ t number of eorbod
oom Boater the ionic exchange in Ar 4 solrg~nd it ho
p 23 ti
o the numb�r of H~ lone forded out of the ~oello~
cations equivalent t
These wero the special gaeetionr for ~hioh we rriehed to find an answer
in our work
l+~thod of Freparing and 8tucng ~s 0~ $
the Aa S sole sere prepared in the usual w~~ by passing HZS throng h
23
le distilled Asterwith o specific electric oonduotiwlty of (x)
doub
l�2'10�b mho at 25�.~ while adding si~lteneously an As20 solution sat-
3
fed in boilin and cooled to various temperatures ~ The surplus HZS
ura g
f b dro en eased through an alkalized solution of K1~04,
was blown of y ~Y g p
o ntratod H S04 end through 2 Drexel fleskr with distilled
through done 2
watery Hydrogen sulfide was obtained from Ferrous sulfide by the action
k,
of sulfur3o aoid end ~eghed through 3 fle~sks with doubly distilled weter~
re As 0 rrhioh did not
In As20 solution ass obtained from o1~mi~oallY pu 2 3
3
e dirt~nt after bein heated on glass nor contain As 0 [19.7.
leave a e 6 2 5
A
1:
~ Sol g was prepared with surplus As 0 ; it did not have the odor of H~9
3 3
and was not blown off by dydrogen~ 5ols 9 and 11 (with some slight HaS
residues are prepared in large quantities in 1~ lit�r flasks of Pyrex fi
;r
lase steamed after boiling water in them a loag time ~ ~ They ware kept k
g (
in these flasks closed with corks, in contact with the air. over them in
tho retorts Theso sole mere studied, both be . fresh end the abed, u~ r
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 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100030-7
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~arioua oonditions (Table ~ The ionio exohange in theca wad studied at
the eamo tiao
Det�rmination of the oolloid As 5 was carried out after coagulation
a3
ml o! droohlorio avid sol as deaoribed in our artiole ~19]~
of 100-~00 1~? r
The artiole aloo de soribod other methodo ueod by us in studyiag sole ~ the
determination of oonduotivity (at 2~�), oonduotoaatrio titration of soli
and ultrafiltrates by alkali (at 2~�), potentiomotria determinations Kith
glass ele~trodee~ a method of ~repari~ng ultrafiltrates and obtaining
ultrafiltrates (always reduoing the wolua~e of the sole two braes) ~22,].
In addition, filtrates were studied after the ooagulation of (x0 cal) Bole
with hydroohlorio avid (or pia 4l) ~ their were titrated by a 001 N solution
of iodine to determine the e~betanoes whioh reduoe iodine in an avid
modium (N2y, 90Z and others) .
To determine As 0 ~ the avid filtrate was blown off with air (to
~3
eliminate K 9~ eto) and, aft�r adding eod~ium biaarbonate~ we titrated it
2
with the same solution of iodine (sometimes we used the grdviraetric method
of oontrol)~ Besides we tested the filtrates for their we~05 content by
with HNO and (NH4) Mo04 and other methade ,~22�~~ and for their
boiling 3 2
o bionic said content (coagulation through the aotion of NANO) through
p ~ 3
the aotion of AgNO in the preeenae of HNO when heated (after previously
3 ~
blowing off the S, if any Nero diacoYered) [l~,], Finally, after the
ova lation of 100 ml of eol with hydroahlorio void, the d0~rin filtrates
~ 4
was detercained by aotion of 9aC12 solution.
Charaaterietioe of Fresh and A ed dole
dinae we had alrea studied the first stage of char~gee in eats x'19),
c ~Y
the moat interesting question now was what beoame of the sole in profound
ohanges ~ It was espeoially interesting to ascertain what free strong acids
were aooumulated in sole in aging, together with weak arsenous said, whioh
~ appeared ae a reealt of hydrolyming Ae 9 , thioareenaus and tbioxy~reenous
~ 3
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jthe {~!'Era~fl rn C~ramS-�- Q.Oy09 - oyoq O:o2ao Q. ~$9g D. p3~~il G. o~aZQ o�~i/~~ 6�~~7y ~ 3 ~
E wl~br.u.~m CCnCer?- /~'L

_ ~ra~W~'1 6f ~d~~M~{f~ 3.88 ~.7c3 ~ 77 0. ~4 ~.1y c~. I c7�~r~p 79.9=33
rr,- ~c~u~~.2 a~ sots � ~ 3, 6,as 3. 68 3.77 S,'~6 3. 3`f
~n sots - - ~ 32 j /�31 1.2g SY 66 /z 27 23 0. g6 4. 7s ~�2C o,7'f/ 6�~/ D. 67
~a*rt'~M9~')eornbmed
',1n ~nterM+GCIFerY F~e.�d
,o~ sors ~,-~q~,
j.~ aT a o O o o� 67 0 0, 05~ o o, 09 0 0. y6 o f =S/ o
sots---
~,~~''(N! ff sorbed
6y ~~~t,i~s..-- 1 /.32 ~ 3z / 23 /.Sy 0.99 ~.~2 x.23 1.23 o.ez x.76 0�8o a. 7y e-?o 0.6~
RC~dify a-F Ftltra-E'es
m-eg~.~ f1 0~ sols J ~/3 h 39 ~/9 63 6 3 32 /-28 D� 8Sl p_gg /3 /./3- 6, 051 6.11
Rcrdrt e~f Ul~tra+~ Itrai'
~,-e9~.y/.~ m~ ors . _ o a. a6 v.ob ~�ob a. So 0.50 0. ~3 ~3 r~.:3 0,,3 6 2~ 0 2~ s 3! 5 .fir
"f#~~a~~�at.o~�o-F so~s.a /6 ~ ..1. 37 I~~j - -
rn.u u~ wa-
- -Fr ~~rs~.ts.
~~rIA~ the5~e roncentrart'iw~'S t6~ eaa~cn4itlan o~ 17~a s'ols was no'r eomplete~ In these ~xsf6e 8 ~9
~s e a second anal sus o� foo+^~' a ~"il~;~r-ale '~rom ~
~f" ~E- ~'aR'~ro{ cJ~s eacerG~St3d from ~OrnL o~ "tote ~~~~rd't2 or, et tern S~ ~ Rn~xrtLLr~-
~i~;*t~ ~ilY`~4.~~~~.
- . - - C:3~':i i~ ff
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Figure 1 ~ Conduoto~etria titration curves o! ao19 ~?ith alkali f
---1�--aged soli ---o---aged ultraliltrate; ---x--- fresh eolf ono
:
/rash ultraliltrate
Table 4
Absorptions d! Chlorine Aaiofle by Ae29 Bole
3
901 ll (7 days)
_ _
n , 20 0~..of ZO om3 0!
Added to 200 on~ o! sole 1 7 0~ of 0 ~ d
~ a~ o~ ~I 9e NC1 NaCl
Clz p.l N 0.1 N
Original oonoentration off' Cl-~
~.�qu~,/1 3 ~ 00 10.00 10 ~ 00
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Equil~bi~um oonoentration o! C1` 3~0~ 10.00 ~ 10~11~
Absorbed Cl- +0.08 +O~10 +0~11~
' Original oonoentration o! free acids
- i 1 of sole 10.13
is m equ
Equi~brium~ acidity o! sole ~ !i 10 ~ 1!~ !
~ + , 'i
Absorbed H o! ions ~ 0.01
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,Declassified in Part -Sanitized Copy Approved for Release 2012J05/25 :CIA-RDP82-000398000100100030-7

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,,o tho Re at~t,,,,~t
Tt is e~dent ~ro~ 411 these da
~ Ott by iatroduoing up to l0 m�
equi ~fl oP berio� or ~6naaium ohlari
des into fah aola, the quantity og
'orbed oatioAa oainoidea eitbin the ra op
~ aoouraoy of the determinati o~
C4AA~'oximdtely ~ O.l m�equi ~ ~ with t
he 4oidi~,oation oi' eola o
with the other, end, as the avidity at the u
ltraliltratea Trom !yeah pd, a
is vory alight, also pith the avidity oi' the !il
traty' (and sole j a'e
=Ti~ble 2)~ This is identiosl vith the obeeroat
ion~a o!' ~ebinoYioh j,~]
and with t~,e earlier observations o! Whitne and Ob
Y er
Obviously suob a r�eult ie the oonaoquenae off:
1) the ebaenoe o!
t~ oombining of oationa in the interaioell !1
arY uid o! /yeah sole and 2)
the abeenae o! ~~moleouler" adsorption oi' ohlorine
s on the eol mioellesf
Yn these oases a oleer~y expressed ionio exohen e
B takes plaoe,
unoompliaated by ashy other proaepae1di kith a uel conv
a entrations o!' salts
exoeodir~g tt~e oonaentratioA oP ooeguletion, a reotio 1,1:
p e y tots/ displaae-
ment o! the ~I ~ ions lromf the mioe1les ~,s obae
rved~ If moleouler ad8orp-
tion of the ahlorinea takes plane, sn a uivelent
q exvbsr~ge is not obeerveds
besides, adsorption o~f the C1' ions should be ob
served, +whioh veanot be
eetabli abed by divot ana~yaes o! the
filtrate�~ This aoinoideo Frith
the observations of Kergin j17,~, 1Phitne end Ob
Y er ~2,~~
In aged cols the avidity o! the ul
trsfiltratee is more marked then
�a,
in /yeah sole, and the aoidifioatian
observed on adding barium and meg-
nesium ohloridea is less The tots/ _uenti
9 ty of absorbed Ea ie vlos a
to the avidity of the liltratee (end sole but f
the quantity oP absorbed
Mg'"~ is always lees than the aoidit
Y oP the filtrates (and sole) rind
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leas than the absorbed 8a
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 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100030-7
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s di!lorenoo in slightly aged cols (io the dark) is dot very groat
Thi
tt~e me order as in the ox ria~at a! Xar in ~l7�]~ ~ bit in the
~o! sa ~ 6
greatly aged ~ (in the light) this dit~`orenoe is vary great. It is evident
from Table ~ that g~~ is never oombined in the intera~ioell'ary /laid o!~'
d
aged sots, chile Hai; is alr~ays notioeably aombined~ I! this quantity o!
oombined 8a'~'~ tone be taken into acoount and subtraoted from the total
quantity a~ ioae absorbed by the col, the dil~erenoe in all oasos will be
in good agr�ement both with the ~aaidilioation~~ and with the gaantity a!
sorbed magneeiu~c ions ~ In our obeervatioaa, oarried out on old sole, the
ruled obaetwed by Kargin ,~17,] and partly oleo by fleiiex 1"13] appeared
very ole ar
It is not di!'~'icult to understand t~;t euoti results depend on the
presence o~ H SO in an intermicellary fluid o~ aged cols. The quantity
24
o~ barium oombined in the intermioellary t'luid is in good agreement with
the quantity o!' SO�' in sole ~ In sol 9, 0.6? m-equi ~/1 Ha+~ is oombined,
4
as~d SO�� oontent in a ao1 ie 0~5g m�equi~/lf in sol 11 (et8nding in the
4
dark) 0.1,6 m�equi ~/1 of Ha+~ oombined ar~d the S04� content is the same;
in greatly aged 801 11 Ha~~ 5.51 m�equi ~/l is oombined, and the SO�� oontent
in the 801 is ~~65 m�equi./1~ These resalts mean that the Ba~~ is ooc~-
bined in the intermicehary fluid only in the t'orm BaSO~~ In the ultre~-
liltrates of aged sole ll and 9, on adding 8aC12, a sedimont is formed
whiob is not soluble in ~IC1, but on adding MgCl a sediment is never i'ormed
2 i
T sag g
hi tees with our reason got the sli fitness oi' the probability of the
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formation of insoluble arseni.tes in aoid solutions Areenites whioh are ,g
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ca able of being formed in small quantities, obviously, ors. also not absorbed
p
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completely on Asz33 partioles ~
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 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100030-7
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t be a haeieed that ~ on ad~ng 8a01 to aged sole ~
To eu~ up, it ague ep g
eaoha a o~ ~ ~ and 8a * t lone ands eeaion~,
there takes place ~ #'iret ~ an ~
ith ~ SO in the inter~ooYlary ~luid~
an interaction of 8aC1~ w 2 ~ ,
oe the avidity o~ thO eol ie dotermined only by the sum or the
din
brio avid abut not by areenou` avid) ~
eioollary ions and by the tree eu
d? e~i~e~ i~ltii oorreeponde eith the avidity' oi'
~
d tt~e filtrates Srom them obtained a#~er ooagalation eith
the sole ~
ions with 80" ions yield a ealabli~ salt
bariwo chloride) ~ 8ir~oe leg
leo like Ba~+ ione~ do not form an areenite prooipitate, then
end, a
o the Bole a combination of Mg*~` ions occurs only on
on adding MgC12 t
nt of the exchange of Mg~~ Nith mioellary K~ ions. For this reason
aooou
in a �d Bola proves to be ooneiderab~y less tt,ab
tY~e amount of sorbed Mg 6
he solo end their filtrates and leas than the quantity
the avidity of t
,Hut if the quantity of sorb�d I~g~~ be compared ei~
of absorbed Ha
n ion" and not pith the avidity of the filtrates as, in
the eoidif is at
have rrron done ~ the equivalence of the exahange
principle, ma~Y authors 6lY
o M ~~ions Frith micellary K* ions Nill be diaoovered~
f g
u ntitative calculation of the combinAtion of ions
Oux method of q e
fluid ermits the deduction that Ha*+ ions dia-
in th� intermicellary P
* ono a uivalently both in aged and fresh aola*
place micellary ~ i 4
ii
ddin to aged Ae 5 cola Sr and Ca chlorides, such intermediate
Ona 6
0~1 the Ong
ions should be observed as those observed in adding ~:k
relat
the other MgCl , in connection with th� i'act that
hand, 8a01Z and, on , 2 ~~"~r
is increased in the eeriees HaSO~,, 8r50 ,
the solubility of sulfates ~
{ sae ooasiderations~ evidently, are in complete agree- A
Ce?S0~ and MgSO~~ Th
3.
ith the results of the works done by various authors on aged sols~
ment ~t
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rx ~Si
f:
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Declassified in Part -Sanitized Copy Approved for Release 2012J05/25 :CIA-RDP82-000398000100100030-7

 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100030-7

1
i
i
1 tit i~ i ~ ~ ~
~ ~ ~ ~ R~ ~i~`t~
} .
OonolueloA�
1. It hao boon doa~natrated that in agi~?g AagB solo i~ oontaot eitt~
3
the air aulti~rio and araonoua aoic~o aro dooueulatid and t1~at eul~io
aoid oonditiono the aoidi~ioation of th. Dole
2 ~ A simple a~othod i o oPrered for a quantitative aaloulation o~
tho formation a!' ineo3uble salts on aooount o~ the reaation~~ in
whioh prooeodf
the intermioellary Fluid of tho eolewhen eleotrolytos `are added.
8y u�ing thin methods it has boon shoen that the ionio eaahange
in agad Ae s sole prooeede eleo equivalently in manner similar to that
23
in Freoh eola, although in aged aols it ie oomplioated in some inetanoee
by intermioellary reaotions~
Krasnodar Entered at the Editorial OS~ioe
State Pedagogical and Teaohee Institute 4 February 191?
~l oonolueion, like t~:at reQO~aed by ua in studying the
ion exohange in sulFur cols ~'l~).
Bibliography
1. Linder, 5. E.; Pioton, R. J~ Chom Soo, 67, 63, 195; 71, 563, 1897;
1906, 190 ~
2. Whitney, W. T, j Ober, J. A.; Z. Phys Chem, 39, 630, 1902.
3. Pauli, Wo; Semler A.; Koll Z., 34, 145, 1924
' 4� Rabinovich, A. I.; Z~ Phyo Chem (A) llb, 97, 192.
S~ Rabinovioh, A. I.; DorFmen, V. A.; Tr Chem Inet imeni harpov~ S, 19z~.
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Freundlich, K.; Koll Z., 1, 321, 1907; Z~~ Phys Chem, 7,3, 3$5, 1910;
r
Freundlich K.; Zeh, P.; Z. Pbys Chem, 111, 65, 1925; Freundlich H,;
v pt;
I+
Joaohimeon~ K.; Ettiaoh, a.; Z. Phyo Chem (A) 141, 249 1929
d ~ ` Bere etneva, A. Ya.; Kargin, Y. A ~ ; Aata Pbya Chico C SSR, 2 ~ 151, 193 5
9. Desha~yt, N. M~; Yaail ~yev, P. S.; Rabin~oh, A. I Zh. Fiz Khim,
~ r X34, 1934
~i ~
` J
' ~ tea ....e..r"'"" '
1 ~ : t
S t
i
` '
d zc
i
r
~ k i
1
1
' Declassified in Part -Sanitized Copy Approved for Release 2012J05/25 :CIA-RDP82-000398000100100030-7 .

 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100030-7
z
r
i
v. ~ i
~
~r
a
r:
3
~ t N ~ R ~ Zb ~ Fig Kh~m, 4, 60a, 1933
~4~ Vaal yev, P. 8.; DeahalY s t
oak Zeite ~ dor SoN~otuoio~, 4, 3Z8, 1933 r
ll ~ Rabinoviah, A. Z ~ f P~
Zhu Fie KHim, 1, +4~9~ 1~Oi ,
r in V ~ A. Rabigoviah, L. I Zb~ Fie Kbim 6, 1133 ~ 1933
Keg ~ !
d. P a Chem, 29, 99~, l9Z~i 35, 1, 1931E 35r 1369r
13, Meiaor, K~ ~ ~
3 lei aer N f; Grey ~ ! J ~ Ph~p Chem, 3b, ^17~, 1932; i~ei aor, R
193 ~
Iaorg Colloid Che~a, 3, 203, 193�
11~ ~ Khariu, A ~ H~; Aota Pays Cbim+ ~2, 736, 1940
15, Ghoah, s~= Dhar, N~ R�; Koll Z~, 3b, 129, 1925�
kbe~ ee J. N. Chaudhury, S. G.; Ghorh, B � N., Koll Rein, 43,
l6. ~ , ;
67 l9 b Gosh 9.; Dhar, N, R.; J. Pbya Chemr 101, 1394, 1924�
4 , 31
A Klimovitakaya, G� V�, Aate Phya Chien, 1, 1, ?29, 1935�
17 ~ Kargia, V ~
d Coworkers Aote? Phya Chien URSSr 13, 715, 194ot
16. Kharin, A. I ~ ~n 3
ZhOKh ll 239, 1941; ZbQKh, 11, 23z, 259? 1841�
� I. "Tbe Reaotions of 9 and AazO in Aqueous Solutions" ,
l9. K1~ariar A ; ~ 3
Koll Zhu, 9, 462, 1947�
vleva V. S. ~ ZhOK~, 4, 176, 1934E Krestinskayar
20. Krestinekaya, V. N.; Yoko , ,
V. H~; ZbOKh, 4, 209,.1934�
Aata Phys chip uRSS, ~z, 703, 1840�
2l. Kirin, N~;
oidal Chemioal Researoh on Sulfides and Sulfur"
22~ Kheurin, A� N.; Coll
rtation for Doctorate), Fiz�Khim Inet imeni Karpov, 1943;
(Dieee
ntiel Boundary Ians in Deep Ultr~?filtration of
Desorption of Potante
i
i
Colloid Solutions (At the Printer's).
2 � Kar in, V, A., Usp Khim, B, 99$, 1939
3 6
in V. A~ Koll Zb~, g, 101, zb9, 1946,
24� Shishirie~shviif! M~ Ye.; Kaxg , ;
4a
i
I
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�END~

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