COLLOIDAL CHEMISTRY

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP80-00809A000600200210-7
• Release Decision: RIPPUB
• Original Classification: R
• Document Page Count: 12
• Document Creation Date: December 22, 2016
• Document Release Date: June 29, 2011
• Sequence Number: 210
• Publication Date: August 3, 1948
• Content Type: REPORT

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CLASSIFICATION
7W (-CENTRAL INTELLIGENCE AGENCY '-` REPORT
ONFQRMAT RT
JAN 31 1955 k"eFDD
FOR OFFICL4L USE ONLY
M er .rm. w.ws ...
'Wr 77/ ONiI~M M N! sa. is AO uuaITi f RMM1
1555 .iw wM a to W " iSI
DATE DISTR. 3 August 1948
SUPPLEMENT TO
REPORT NO.
THIS IS UNEVALUATED INFORMATION FOR THE RESEARCH
USE OF TRAINED INTELLIGENCE ANALYSTS
al, Vol II, No 4, 1947? (FOS Per Aba
MRMian P~ alr gollo Igrn.
Oables and figures referred to in the text aresppended. Nuwrala in
7
l
ogapy
parentheses refer to the bib
In the present article we shall follow the previously developed plan
(+) Each of the princtpi processes of aging emulsions -- coalescence and
separation -- will be studied separately, so that their relationship may
finally be established. In this it is natural to expect that a nuabar of
fundamentel rules sstablishsd by us for gelatin emalsiona (1, 2, 3) will also
__..1_4e4._ we "J .'
apply to cleats esnlsiaas. however, in view of the essential differences
.h _
k mxmct
two
ee
Olean a vary accvrvaaa, vv ....._..?-- ..- -- + ]ylecular film form
and than expanded single layers are formed, while pome
'5=0' OLE OJT
Military Academy of Chesi.ial Warfare
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wean we consider eaFilaiene with 7B-OpOmOlecw3leS' protective layers, it
ant be expected that coalescence in systems with expanded and condensed
single layers will fail to wocsed uniformly. Since in the first case the
protective films are unsaturated as far as adsorption is concerned, accor-
ding to our ideas of the coalescence mechanism a limited coalescence will
take place. This process is characterized by the fact that its rate in
time drops almost to zero, while the dispersed oil is practically unsepara-
ted in the form of a macro-layer. The changes taking place in the system
daring its aging amount to the well-kaorm diminishing of the degree of dis-
persion and increase of the density of the cover by the emulsifier at the
interface between phases.
For a similar limited coalescence we introduced (1) an equation oonrioo-
ting the mean diameter of the pertiwith the time of aging of system
where d is the mean disaster of_the drops of oil at time t do is the
initial mean diameter (T a 0)y d-is the mean diameter withr-"Vis a
constant.
Actually, Harkins and Beeman (5) and subsequently Fisher and Harkins
(6) established rules for an ion of benseno in water with expanded
sodium cleats files (ti 46 IN in the process just described. This is
illustrated by the curves in Figure 1, constructed according to the data
of Fisher and Harkins. The dotted curve O (r) represents the conga in
time of the area occupied by soap moleculw in an adsorption layer. The
curve a(T) represents the change of the mean diameter o of oil drape also
as a function of the time of aging of the systems. It is evident from
the drawing that as the drops increase in site the density of the sop
fits also increases to the point of a state of condensation (19.5 'ter
10 days of aging).
W. used tbVw date':br checking equation (1) graphically. In the system
the equation (T) is a straight line and, as can be seem rim Figure
1, the expsrimunn points provide the required relationship. We note in
this connection that for do in the calculations we took the value d
throughout 16 hour. of aging, since the magnitudes for the earlier period
(up to 16 hours) vary irregularly. ,Consequently, the time reading is.
also taken from 16 hours.
Thu;, our equation for the ooaluseence energy is justified for eemisions
protested by expanded files of oleate just as for gelatin systems. We may
*oval ads from this that the coaleaoecoe mechanism fundamentally done not
depend upon the eatura of the emulsifier, provided certain general condi-
tions are observed (adsorption saturation of the layer).
Hitherto we have been considering a spontaneous process. However? we
may cams to the n ul.tsute result in the change of adsorption layers by
another method, that is, by subjecting a freshly prepared soul sion to a
wash random mixture by hand (shafin in a container). In this case the emul-
" begins to break down rapidly at first, and then slowly and after about
bait an hour the all phase is distinguished by spares drops. TM remainder
oomptisss a such nwre stable system. It we make an analysis of the initial
system and the remainder after mixing, we can readily discover the essential
mature of the process.
We conducted such an investigation for three emulsions containing benzene,
cleats, and water, prepared in the usual way (4). The dispersion analysis
and determination of soap adsorption was done by the methods described in the
preceding artirle. The results arc caellerted in Table 1.
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As can be seen from the table, the pscessary process is accompanied by
a considerable compression of the interface, chiefly due to a partial break-
dawn of the emulsion, while the protective cleats film are contracted a moat
to the point of condensation.
Passing now to a system with condensed protective oil films, it is
possible to expect that their aging will take place in a quite different form.
Similarly, it appears that the dispersion of a similar type of emulsion
resins constant for a long time, according to Table 2, where the collected
results of dispersion analysis of three emulsions, contained in test tubes
with around-glass stoppers (33 e in d{. ?meeter) for about a r---* .h at 14-1
degrees, arm given...
Harkins (5) also notes the great stability of such systems. For one of
the samples he could discover no appreciable variation in the degree of die-
pereion after keeping it a year.
However, it is not yet possible to draw conclusions from these observa-
tione as to the absence of any coalescence. The latter, as we aha ll am
below, takes place in a very peculiar fashion.
Our emulsions, when stored, display a marked tendency to g *e off free
bensaas, which, it stands to reason, is inconceivable without mutual fusion
of the separate drops. This breakdown of the emulsions is illustrated by
the curves in Figures 2 and 3, where the quantity of released benzene is
given on the ordinates in percentages of its initial content in the system,
and the aging time in hours is given on the abscissae. The curves in I"lgure
2 refer to the series of saturated emulsions with diverse concentrations and
conden protective cleats films (see also (4)). The emulsions were kept:
in test tubes with ground-glass stoppers (diameter, 33 me), while from time
to time the liberated benzene was meaerred with a measuring cylinder after
the eaul.aion had been thoroughly mixed with a glass rod. The curves in ,
Figure 3 wen's obtained by the same method for a 12:1 emulsion, uniform amounts
of which were kept in oylindr,aal wntainers with diameters ranging from
46 to 106 a. During the escape of evaporating bensene the emulsion containers
were placed in a d.^ier ovar a layer of free benzene.
As can be seen directly from the figures, all emulsions, and, especially
diluted owe, had broken;down considerably. Another fact is very noticeable,
that is, the relation of the breakdown rate and the form of the breakdown
curves to the diameter of the container.
The breakdown rate generally ireaass with the circumference of the
container in which the emulsion ie,ore+A(9igure 3). On the other h.9td, the
breakdown curves in small containers have an S-form, that is, the process
here has a somewhat autocatalytic nature. The curves for the large containers
are concave in relation to the abscissas during the entire time of study of
the aging process.
As it appears to us, the., last ducts throw light on the breskdosn
mbahsaiss of emalsioos with condensed soap films. Sims the rate of
breatdoen depends upon the also of the emulsion column 5a the containev]
we ay assume with greet probability that the drops of the ell phase on th
the eartace layer of the emulsion in contact with the external non-
polarized msdiwa (originally air, and then the maorolayer of benzene)
are rider mush lose favorable conditions than those within the son-
Gouts. 1vtdeatiy the ymetry of the oonditions of existence of an oil
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1
Let no note in conclusion that system with polymolecular? protective
file have not been investigated intensively?.by us. It is nevertheless to
Thus, 'ten protected by condensed sopp files, coalescence proceeds
very rapidly, especially in the layers near the edge of the emulsion.
If the free surface of the smulsion is small (small container), the role of
similar aaara-occlusions become relatively greeter, as a result of which
bsnaiee. The latter are, so to speak, the centers of coalescence, and as
they gradually increase in size they in their turn speed up the process.
lytic nature of certain curves (saall-osntsiners). Similarly, surface coa-
mmy take place not only no the edge of the free surface of a system,
bul also wit :ic its plume at the edge of coarse macro-conk sis~ ..: of -i.^ and
or which the drops hare fuss with each other incomparably faster, as well as
with the mmorolww Of be"".
This peculiar process is called surface coalescence as contrasted with
voles coalescence, the probability of which doss not depend upon the spatial
position of the dispersed drops.
be noted that they have a still greater stability.
greatest importance to the theory of the stability of highly concentrated.
emulsions. With the help of the studies of these processes in previous arti-
cles (2, 3) we were able to explain in'detail the active function of water
when protected by a colloid emulsifier (gelatin). We shall now carry out
an investigation along the same plan in the case of smilsiona. protected by
sodium cleats.
We are interested in tw basic problem: (1) reversibility of the
water bond and the critical state of emulsions,. and, (2) the nature, of the
here the peeoipitatioa of water is also at least a partially reversible
proceas?
^e muds a detailed study of the kinetics of separation in centrifugal,
fields of different strength (from 1,000 to 4,000 rpm) and the kinetics of
expansion of files for a series of saturated emulsions with condensed protec-
4 (an the right is the separation, an the left, the expansion); time 'r
serves as the abegiaee, and along the ordinate is given the relative water
forth in previous reports (4, 2).
content in files q ? in percent.
o
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emulsions in their separation in centrifugal fields without breakdown, and
the maxima water content in the films after their saturation expansion.
curses by extrapolation toT-, oo. This quantity, of course, will diminish
with the increase in strength of the centrifugal field.- The experiments,
The second of the indicated quantities (maximum remainder) can b e
separated water. One can suppose, that here the original water content is
below the equivalent remainder, and therefore such enmlaions should expand
water after the expansion of the films. And meopwhile the film obtain .
from highly ooncentrated oaten (18,1 and 92x1), counteraboorb all the
found fires the cursss far the expansion of the files. However, this method
am give a correct result only if there is still a certain rani alder of free
ex paaurlsa.
water within a larger. test tubs with a ground-glass .topper. After a quick
double turnover of the whole system, the small test tubs was iilied with
A test tube wee approximately half filled with a ulsios,. The surface
of the a ilsicn was owfu].1y leveled and the grease was removed from the
will. of the test tube. Miss the test tube was isaerssd upside down in
diagram of this expsriaent is given in Figure 5.
tial volume in the test tube, and the increase in volume upon ,upending, it
is not difficult to detea:ns the equivalent content of the beaded water. A.
sufficient to setablish an equi2lbrima, the dearmrd di plaoeosnt of this limit.
was measured. Moving the original concentration of the emulsion, its ini-
5m1, 16,1, = 12,1), and the capacity just described of the original amid.
slow to expand, and we were able to establish for a awabsr of systems the
of the agwons layers according to the formula
3"
!'isms knood-mg the equivalent valued of the water r. .J r in expan
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These final results of our experiments are assembled in Table 3..
Thus, Table 3 indicates the area of reversible change of the intetmme
diate water layers in our emulsions and, as can be seen from the table, in
the first spproxisation the Limits of this area are not related to the
concentration of the system.
We have already encountered a similar fact in studying the intermedi-
ate layers of the acntU W O- phase in gelatin emulsions with the sole differ-
ence that there the equivalent films in expanding rose only after their
known nonreversible condensation as a result of the single centrifugal
quality of the system (2).
However, the essential difference between emulsions protected by gela-
tin and soap was another matter, in that it lay in the relative position of
the critical state. We recall that the latter is reached with such a thick-
now of the layers of the continue phase, when with the external mechanical
effect (mixinE the emulsion begins to break down with the liberation of dis-
persed oil in the form of a macro-layer. In the case of emulsions protected
by gelatin the critical thickness of the films lies between the upper and
lower equivalent values of $ , that is, it falls in the area of the revers-
ible change of films (3). In the case of emulsions with condensed protective
cleats files the extraction of water to the point of the minimum remainder
does not bring about breakdown of the systems. Evidently the critical thickness,`
of the layers here coincides with or is even somewhat lose than the minimum
equivalent value of S . This is also supported by the results of previous
work. As was found there, the average thickness of the water layers in which
?'.
a synthesis was still possible of saturated emulsions with condensed cleats
layers is equal to about 900 R, which corresponds well with the average
mg itude of SnuN In table 3 (1037 2).
However, if in our systems the critical limit cannot be transcended by
the mechanical method (centrifugal effect) another method can be used, namely,
that of Erasing the water. For this purpose we subjected two.eyatoes with
ratios of 12il and 32tl to cooling at a constant temperate below zero.' A
known volute of each of the eawileione was continually atir:^ed with a thermome-
ter, permitting measurements of the temperature of the eysteme.from time to,
time, while the volume of released beaten sac:dete gained by pouring it off
in a measuring cylinder.
The results of the experiments are shown in Figure 6 in the form of two.
pairs of current one pair corresponds to the temperature change of the aye-
tee with tits t (?) and the other pair represents the amount of separated
benzene in percentages as functions of time', 0/0 ('h.
In considering the curves for t (T) their peculiar form immediately
strikes the eye. After following a smooth path in the process of cooling
the emulsion from room temperature, the curve takes a sharp jump, the cause
of which can be interpreted as the beginning of the supercooling of the
system. Then there is a horizontal section of constant temperature, the end
of which coincides with oca.pwete freezing of the water. Oa the other hand,
from a comiparieon of both pairs of curves t (T) and 0/0 (1-) it appears
that the progressive breakdoen of emulsions only starts from the moment of
freezing of the known part of the water, and the smaller that part is, the
more concentrated the original emulsion is. For a 32t1 emulsion, in which
the water fifes are thinnest (- 900x) the beginning of breakdown practically
eoiroideu with the temperature jump is curve t 001 that is, with the begin-
ning of the freezing of the water phase.
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,,, - ~rfau ac the Previous value for the
critical thie-mese of the water ,,,layer, and consequently for emulsions with
condensed soap films it actually coinotdea with the adnimum egdval,mt
thiekeese indicated by the lower lino in Table 3.
It is Interesting to note that if the freez4ng point of the continuous
phase of the emulsion is lowered, the temperature limit of the breakdown of
the system is changed accordingly. NO diluted a 48#1 emulsion (97, 96% by
volume) with glycerin three times the volume of the water phase. The gl_
cerin was added in small Portions with brisk
mixing finally we obtained a very stable and transparent y12an electric 1 emulsion dry
a continuous phase composition of 25 percent by volume of water and 75
percent by volume Of.glycerir:;, For this eniuieian we plotted the cooling
curve t('C) in Figure 7, along with the corresponding curve for the 12:1
emulsion without glycerin (dilution of a 48:1 system by water).
As is evident from Figure 7, the curve t(T) for an emulsion with gly,
cerin is a steadily falling branch showing cooling
ture. It is evident that the horisontal plateau ofcurve ert(T) and tconsea_
quently,the area of breakdown can be reached only t(T) enolng
upon much deeper cooling.
eion nseq protected l , by adding glycerin to prepared, highly concentrated emul-
sion protect, acetone soap, ethylene ~ stems can b e euccessfull,- prepared.
Sthyl this glycol, and thiodiglycol are not suited
purpose, nor are salt solutions. All of them, in the absence of
glycerin, iawidiately break down the emulsion.
We *tin have to determine the nature of the forces which sustain a
oonriderable ;sr', of the water phase in a combined state in emuleic.,s with
condensed protective cleats films. As was noted before (4), on the border
of the section of oil drops an slsctrloal double layer mast develop due to
the partial li!osooiation of i n-generating groups of soap molecules, forming
a protectivel?ila. It is not difficult to demonotrate this by electro-
ptioresie made on a concentrated emulsion.
We carried out an esperimsat for this purpose, illustrated in Figure 8
(platinum elec.crodes) If the negative pole in this system is located on,
the bottom, and the circuit is closed, the water foams the border of the
emulsion sections this Isvel, recorded by a cathetometer, remains' steady.
If the pales are interchanged, the border very quickly drops toward the
lower positive elsatrede -- the lion absorbs the water, no to apeak. In
the subsequent ormitching of poles the emulsion column is contracted to its
former level, but the process is much slower.
I easuramunte of Y, made fbr an 18x1 emulsion with condensed oleate x4lme
motion of the border of the section below, gave a value of 5.85.10-'
c for the elsctrophoretic mobility of the oil drops. This figure shown a 22 a good Correspondence with the data of other authors (7, 8, 9).
Thus, in discussing the behavior of our systems we must consider the
interaction of electrical double layers. From this point of view it is not
d
ifficult to understand that spontaneous separation of our emulsions can
take Place
yet ce 0124 0whenlm diffused ionic atmospheres of the adjacent drops do the opposite case, electrostatic repution forces
not
arise between the drops of oil which preveata their joining and separating
from the water. Separation again becomes possible only under the influence
of the external forces of a centrifugal field.
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nisn.er, Poor eve.-y rorce applied externalt a
will ultimata be reached which corresponds to the Uexpan condition to estaticrfm>fa
the diffused atmospheres. This is also the cause of expansion tesuof
protected by soap. expaasiexpansion Of emulsions
It can be concluded from the a bona that the maximum squiliburiu (expen-
aiam) and the minimm sc ltbrima (separation In centrifugal fields)
thickness,. of the water layers oorreepondo to the undistorted and fully
4121erted condition of the ion atmospheres of the electrical double layers
In an avulsion.
The conclusion that salt solutions prevent emulsions from expanding, ,...
foil ee, cnroject to experineatel verification.
Thus, in contrast with gelatin emulsions, where the known part of the
water to combined by the osmotic expansion forces of the gelatinous pro-
teetive layers, In the cars of oleate emulsions the water remains corbined
In the system because of the electrostatic repulsion forces which prevent
the oil drops from joining. This is what prevents decrease of the thick-
mew of the water phase layers to the critical amount, and this in turn
keeps `.bs system from very swift ooaleaoence and from bre.too n.
Thus, on the basis o4 cur !.nvestigations we can make a well-supported
assertion that the stain cause of the stability of highly concentrated eeul-
sione is the active forceful interaction between protective films of oil
drops. The nature of this interaction (osmotic or electrostatic) depends
upon the nature of the emulsifier, and consequently upon the n.ruoture and
proportion of protective films.
gcwever, in any emulsifier thin intermediate layers of the water phase
asst indicate a loosening effect (Deryagin an authorJ), which also psevent@
the oil drops from Joining. We cannot decide hers what the relative impor-
tance of the loosening effect is compered with osmotic or electrostatic
effects in the stabilisation of our systems.
1. Coalsscence in highly concentrated oil-eater type emulsions protea-
ted by sodium skate was studied.
2. It was found that in amalsione with expanded films the volume coal..
cones is relation to aging conditions produces either the known decrease in
d
the ,pw of dispersion of this system or Ito partial breakdo.n, but in both cases
rption layers were concentrated to tame point of condensation.
3. In ewnlaions withoondmsed filM the rats of surface coalescence is
inccmpsrably higher than the rate of volume coalescence, as a result of
which the system breaks dam with aging in the. ftnmdso.7, areas (near the free
surface or on the border with large deposits),
4. The separation and expansion of emulsions with condensed filne'of
oleate under divers, conditions was iemestigated.
3? The obaraeteristio of equilibrium and critical layers of tt'e water
peas, was given.
6. It was proved that bonded water in these systems is maintained by
the slactrosttatic interaction of single cleats mayors.
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1. &vmbr6, g.?
.
8,
281,
1946
2. ftv~vb*Tg, ! uea?., 8, 288,
1946
3. Bromberg,11a
?,
8,
377,
1946
4. Bromberg, boil
.,
91
13,
1947
5: Rerkine and Beeman, Jim- Chem. Soc., 57, 1674, 1929
6. Fieb.r acid harking, J. %To. ,.Chem., 36, 98, 1932
7. Eflie, Z., _PhV. Chain., 78, 321, 1912; $0, 606, 1912
8. Powd.s, ibid., 89, 186, 1915
id=Hs_I&?, 22, 192, 1926
Ilg
9, Tuarina, Q
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0.02864
22.5
0.48
42.8
24.8
13.3
0.14
33.0
?.8.9
0.04296
25.0
0.09
86.8
33.2
18.0
0.17
51.3
19.6
0.05728
31.0
0.07
127.5
36.8
22.0
0.07
79.1
22.8
Amount of 02eate
in will Ratio
Man Diaaeter.d for the Tim of
Aging in Boars
0.00716
3.8
11
20.2
0.0132
5.2
13.
13.7?
0.02864
12.0
15
12.6
144
300
526
650
20.2
21.0
21.5
21.2
12.1
ll.?
12.5
12.4
13.0
13.4
13.8
13.0
Table 3? i iolmeee .,f Water layers Order Various 013ate Emulsion
CoadttiCei (Sin 2)
0i1-Water ratio of the seulaioa ...............
5.16
12
18
32
d .aximve (expansion) .....................
n 3R0
4
310
4200
4
160
a minus (separation at 2,000 rpm).......... 1830
150
705
866
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Figure 1. Ocalescence in Monte
xr'11'Acne (according to Fisher
and 2"Ides )
Fimurs 3? Meet of Cis. of Coo-
taimer oa BrMblom of lbalsion.
Attic LRii. ?de figures on
the arras are the diameters of
the oontainers is -(' is the
tiem is boars.
Figure 4. The Fssr6r' of 8epnration
(Right) and the Rnesgy f Exp4.9sian
(Left) of an *.eiulsica With Cotdensed
Filar of Oleate la a Ceotrifudal
Field of 2,000 Ma
Bigure g. Diagram of Eipertment to Determine
the Eepameion Egaillbrisa of an Emulsion
1 - smalsiom{ 2 - Matere 3 - cathetoaeter
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Figure 2. Breakdove of Oleate I=-slow
With Aging
Thee.figures on the curves are the
oil-Mater ratio of the emulsioo;'t is the
time in hours; the amount of bentioe separated
in % of its original content is on the axis
of ordinates.
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Itgure 7. Behavior of Emulsion
to NYeeaing (-12 degrees 0)
-0- 0leste condeaeattoo equal to -0- Continuous phase later 100%
0.025 N/liter, ratio 12:1 -s- Continuous phase: later, 25%,
-'- Oliite coedentiattoo equal to glycerine 75%
0.143 K/lttsr, ratio 32:1 A - Caaplete breakdown of esaletco
2t~tre 8. ~lagr * of AYpertoent od Catapkoreate of Ye ieioo
l - eaalatoo= 2 - water; 3 - oatbetoaeter,
,
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