USE OF TRACER ATOMS IN THE STUDY OF THE PHENOMENA OF ADSORPTION AND CATALYSIS

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• Sequence Number: 385
• Publication Date: May 26, 1950
• Content Type: REPORT

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USE OF TRACER ATOMS IN THE STUDY
OF THE PHENOMENA OF ADSORPTJ(3fSL.AND CATALYSIS
N. P. Keyer
Moscow
/In the following text only work done by Russian investigators has been con-
sidered, with one or two exceptions, although the original article covered the
whole field, including work done outside USSR. Figures are appended]
The experience acquired in work with deuterium can be utilized in work on
the introduction of tritium into organic molecules. The basic methods are cat-
alytically activated exchange between HT and the organic molecule, hydrogena-
tion of unsaturated compounds with tritium, interaction of tracer containing
water with a carbide, etc. The question has been adequately treated in reviews
published in Soviet periodicals(l, 2, 3).
A review published by Ayvazov, Neyman, and Tal'roze (I+) deals with the in-
troduction of carbon tracer atoms, particularly C14, and gives a list of com-
pounds which have been synthesized by methods described in that review and
elsewhere.
The introduction of tracer halogens (F98) by means of a catalytic exchange
reaction was considered in detail in a revd.ew, by Berezhneva and Roginskiy(5).
The separation of bromine and iodine isotopes from other isotopes of the same halogens on the basis of their differential reactivity has received consider-
able attention(7). Work on this subject has been done in both the US and the
USSR.
As a phosphorus indicator the tracer atomlP 5 with a half-life of l4 days
is used. Extensive data on the application of this tracer are given in two re-
views(6, 7).
ARMY:"c. AIR
NSRB
FBI
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One of the earliest applications of radioactive isotopes was in the study
of adsorption. The principal lines of investigation based on this method were:
(1) investigation of adsorption laws, particularly those of adsorption equilib-
rium, at minimal coverage of the surface, (2) study of the adsorption of mix-
tures, (3) study of surface inhomogeneity by means of differential isotope ad-
sorption, and ('+) investigation of the properties of substances adsorbed on
active catalysts.
Aside from these four theoretical subdivisions, a problem of great prac-
tical interest which has been thoroughly investigated is the capture by freshly
formed precipitates or crystalline sorbents of small quantities of substances
from solution. Only the use of radioactive tracers has permitted some clarifi-
cation of this complex phenomenon, so that it could be separated into simple com-
ponent processes. The work of Soviet radiochemists headed by V. G. Khlopin is
particularly outstanding in this field.
Investigations conducted by members of this group demonstrated first that,
to be co-precipitated, components which are present in small quantities must be
isomorphous with the carrier precipitate. Khlopin, Polesitskiy, Ratner, Tol-
machov, et al. (8, 9), showed that the distribution of the microcomponent be-
tween crystals and the solution follows the Berthelot-Nernst law when equili-
brium has been reached and conforms to the logarithmic Doerner-Hoskins law ff.
J. Am. Chem. S. 47, 662, 19257 in the case of nonequilibrium systems. Khlopin
proved experimentally that in the capture of small quantities of substances by
so_ido the adjustment of the concentration of microcomponents in crystals pro-
ceeds over recrystallization of the latter in solution(10). This refuted Tam-
mann's theory that diffusion plays an exclusive role in this process.
}Oilopin and Nikitin clarified the nature of Grimm's type of isomorphism
and of its differences from the classical type(ll). It was shown that the ab-
sence of mixed crystal formation below a certain concentration of the microcom-
ponent is typical of Grimm's isomorphism. The microcomponent presumably re-
places whole regions of the crystal lattice under these conditions. The theory
of distribution of microcomponents between the solid and the liquid phase was
developed by Ratner(12).
The method of measuring surfaces of crystal suspensions with the aid of
radioactive indicators is dealt with below. It is closely connected with the
isolation of microcomponents. The important problem involved here, which has
been briefly indicated, is of interest from another point of view and will not
be considered in this paper.
A. Use of Radioactive Tracers in Determination of the Absolute Surface of
Crystal Suspensions
There are three methods for measuring a surface with the aid of radioac-
tive indicators. The first is based on the exchange of an inactive ion enter-
ing into the composition of the solid phase with its radioactive isotope con-
tained in a saturated solution. The second involves the exchange of an inac-
tive ion entering the composition of the solid phase with its radioactive iso-
tope contained in the isomorphously crystallized part of the solid phase. The
third method is based on measurement of the emanation of a radioactive sub-
stance which is distributed homogeneously throughout the solid phase. The
first two methods originated with Paneth, while the third was proposed by Hahn
(compare review listed under Item 13 in bibliography).
The results obtained by the first two methods frequently deviate in both
directions from the true result. If only a fraction of the surface participates
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in the exchange, a value which is too low will be obtained. If layers lying
below the surface participate, the value will be too high. Khlopin and Mer-
kulova (14) studied the limitations of the three methods and clarified the
conditions under which they can be applied. The investigation in question was
carried out with suspensions of the following crystals: lead sulfate, barium
sulfate, lead chromate, barium chromate, and silver chromate. As the radio-
active isotope of lead, HaD was used; radium was used as an ion supposedly
isomorphous with ions of lead and barium; anu RaD was used as an ion supposedly
isomorphous with silver. In the case of suspensions of PbSO4., BaSO4, and
BaCrO4, there is good agreement between the results obtained by the three meth-
ods in question. In the case of silver chromate, the method of exchange with
RaD ions leads to a value which is much too high. The authors doubt for that
reason that PbCrO4 and Ag2CrO4 are actually isomorphous. They reached the con-
clusion that radioactive tracer methods are of value when the surface is clean
and there are no extraneous adsorbed ions. The exchange with the surface atom-
ic layer is completed rapidly (within the first 15 minutes), whereupon a secon-
dary exchange with inner layers, which is accompanied by recrystallization, takes
place. For the application of the method of exchange with an "isomorphous" ion,
a knowledge of the crystallization coefficient of the system at the temperature
in question is needed. This coefficient enters into the appropriate formula in-
stead of Paneth's solubility ratio.
Khlopin and Merkulova developed a special relationship according to which
the ratio of the quantity of inactive ion on the surface to the quantity of that
ion in the saturated solution is proportional to the ratio of the quantity of the
adsorbed radioactive "isomorphous" ion to the quantity of the latter ion in the
solution. The coefficient of proportionality is equal to the crystallization co-
efficient of the system in question.
In the emanation method, one must be sure that the radioactive material
evolving the emanation is distributed completely and uniformly. The correction
for the diffusion of the emanation through the crystal lattice, as applied by
Strassna_n, is unnecessary. Khlopin and Kuznetsova (15) call attention to the
fact that, in the adsorption of radium on lead sulfate, foreign ions in solu-
tion may bring about rapid recrystallization. There is also additional deposi-
tion of solid material due to the altered solubility caused by changed concen-
tr.:tion of the corresponding ions in solution. Both factors are a source of
error. The slow process of the capture of radium ions which follows the rapid
process of adsorption is connected with the slow process of combined crystalli-
zation taking place in consequence of the recrystallization of the solid phase.
L. Ymre (Z. phys. Chem., 1931, A. 153, 127, 138) was mistaken in assuming that
the slow process is essentially a slow stage of the adsorption process itself.
Radioactive tracer methods can also be applied in the measurement of metal
surfaces (0. Hahn, plied Radiochemistry, Goskhimizdat, 1947). The relation-
ships expressed by Merkulova and Khlopin retain '-heir full validity here.
Early work in the field was concerned principally with the exchange ad-
sorption of "isomorphous" ions or the potential-forming adsorption of the or-
dinary ion already present, because the isolation of substances present in
low concentrations is based on processes of this type. A considerable number
of papers dealing with the adsorption of radon from the gas phase have been
published. The qualitative relationships established in that type of work are
covered ii, Section B, below.
B. Investigation of Adsorption Laws
At low degrees of filling of the surface the adsorption isotherm follows
Henry's law. A higher degree of filling results in Langmuir's isotherm. In-
homogeneities of surface properties and of surface forces in the adsorption
layer must lead to still other types of isotherms. Even at low degrees of
filling or coverage of the surface, conditions corresponding to Henry's law
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cannot always be reached. Often the parabolic isotherm
1/n
or the logarithmic isotherm of Shlygin and Fruakin (16)
q = B lg p
most accurately describes the adsorption equilibrium. Both of these isotherms
were tree-.ed theoretically in papers by Zel'dovich (17), Roginskiy (18), and
Temkir(19). Kobozev and Gol'dfel'd as well as Temkin showed that the logar-
ithmic isotherm can also be derived by assuming that adsorbed molecules repel
each other or. a homogeneous surface(20). As :;horns by Vol'kenshteyn (21), the
parabolic isotherm can be explained by repulsion only if a type of interaction
between adsorbed molecules which never occurs in nature is assumed.
It is more reasonable to ascribe deviations from the laws of simple and uni-
form adsorption to differences in active centers with reference to adsorption
1-eat. The deviations from Langmuir's relationship cannot be explained by the
interaction of adsorbed molecules, because the distances between them are too
great.
Nikitin and Vdovenko (22) studied the dependence of adsorption of radium
on glass from the concentration of radiufi ions in solution. Thirty to 60 min-
utec were sufficient to establish an adsorption equilibrium on the surface of a
rc?tating glass cube. The coverage of the surface was very low, but a parabolic
relationship apllied.
A lowered pg had the effect of reducing the quantity of radium which was
adsorbed. Starik and Gurevich (23) observed a somewhat different dependence of
rudi;im Asorption on acidity and established that contamination with foreign
ions has as~st pg effect on adsorption.
That'4iie deviations ::ron Langmuir's isotherm are due to inhomogeneities of
the aULrface and consequent variation of the latter's adsorptive properties
:ether than to interaction be?`ween adsorbed molecules has been confirmed on
the whole by experimental data obtained outside the USSR. Thus, 0. Erbacher
(Z. Phys. Chem. 1933, A. 163, 215; 1937, 180, 141; 1938, 182, 243; Z. Elek-
trochem., 1944, 50, 949) in determining the adsorption isotherms of natural ra-
-'.ioactive isotopes of lead (thorium B), bismuth (thorium C), and polonium on
silver, nickel, and gold, established that the ions in question are adsorbed ac-
to a parabolic relationship (with 1/npscl'.ic conditions obtaining in this case: it is symbatic at a low density of
adsorption and becomes :,ntibatic at higher densities. The simplest case of a
?:'ibatic relationsh?t tetweeen the activation energy of desorption Edes and the
heat of adsorption Qa,is occurs in molecular adsorption when the activation energy
of also ption may be neglected and Edes^' Gads. In this case the molecules which
were adsorbed last will be desorbed first. If the relationship between Eads and
Ed_, is symb tic (7igcre 3). the molecules adsorbed first will be desorbed first.
Unless there is creeping o the surface, no redistribution with regard to the
isotopic composition- will occur, and that composition will vary as the gas is de-
soroed.
ilhen light a :-A Y_::=avy hydrogen (the stable isotope of hydrogen) were adsorbed
on activated carou..made from sugar, gas having the isotopic composition of the
seco_d adsorbed portion was always desorbed first, independently of the order in
which the two isotopes w-re adsorbed. Filling of the surface was 0.5 percent.
The rosalts show that at this density of adsorption creeping is absent. The
equilibritun isotuc:.t., fl---- h:oir ~er, adsorption at minus 182 degrees corresponds to
the parabolic equation q = Ap x.75, indicating a pronounced degree of iahomo-
geneity with an exponential type of distribution of adsorption heats. In the
case of nickel catalyst, light hydrogen and 99-percent deuterium were used. In-
dependently of the order of adsorption, pure gas having an isotopic composition
corresponding to that which was adsorbed last is desorbed first. After this
follow fractions having a mixed composition; the pure isotope which was adsorbed
first is desorbe3 last. These results again indicate a surface which is inhomo-
geneous with regard to adsorption. Zinc oxide both as adsorber and catalyst ex-
hibits behavior which is incompatible with the assumption of a homogeneous surface
(29; of. also H. S. Taylor and S. Liang, J. Am. Chem. Soc. 69, p. 1306, 1947).
Differential isotope adsorption shows definitely and directly that zinc oxide
has an inhomogeneous surface and that, furthermore, the behavior in question can-
not be due to mutual rsoulsion of molecules on a surface which is homogeneous
s. L~J!." ,:
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with respect to adsorption. In the case of zinc oxide, gas having the isotopic
composition of the second adsorbed portion is desorbed first, whereupon there is
a sharp change to the composition of the other portion.
Similar results obtained with substances which differ from each other to
the extent to which activated carbon, nickel, and zinc oxide do permit the gen-
eralization that deviations from Langmuir's type of adsorption must be due pri-
marily to inhomogeneity of the surface with respect to adsorption.
A. Effect of Promoters
Roginskiy and his collaborators showed that metals deposited by the vacuum
vaporization method are inactive catalytically when foreign substances are com-
pletely absent at the time of deposition of the layer(30). Metal layers ob-
tained in a gas stream (oxygen, nitrogen, or hydrogen) are activated by the con-
tent of gas acquired under those conditions. There is a maximum of catalytic
activity corresponding to a gas content which is rather low (below 0.5 percent
with reference to the weight of the metal Using P3332~ with a half-life of 14.3
days (obtained by the nuclear reaction S + nC = P15 + pi), Berezhneva, Ozi-
raner, and Roginskiy prepared palladium catalysts containing phosphate ions
which had been captured during the precipitation of the palladium. The effect
of the promoter introduced in this manner is apparent from Figure 4. In the de-
composition of hydrogen peroxide, the maximum promoter action occurs at a phos-
phorus content corresponding to 0.001 percent of the palladium weight. In the
hydrogenation of ethylene, the maximum promoter action corresponds to 0.7 per-
cent of phosphorus content. At the point of maximum promoter effect, the activ-
ity of the catalyst is ten times higher than that obtained without the promoter.
By using the radioactive indicator method, the optimum concentration of the pro-
moter can be determined very precisely, so that the exact quantity needed for
the most effective action can be added to catalysts.
B. Investigation of the Mechanism of Catalytic Reactions
Two broad lines of investigation are being pursued here: one tests the
hypothesis of the function of catalysts as transfer agents or, more generally,
the hypothesis postulating the formation of an intermediate complex consisting
of the catalyst and one of the active reaction components; the other is con-
cerned with the succession of reaction stages on the catalyst surface, and the
way these stages tie into each other.
An example of work along the first line is the study by Berezhneva and Ro-
ginskiy (5) of the interchange of bromine between ethyl bromide and ethylene
bromide in the presence of A1Br3 as a catalyst. Br32 with a half-life of 34
hours was used as tracer. Since both ethyl bromide and ethylene bromide inter-
change bromine atoms with aluminum bromide and since no exchange of bromine
between the two organic compounds takes place in the absence of aluminum bro-
mide, one must conclude that aluminum bromide actually functions as a transfer
agent.
On the other hand, in the bromination of benzene with Br2 in the presence
of ZnBr2 it could be shown that bromine atoms of zinc bromide are not trans-
ferred to benzene(31). Comparison of the kinetics of interchange of bromine
atoms between ZnBr2 and Br2 with the kinetics of bromination of benzene shows
that there is no connection between the two processes. The authors concluded
that ZnBr2 does not function as a transfer agent and that a deformation mech-
anism appears probable in this case.
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Berezhneva and Roginskiy next studied the isomerization of alpha-bromonaph-
thalene to beta-bromonaphthalene in the presence of aluminum bromide(s). The
isomerization does not take place in the absence of aluminum bromide. However,
by using aluminum bromide tagged with a radioactive tracer it could be shown
that the interchange between aluminum bromide and both bromonaphthalene isomers
proceeds at a rlte which is incompatible with the speed of the isomerization
reaction. Consequently, there is no catalytic transfer of bromine in this case.
Lyubarskiy (2) assured that there is transfer of hydrogen over the catalytic-
ally active complex A1Br3 according to the following scheme:
This is in keeping with results obtained by Moldavskiy and collaborators,
who showed that the isomerization does not proceed with A1C13 or A1Br3 alone in
the absence of HC1 or HBr(32).
In connection with research on reaction stages and the mechanism of cata-
lytic reactions on surfaces, the theoretical treatment of the question by Ro-
ginskiy (33) must be mentioned. Roginskiy showed that these reactions are of
the first order both for homogeneous and heterogeneous conversions. In the case
of heterogeneous exchange reactions, this is true for both simple and complex
surfaces. It follows from the essential simplicity of the reaction kinetics in
this group of reactions that the dependence between the reaction mechanism and
its operation in time is lost. Profound differences in the reaction mechanism
are smoothed out and find no reflection in the time relationship. To clarify
the true mechanism of catalytic interchange reactions, one must investigate the
dependence of the reaction rate constant on the initial concentrations and the
temperature within a wide range of changes of these variables. The theoretical
conclusions outlined above do not apply when the reaction is of the diffusion
type or when the surface is altered through catalyst poisoning or recrystalliza-
tion. The use of tracer atoms in this line of investigation does not lead to
unilateral results: several explanations are possible in many instances.
Successful application of differential isotope adsorption in the detection
of the inhomogenecus nature of the surface of typical adsorption agents and cat-
alysts has shown that thie is a fruitful method of investigation (26, 27), es-
pecially since definite conclusions regarding the mobility of molecules and
atoms on the surface can he drawn. Application of this method in catalytic re-
actions permits a study of the effect of surface inhomogeneity in these reac-
tions. If two portions of the same gas having different isotopic compositions
are adsorbed first, and the second reacting component is introduced afterwards,
information in regard to the effect on the catalytic reaction of variations in
the adsorptive activity of surface centers, i. e., of inhomogeneity with regard
to heats of adsorption, will be obtained.
1. G. P. Miklukhin, Uspekhi Khimii (Progress of Chemistry), 1948, Vol XVII,
663. fFDD Per Abs 64/49T77
2. G. D. Lyubarskiy, Uspekhi Khimii, 1947, Vol XVI, 422. [oo-w-69
.~
3. B. V. Ayvazov, Ii. B. Neyman, UFN (P ogress of Physical Sciences), 1948,
Vol XXXVi, 148. J DD Per Abs 33/49T2 77
4. B. V. Ayvazov, M. B. Neyman, V. L. Tal'roze, Uspekhi Khimii, 1949, Vol
XVIII, 402. fDD Per Abs 53/49T837
5. N. E. Berezhneva, S. G. Roginskiy, Uspekhi Khimii, 1938, Vol VII, 1,503.
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6. I. Verhovskaya, Uspekhi Sov remennoy Biologii Pro ress of Contemporary
Biology), 1947, Vol LXVI, 335?
7. B. G. Dzantiev, M. B. ire n, 452 1949 Vol XXXVIII 338.
8. A. P. ilaxner, "Radioactive Tracers and Their Application," ONTI (United
Scientific Technical Press), 1936.
9. V. G. l lopin, A. Anorg. allg. Chem, 1925, Vol CXLIII, 97.
V. G. Khlopin, B. A. Nikitin, Z. Anorrg. allg. Chem. 1927, Vol CLXVI, 311.
V. G. Khlopin, A. Polesitskiy, P. Tolmachov, Z. phys. Chem., 1929, A.,
Vol CXLV, 57.
V. G. Khlopin, Ber., 1931 Vol LXIV, 2655.
A. '_'oi:sitskiy, Z. phys. Chem, 1932, A., Vol CLXI, 325.
M. S. Merkulova, Trudy Radiyevogo Instituta (Transactions of the Radium
Institute), 1937, Vol III, 141.
A. A. Grinberg, 25 Years of the Radium Institute, Academy of Sciences USSR,
1947.
10. A. P. Ratner, M. Polesitskiy, P. Toimachov, Z. phys. Chem., 1933, A., Vol
CLXJ, 472.
11. V. G. Khlopin, B. A. Nikitin, Z. phys. Chem., 1929, A., Vol CXLV, 137.
12. A. P. Ratner, Trudy Radiyevogo Instituta, 1933, Vol II, 67.
Acts, Phys. Chico. URSS, 1939, Vol xi, 475.
13. N. E. Berezhneva, article in the handbook Problems of Kinetics and Cataly-
sis, Vol V. Academy of Sciences USSR, 1948.
14. V. G. Khlopin, Merkulova, ZhFKh (Journal of Physical Chemistry), 1939, Vol
XIII, 1282.
15. V. G. Khlopin, V. N. Kuznetsova, ZhFKh, 1939, Vol XIII, 1145.
16. A. N. Frumkin, A. V. Shlygin, Izv. AN SSSR, OKhN (News of the Academy of
Sciences of the USSR, Department of Chemical Sciences), 1936, 773.
17. Ya. B. Zel'dcviah, Act': Phys. Chin. URSS, 1935, Vol I, 961.
18. S. Z. Roginskiy, "Adsorption and Catalysis on Heterogeneous Surfaces,"
Academy of Sciences USSR, 1948.
19. M. I. Temkin, ZhFKh, 1941, Vol XV, 314.
20. N. I. Kobozev, Yu. B. Gol'dfel'd, ZhFKh, 191ri, Vol XV, 257.
21. F. F. Vol'kenshteyn, ZhFKh, 1947, Vol XXI, 163.
22. B. A. Nikitin, V. M. Vdovenlso, Trudy Radiyevogo Instituta, 1937, Vol III,
256.
23. I. Ye. Starik, A. N. Gurevich, Trudy Radiyevogo Instituta, 1937, Vol III,
241.
24. B. A. Nikitin, E. Y. Ioffe, Izv. AN SSSR, OKhN, 1944, 210.
25. S. Z. Roginskiy, 0. M. Todes, Acts. Phys. Chin. URSS, 1946, Vol XXI, 519.
26. N. P. Keyer, S. Z. Roginskiy, DOT (R-ports oithe Academy of Sciences USSR),
27. N. P. Keyer, S. Z. Rog ns y, zv. , OKhN, 1950, No 1-
28. N. P. Kever. S. Z. Roginskiy_, ZhFKh, 1949, Vol XVIII, 897. _
29. V. I. Levin, "Problems of Kinetics and Catalysis," Academy of Sciences
USSR, Moscow, 1949.
30. 0. I. Leypunskiy, Acta Phys. Chin. URSS, 1935, Vol II, 737.
K. S. Ablezova, S. Z. Roginskiy, DAN, 1935, Vol I, 487, 1941, Vol XXX, 29.
I. Mochan, ,SAN, 1941, Vol XXX, 26, 32.
S. Z. Roginskiy, ZhFKh, 1941, Vol XV, 1.
31. S. Z. Roginskiy, Izv. AN SSSR, OKhR, 1940, Vol I, 17.
32. B. L. Moldavskiy, L. S. Bezdel', ZhOKh, 1946, Vol XVI, 1633.
33. S. Z. Roginskiy, Izv. AN SSSR, OKhN, 1940, Vol V, 601.
fForty-four foreign references were also listed.7
ffigures follow.7
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Figure 1. Representation of Homo-
geneous Surface under Assumption of
Repulsive Forces Acting between Mol-
ecules
L
Figure 2. Representation of In-
homogenous Surface
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Figure 3. Example of Symbatic
Relationship between Energy of
Adsorption and Energy of De-
sorption
1-10-3 24-3 3.10 3 4.16 -3 2)
l0. to S 20.10 30.15''10.1C 3 (7
I>
Figure 4. Effect of Phosphate Ions Cap-
tured during Precipitation of Metallic
palladium on Catalytic Activity of the
latter
Curve 1 represents the catalytic decomposition of hydrogen peroxide.
Curve 2 represents the catalytic hydrogenation of ethylene. The concentra-
tion of phosphorus with reference to the weight of palladium is plotted
along the axis of the abscissae.
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