April, 1963 HYDROLYSIS OF URANIUM(VI) 82 1

more negative than -15.5.64760 Kote that the lack of AHf(SiOz), which is independent of the data for silica,
agreement among these studies is independent of the do not agree with each other within their estimated prc-
heat of formation of Si02. cisions. (For comparison with the results given in the
Consider also the two studies which appear to involve previous paragraph the studies of Humphrey2* and of
silica in t,he determination of the heat, of formation of TaylorR1 give, with OUT value of AI l f0298 (SiO,, a-quartz)
silicon carbide. From the combustion mrasurrincnts AWfoZg8 (Sic, cub.) = -20.9 f 0.9 and -15.%j
of FIumphrey28 for the reaction f 1.1 kcal. mole-I, respectively).
From the foregoing discussion it is clear that there
exist unknown sources of error in some of the measure-
SiC(cub.) + 202 =SiO, + CO,
(9A)
meobtain AHfnZg8 (Sic, cub.) - AHf0298 (SiOz, a-quartz)
=+196.86 f 0.88 kcal. From t,he equilibrium pres-
sure measurements of TaylorG1 for the reaction
ments leading to the above values of the heat of forma-
tion of silicon carbide. A critical redetermination of
the heat of formation of silicon carbide by calorimetry
should shed light 011 these discrepancies.
IV. I n conclusion. we find that the value for the heat
Si02 + 3C(graphite) =SiC(cub.) + 2CO(g)
(10A)
we obtain by the third law (after a minor correction for
the Presence of in the gas) aHf0z9e (sic, Cub.)
-AHf0298 (SiOz, a-quartz) =+201.9 * 1.1 kcal. It is
obvious that these values of the quantity, AHf(SiC) -
of formation of a-quartz presented in this work is in
good agreement with all the high temperature equilib-
rium measurements on substances which appear to be
reasonably well characterized. Thus, the discrepancies
( 00) . J . Smiltens, J. Phvs. Chem. , 64, 368 (1960).
D. A. R. Kay and J . Taylor, ibid., 66, 1372 (1960).
discussed by Chipman (except those involving Sic)
appear to be substantially resolved.
( 01) J . D. Baird and .I. Taylor, Trans. Faraday Soe., 64, 526 (1958);
HYDROLYSIS OF URANIUM(V1) : ABSORPTION SPECTRA OF CHLORIDE AND
PERCHLORATE SOLUTIOKS1
B Y RI CHaRD bf. RUSH AND J AMES 8. J OHNSON
Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee
Received September 21, 1962
Optical absorptions of hydrolyzed U(V1) solutions in 1 M chloride have been measured for U(V1) concen-
trations in the range 0.001-0.1 M and for values of n (average moles of hydroxide bound per mole of U(V1)) up
to 1.3. The molar
absorptivity E increases sharply with n; chloride complexing of the unhydrolyzed species and at least one hy-
drolyzed species is indicated by higher values of E in chloride solutions than in perchlorate solutions with the
same n. The chloride measurements are correlated with a hydrolysis scheme previously derived from ultra-
centrifugation and acidity measurements. These results are combined with acidity measurements and spectra
in perchlorate media to give values of the formation quotients for hydrolytic species in perchlorate media.
The results are consistent with the earlier indication that the species (UO~)Z(OH)~+~, which appears to be present
in substantial amounts in 1 M chloride, is of little, if any, importance in 1 A+' perchlorate.
A few measurements have been carried out for 1 N perchlorate solutions with n up to 1.0.
I n a recent publ i cati ~n,~ we presented a hydrolysis
scheme for U(V1) in one molar chloride, which was con-
sistent with acidity measurements and with ultra-
centrifugation estimates of molecular weights (25').
The major species proposed were (UOz)z(OH)2+2,
(UOZ)~(OH)~+~, and (UOZ)~(OH),+. Formation quo-
tients were given for these species. A scheme, similar
except that it did not include (TJ02)3(OH)4+2, based
on literature acidity measurements3 carried out at 20',
was also presented for one molar perchlorate solutions.
Although the species as written do not indicate com-
plexing of other ligands present in the solution, from the
fact that (UO&(OI)4+z appeared to be of importance
only in chloride solution, presumably this species in-
cludes complexed chlorides and it seemed possible that
other species also complexed anions.
We have recently carried out optical absorption
measurements of hydrolyzed uranyl solutions in chlo-
ride and perchlorate media. I n this paper we attempt
to correlate the spectra of the chloride solutions with
(1) This document is ba3ed upon work performed for the United States
Atomic Energy Commission at the Oak Ridge Xational Laboratory, oper-
ated by Union Carbide Corporation.
(2) R. M. Rush, J. S. J ohnson, and X. A. Kraus, I n o i v . Chem., 1, 378
(I 962).
(3) S. Ahrland, Acta Chem. Scand., 8, 374 (1949).
the hydrolysis scheme earlier reported. From the
species absorptivities thus obtained, plus the spectra
and acidity measurements in the perchlorate media, we
have estimated formation quotients for the hydrolyzed
species in 1 M NaC104.
Experimental and Computational
Procedure
Spectra of solutions having the following hydroxyl numbers n
(average number of hydroxyls bound per uranyl) were measured:
1 M in total chloride (with Ea+): 0.1 M U(V1)-n =0.38,
0.67, 0.90; 0.01 &f U(VI)---n =0, 0.12, 0.21, 0.30, 0.42, 0.51,
0.61, 0.71, 0.79, 0.89, 0.98, 1.07, 1.21, 1.30; 0.001 M U(V1)-n
=0.45, 0.73, 0.99, 1.21. I n 1 M total perchlorate (with Xa+):
0.1 M U(V1)-n =0.42; 0.01 M U(V1)-n =0, 0.43, 0.62,
0.81; 0.001 M U(VI)-n =0.45, 0.64, 0.82, 1.00.
Interpretations are based on measurements in the range 3650-
5000 A. , carried out on a Gary Model 14 PM spectrophotometer;
cells were of 0.5, 1, 2, 5, or 10 em. path length. This instrument
gives a recording of the absorbance of the solution, A =log
( I o/ I ) , I being intensity of light transmitted by the solution and
10, of that transmitted by a reference solution (1 M KaCl or
1 M NaC104). From these values, the molar absorptivities E
=A/ c b are obtained, where c is the total stoichiometric U(V1)
concentration (moles/l.), and b is the path length in cm. The
molar absorptivity is related to the species absorptivities,
e,,,, by the equation
822 RICHARD AI. RUSH AND J AMES S. J OHNSOS Vol. 67
where ci.j is the concentration of the species (UO,),(OH)j+(Zl- j )
(complexing with other ligands being ignored), Fi,j =ici,j/c is
the fraction of total uranium found in the (i,j) species, and
di , j =~i ,i /i .
I n the computational procedure, the species fractions Pi, j are
computed from the formation quotients of the scheme being
tested, for the hydroxyl number and total U(V1) concentration
of the solution being considered. The formation quotient kl, j is
defined as
(kOi,j being the formation constant, Gi,j the appropriate activity
coefficient ratio, and brackets indicating concentration in moles/
1.). For a given solution the hydrogen ion concentration CH and
free uranyl concentration c1 , are obtained from the hydroxyl
number n and the formation quotients ki,j by solving the follow-
ing equations by the h-ewton-Raphson method
The species concentrations c ~ . ~ and fractions F,,j are then calcu-
lated from CLO, CH, and the formation quotients. With these
fractions for each solution in a given medium (chloride or per-
chlorate), values of at a given wave length for each hydro-
lyzed species are calculated to give the minimum sum of squares
deviation4 of the values of E for all of the solutions. The values
of 1.0 are obtained from the spectra of an unhydrolyzed solution.
The program also computes the standard error in each e l l t J and
the deviations between observed E and values computed by equa-
tion l . Computations were carried out on an I BM 7090 com-
puter.
The criterion for correlation is the degree of success with which
the observed spectra of individual solutions can be reproduced
from the values of el L, , obtained in the manner described.
Equilibrium quotients for the same conditions as the measure-
ments on perchlorate solutions (25, 1 M KaC104) were not avail-
able. Estimates of these values were made in a manner to be
described in detail below with the help of separate measurements
of the solution acidities. The correlation of the absorption
spectra was then tested as with the chloride solutions. Acidity
measurements were carried out by the technique described pre-
viously2 with the cell
glass electrodel 1 (UOz(OH),+(2-n), H+, Xa+)C104-
(1 J l)jHCl (0.01 M) , HClOd (0.01 M) ,
NaC104 (0.98M), AgCl(s); Xg(s)
Results and Discussion
1. Results-The general features of the absorption
spectra can be seen in representative curvoes given in
Fig. 1 5 (measurements were made to 5500 A. at which
point the absorption was negligible indicating the
absence of serious turbidity). The values of E in-
crease sharply with hydroxyl number, and the position
of maximum absorption shifts to longer wave length in
both chloride and perchlorate media. Similar results
have been reported in perchlorate by Sutton.6 Chlo-
ride complexing of the unhydrolyzed species is in-
(4) We are indebted to &I. H. Lietzke for use of his Fortran generalized
least squares subroutine; see U. 8. Atomic EnerRy Commission, ORNL-
3259 (1962).
(5) Those interested in a more detailed presentation of the primary data
are referred to R. M. Rueh, J. S. Johnson, and K. A. Kraus, U. S. Atomic
Energy Commission, ORNL-3278 (1963).
(6) .J. Ruttcn, J . Chem. Soc. , S275 (1949); see also National Reuparch
Council of Canada, Atomic Energy Project, Division of Research, CRC
325 (K. R. C. No. 1612) (1947).
WAVELEVSTH, anqstroms.
Fig. 1.-Absorption spectra of 0.010 M U(V1) solutions in 1 1%
total chloride (--- ) and 1 M total perchlorate (- - - -) at 25.
I r y - 1 -1
80- -I
4000 4500 5000
WAVE 1. ENGTH , o nqs t rom s.
Fig. 2.-Species molar absorptivities for U(V1) species in 1 M
total chloride: equilibrium quotients used are k z , ~ =6.7 X IO-,
ka,a =4.7 X l O-l 3, and kj,s =1.0 X lo-; vertical lines indicate
one standard error on each side of the value.
dicated by the difference in spectra at n =0, and of at
least one hydrolyzed species by the greater absorption
in 1 M NaCl than 1 M KaC104 at a given n. Since
free chloride is nearly constant in all experiments, the
ratios of species of a given (i,j) which are complexed to
different extents by chloride will be essentially constant
and the values of Ei,j will be a composite for species
2. Uranyl Spectra in 1 M Chloride Solutions.-In
the interpretation2 of our acidity measurements of
U(V1) hydrolysis, the simplest scheme giving an ade-
quate fit involved the hydrolyzed species (UO&(OH)z+2,
(UOn) i(0H) jCl~+(2i--1).
April, 1963 HYDROLYSIS OF URARIIUM(VI) 823
( U~Z) ~( OH) ~+~, and (U02)3(OH)sC; these species (as
well as the unhydrolyzed uranyl) may further complex
chloride ions. An equally satisfactory fit was obtained
if the species U02OH+was included. Although there
is some evidence from other studies for this species,
especially at higher temperatures,$ it does not seem to
us conclusive at the temperature and concentration
range of our studies. I n any case, the formation
quotients we obtained indicated that, if present, it did
not constitute a major fraction of total U(V1) under the
conditions of the present study, and we have therefore
neglected it for the most part in this discussion.
The formation concentration quotients which we
obtained2 for the scheme without the (1,l) species are
as follows: kz, z =6.7 X lo-, ka, r =4.7 X and
1c3,5 =1.0 X If the (1,l) species is included,
the other quotients are modified slightly.
The values of the species absorptivities, obtained by
computing the concentration of the individual species
with the above scheme, and finding the values of e i , j
which give the best fit to the observed spectra for all
solutions (see Experimental section) are given in Fig. 2.
Vertical lines given at representative wave lengths in-
dicate one standard error in on each side of the
best value.
Correlation is illustrated in Fig. 3 as deviations of ob-
sewed values of E from those computed for individual
solutions. Most 0.1 the deviations represent less than
one chart division (0.01 at A) on the recorded spectrum.
I n the most notable exception, 0.1 M U(VI), n =0.899,
A was very high (up to 2 ) , and the computed values are
within 2% in A where the deviation is greatest.
Inclusion of the (1,l) species modified the values of
e i , j for the other hydrolyzed species shown in Fig. 2
slightly; the over-all fit corresponding to Fig. 3 was
about the same.
3. Uranyl Spectra in 1 M Perchlorate Solutions.-
The equilibrium quotients2 derived on the basis of Ahr-
lands acidity mearurements in perchlorate media3
are not strictly applicable to the interpretation of the
spectra reported here, since Ahrlands measurements
were at 20. Our interpretation of his results had
indicated that the (3,4) species is not present in im-
portant amounts in perchlorate solutions. From this,
it is reasonable to suppose that this species includes
complexed chloride ions. If it is further assumed that
the ( 2, 2) and (3, 5) species do not complex chloride, and
that the values of E ~ , ~ and e3,5 are the same in chloride
and perchlorate media, the following expressions are
obtained which ma:y be solved for the fractions Fi ,j of
the various species (qO is known from measurements
on an unhydrolyzed solution)
n Fw + (5/3)F3,5
8 =Fi,oci,o + F2,zez,z -I- F3, 56 3. 5
1 =Fi9o + Fz,z + F3,6
(5)
Further, since
(7) See, e.& J. Rydberg, .Arkiv Kemi , 8, 118 (1956).
(8) (a) C. F. Baes, J r., and N. J . Meyers, Inorg. Chem., 1, 780 (1862); see
also (b) K. A. Kraus, Hydrolytir Behavior of the Heavy Elements, Pro-
ceedings of the I nternational Conference on the Peaceful Uses of Atomic
Energp, Vol. 7, p. 245, Session 10B.1, P/731, United Kations (1956).
O P r
0.980
*w*- n***-.e*
O I =**-
* . .
- 0 6
1.205
.
/ / , I , I / , / , ! I
1
3500 4000 4500 5000
WAVELENGTH, angstroms.
Fig. 3.-Deviations of observed molar absorptivities for U( VI )
solutions in 1 M total chloride from values based on kz,z =6.7 X
k3,a =4.7 X 10+s, and ka,s =1.0 X lo-. Numbers to
the right of each plot are the hydroxyl numbers; vertical lines
at the left of each plot represent 0.005 in A, symbols represent
M U(V1)as: A, 0.1; 0, 0.01; m, 0.001.
from the optical absorption of a single solution at one
wave length, values of ki,j may in principle be obtained,
if the acidity of the solution is also measured. I n
practice, of course, the solutions must be selected to
have an appreciable amount of all species present.
We have carried out such measurements with eight
solutions, and the quotients evaluated at 4300 A. are
listed in Table I. Agreement between the values ob-
tained from the individual solutions is about as good as
could be expected. The acidity measurements on the
824
80
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W
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RICIUHD 31. RUSH BND J AMES 8. J OHNSON Vol. 67
0,420
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TABLE I
EQGTLIRRIUM QCOTIENTS OBTAINED FROM SPECTRA AXD ACIDITY
MEASUREMENTS IN 1 M TOTAL PERCHLORATE
E ke,n ka,a
F n --log [R"I (4300 A. ) x 10' x 10'7
0.1000 0.420 3.322 13.26 1.33 4.07
,0099s .429 3.833 14.58 1.12 4.06
,01007 ,623 3.996 20.95 1.13 4.05
.Ol005 .806 4.137 28.46 1.13 3.87
.000996 ,454 4.299 17.17 1.06 4.28
.001004 .638 4.434 24.00 1.05 3.54
.001002 ,816 4.548 31.64 1.05 3.35
.001011 1.003 4.652 39.76 1.34 4.16
Av. 1.15 3.92
- -
Values obtained from least squares fit
of acidity measurements alone ( u =
0.0107 in n) 1.22 3.69
XOTE: At 4300 A. e1.0 =5.233 from unhydrolyzed perchlorate
solution and ~ ' 2 . 2 =23.34, e' 3,6 =77.59 from measurements in
chloride solution (Fig. 2).
The assumptions made in interpreting the absorption
data were tested by correlating the spectra for all wave
lengths in the same manner as with the chloride solu-
tions, with the constants k ~ , ~ =1.15 X and I C ~ , ~ =
3.9 X lo-''. Comparison of the values of d Z , 2 and
d 8 , 5 obtained from chloride and perchlorate for all wave
lengths is shown in Fig. 4, and the deviations between
experimental and computed values of E for perchlorate
solutions are shown in Fig. 5. The agreement is
coiisistent with the assumption that the (2,2) and (3,s)
species do not complex chloride.
The values of kz,z and of k3,G are somewhat smaller in
chloride than in perchlorate. This direction is ex-
pected if UOz+z is complexed by chloride, in agreement
with the conclusions of many pe~pl e. ~ More quantita-
tively, if the only important complex of the unhy-
drolyzed species is UOzC1+, if the values of Gi,j are as-
sumed to be the same in the two media, and if no
chloride complexing of the (2,2) or the (3,5) occurs,
the ratio of the apparent quotients for the tu70 media
should be
where kl,o,l =[UOzCl+]/ [U02f2] [Cl-1.
An estimate of kl,o.l can therefore be made from com-
parison of the apparent values of ki,j in chloride and per-
chlorate media. From such a comparison of the
quotients for the (2,2) species, kl,o,l =0.35 is obtained;
from the (3,5) species, kl,o,l =0.52. These may be
compared with the value of Nelson and Kraus,lo cor-
rected to M =1, kl,o,l =0.50. With the assumptions
made, the agreement between these values is good.
Discussion.-The optical absorption of hydro-
lyzed U(V1) chloride solutions seems to be con-
sistent with the species postulated, and the formation
quotients evaluated, to explain acidity and ultracentrif-
ugation results.2 Analysis of the chloride and per-
chlorate spectra support the conclusion based on
acidity data that the (3,4) species, which is important
in chloride, is not very important, if present at all, in
perchlorate. The values of the equilibrium quotients
derived for perchloratme solutions are reasonable. They
4.
(9) .J. Bjerrum, G. Schwarzenbach, and L. G. SillBn, "Stability Con-
(10) F. Nelson and K, A. Hraus, J. Am. Chem. Xoc,, 73, 2157 (1951).
stants." Part 11, The Chemical Sooiety. London, 19.58.
ApriI, 1963 I ONI ZATI ON OF a-PARTI CL ES I S BINARY GAS 3hXTURES 825
are somewhat greater than those estimated from 20
acidity data; however, this is the direction expected,
and of the approximate magnitude predicted, from
studies of the temperature coefficient of U(V1) hy-
drolysis in nitrate medium.*a
The question of the importance of other species which
may be present in minor amounts is no more resolved
by the present results than by the earlier study. For
example, it was apparent that about as satisfactory an
interpretation could be obtained with a scheme in-
cluding UOzOH+, although there would be consider-
able uncertainty in the values of el , l . Similarly, our
conclusions for the perchlorate solutions agree in gen-
eral with those of SuttonJ 6 though he includes a small
contribution of the (3,4) species.
The most important point of disagreement with the
interpretation of acidity measurements on a core-link
modelll seems to be resolved, since the St>ockholm
group now postulate an important contribution by the
(3,5) species, which is not of the core-link type.l2
They still postulate the presence of several higher core-
link species, for which we do not find any evidence in
our results, but since the constants quoted for these
species are rather low, the remaining disagreement is
perhaps more in a conceptual model of hydrolysis
rather than in a practical description of U(V1) solution
chemistry. From a recent publication,13 it appears
that even this disagreement may no longer exist.
Acknowledgment.-We wish to express indebtedness
to Kurt A. Kraus for many helpful and stimulating dis-
cussions and to Neva Harrison for technical assistance.
(11) S. Ahrland, S. Hietenan, and L. G. SillBn, Acta Chem. Scand., 8,
(12) L. G. Si l l h, private communication.
( 13) L. G. SillBn, Acta Chem. Scand., 16, 1051 (1962).
1907 (1954).
IONIZATIOK BY ALPHA PARTICLES IS BINARY GAS MIXTURES
BY T. D. STRI CKLER~
Health Physics Division, Oak Ridge Nat i onal Laboratory,, Oak Ridge, Tennessee, and Department of Physics, Berea College, Berea, Kent ucky
Receiiied September 31, 196W
The W value (average energy loss per ion pair) for a-particles has been measured in a number of binary gas mix-
tures of molecular gases as a function of the fractional pressures. The W of the mixture ( Wij) can berepresented
in terms of the 14s of the pure constituent gases Wi, Wj) and the fractional pressures ( Pi , Pj ) by the relation:
Wij =(Wi -- Wj)Zij +Wj, where Zij =Pi/(Pi +f i j Pj), in whichfij is a constant determined empirically for
each pair of gases. These constants verynearly satisfy the relationshipfij =fj/fi =(fj/fk)/(fi/jk) =jkj/jki,where
i, j , and k refer to any three gases. Thus, if the followingj-values are assigned to the gases in this study (Nz, 1;
COz, 1.8; H,, 0.5; 02, 1.3; CH,, 1.8; CeH4, 3.4; GH6, 3.5; CJ&, 4.5; C,Hs, 4.5; C9H8, 6.3) then the constant
f i j determined from the ratio of any two of these will serve to predict the W of any mixture of these two gases with
an accuracy better than 1%. Slight departures from the W predicted by the above equation have been noted
in the case of nitrogen mixtures, indicative of an effect similar to that observed in the noble gases when small
amounts of impurities are added.
Introduction
If an a-particle of kinetic energy Eo is completely
stopped in a gas, a,nd in becoming stopped produces
Ni ion pairs, then the mean energy lost per ion pair
E,/Ni is commonly called the W of the gas for a-
particles. The W of most gases lies in the range 20 to
46 e.v. per ion pair and in many cases is found to be
practically independent of the energy of the initial
ionizing particle.
The practical importance of W (in the measurement
of radiation dose, in the calculation of energies of parti-
cles in nuclear reactions, and in the interpretation of
radiation-induced chemical reactions) and its theoretical
significance have been pointed out in many recent publi-
cations on the ~ubj ect.~
I n the case of binary mixtures of gases, two distinct
phenomena have been observed. One is the marked
increase in ionization, and consequent decrease in W,
when small amounts of some gases are mixed with the
noble gases. This has been studied by J esse and Sadau-
ski^^-^using helium and neon, and by Melton, Hurst,
(1) Dent. of Physics, Berea College, Berea, Kentucky.
(2) Operated by Union Carbide Corporation for the U. S. Atomic Energy
Commission.
(3) (a) S. C. Curran and J . M. Valentine, Rept. Progr. Phys., 21, 1
(1958); (b) W. Binks, Acta Radiol., Splppl., 117, 85 (1954); (c) R. L. Platz-
man, NAB-National Researoh Council Publication 752, 109 (1960).
(4) W. P. J esse and J . Sadauskis, Phys. Rev., 88, 417 (1952).
(5) W. P. J esse and J. Sadauskis, kbid., 90, 1120 (1953).
(6) W. P. J esse and J. Saudauskis, ibid., 100, 1755 (1955).
and Bortner using argon. The effect is attributed, in
part, to the excitation of the metastable level in the
noble gases and the subsequent ionization of the
impurity (by interaction with the excited atom),
provided the ionization potential of the impurity is
lower than that of the metastable state. This has been
referred to as the J esse effect.8 The fact that in-
creased ionization occurs in argon, even when the im-
purity has an ionization potential greater than that of
the metastable level, has been demonstrated by
Melton, Hurst, and Bortner, but the explanation of the
effect is not entirely clear.
On the other hand, in the molecular gases, the W of
the mixture is found to lie between the extreme values
for the pure gases and to change smoothly from one
limit to the other as the composition of the mixture is
changed. This has been studied by Huber, et U Z . , ~ ~ ~ ~
and by Hurst, et uZ.11--13 It has been shown that the
W of any mixture of two of these gases can be expressed
(7) C. E. Melton, G. S. Hurst, and T. E. Bortner, ibid., 96, 643 (1954).
( 8) R. L. Platzrnan, The Physical and Chemical Basis of Mechanisnis in
Radiation Biology, Radiation Biology and Medicine, W. D. Claus, Ed.,
Addison-Wesley Publishing Co., Inc., Reading, Mass., 1958, pp. 15-72.
(9) P. Huber, E. Baldinger, and W. Haeberli, Hel u. Phyg. Acta, 23, Suppl.
111 (1949).
(10) W. Haeberli, P. Huber, and E. Baldinger, ibid., 26, 145 (1963).
(11) T. E. Bortner and G. S. Hurst, Phys. Rev., 93, 1236 (1954).
(12) H. J. Moe, T. E. Bortner, and G. S. Hurst, J. Phya. Chem., 61, 422
(13) G. S. Hurst and T. D. Strickler, NAS-National Researoh Council
(1957).
Publication 752, 134 (1960).