Journal of Fusion Energy, 5, No.

3, 1986

Research Note

Lithium Nitrate As a Fusion Reactor Coolant Fluid?:

A Thermochemical Assessment

M . G. Adamson, 1 D. Calef, 1 and R. W. Moir 2

Received June 26, 1985; revised September 24, 1985

In connection with possible application as a coolant fluid in fusion reactors, molten LiNO3
and LiNO3/LiNO2 mixtures, and their mixtures with N a / K nitrates, have been evaluated
with respect to their high temperature stability, their ability to reversibly dissolve and[ release
tritium and, in a very limited sense, their corrosiveness toward structural alloys. The results of
the primarily thermochemical evaluation indicate that with respect to thermal/radiolytic
decomposition and corrosivity LiNO3/LiNO 2 may be suitable for application up to - 700~
however, with respect to reversibility/irreversibility of tritium release, it appears unsuitable at
all likely operating temperatures ( - 675-800~

KEY WORDS: lithium nitrate; coolant fluid; fusion reactor.

1. I N T R O D U C T I O N required of truly high temperature coolants. ''(1~ In

Alkali metal nitrate/nitrite mixtures (MNO 3-
MNO2; where M = Li, Na or K) have been consid-
ered as candidate coolant materials for fusion reac-
tors. (1- 3)
Although liquid Na and K nitrates meet several
important performance requirements for fusion reac-
tor coolant/blanket fluids, the Na and K tend to
activate rather easily, producing undesirable radia-
tion levels in working fluid. On the other hand, the
corresponding Li salt reduces this activation and
offers the potential attraction of enhanced tritium
breeding capability. Unfortunately, the Li salt is less
well-characterized in terms of thermal/chemical sta-
bility, corrosiveness toward structural alloys (chem-
ical compatibility), and its ability to reversibly dis-
solve and release tritium. In fact, Grimes and Cantor
stated " L i N O 2 and LiNO 3 lack the thermal stability
1Chemistry" & Materials Science Department, Lawrence Livermore
National Laboratory, P.O. Box 5511, Livermore, CA 94550.
2Magnetic Fusion Energy, M Division, Lawrence Livermore Na-
tional Laboratory, P.O. Box 5511, Livermore, CA 94550.
247
addition, somewhat contradictory statements have
been made about the lithium salt's ability to dissolve,
and subsequently release, water. (2'3~ Despite these
caveats, there has been continued interest in LiNO 3-
LiNO2 either as a blanket or as a coolant. (3~
Because of the incomplete and fragmentary na-
ture of the experimental database for molten Li
nitrate and continuing uncertainty about its high
temperature behavior, we undertook a limited
thermochemical evaluation of this material, focusing
primarily on the key technical issues of chemical
stability and reversibility of tritium dissolution and
release. The purpose of this communication is to
briefly report the results of our assessment.
2. BACKGROUND AND REVIEW
Qualitative observations of gaseous L i N O 3 /
LiNO a decomposition products at temperatures
in the range 493-1000~ have been reported by
Buchler and Stauffer, (4) Kramer et al., (5~ and
Krasnovskaya et al. (6~ The latter two papers con-
centrated on measuring rates of
0164-0313/86/1200-0247505.00/09 PlenumPublishingCorporation
248 Adamson et al.

decomposition/evaporation and did not report equi- Table I. Evaporation/DecompositionThresholdTemperaturesfor

librium partial pressure data; Kxamer studied dy- Lithium, Sodium, and Potassium Nitrates~
namic evaporation into an active vacuum; the Rus- Material Tm, K Te,Kb Ta(N2),Kc Ta(NO),K
sian workers studied decomposition under pressure LiNO 3 537 704 650 598
of the product gases. Earlier work on the thermal NaNOB 580 738 714 688
decomposition of liquid LiNO3 and LiNO 2 has also KNOB 607 723 710 706
been reviewed by Stern(7~ and is mentioned in vari-
ous compilations of molten salt thermophysical prop- aSource: From Kramer et al. (5)
erties. (8,9~ In his assessment, Stern included some bTe: Temperature at which evaporation rate is 0.1 mg cm-z
rain- 1.
thermochemical calculations of the O2, NO, and NO 2 CTa: Temperature at which the indicated gaseous species was first
"equilibrium" pressures over LiNO 3 at 300-600~ observed mass spectrometrically.
these calculations being based on reactions 2 and 8
below. Analogous calculations were also performed
for N a N O 3 and KNO 3 up to approximately 1000~ and (in the gas phase)
LiNO 3 (mp = 537~176 and LiNO 2 (mp =
493~176 evaporate and begin to decompose at NO 2 = NO + 1 / 2 02 (8)
lower temperature than the corresponding Na and K
salts; comparative behavior of the nitrates is il- 2NO = N 2 + 0 2 (9)
lustrated in Table I which was abstracted from
Kramer et al.(5) et cetera. The various equilbria consist of forward
In order of decreasing partial pressure, at tem- and reverse reactions which proceed concurrently yet
peratures in the range 600-800~ the following their rates have different temperature dependencies;
vapor species have been identified above liquid this causes different reactions, and hence products,
LiNOB: O~ > N 2 > NO - NO 2 > LiNO 3 - (LiNO 3) 2 to predominate in different temperature regimes. For
> (LiNO2) 2 > LiNO 2. LiNOB-LiNO 2 mixtures thermal decomposition be-
The foregoing studies suggest that evaporative gins as low as 565~ (292~ but N2 is not seen as a
decomposition of pure LiNO 3 (1) in a closed system product until the temperature exceeds 650~ (377~
will eventually lead to a complex quasi-equilibrium As T increases above this threshold, N 2 increases as a
mixture consisting of the various vapor species plus a gaseous product at the expense of NO z and, second-
condensed phase of LiNOB-LiNO2 (1) and Li20 arily, NO. As Stern has noted, (7~ under purely ther-
(solid or d i s s o l v e d ) . Overall decomposition, and the mal conditions (T <1000~ reactions involving
resulting quasi-equilibrium, may be represented by a molecular N 2 - f o r example (4) and (9)--appear very
combination of reactions such as: slow relative to easily reversible reactions such as
(2) or (8). In fact, all the reactions that lead to N 2 as
LiNO 3(1) = LiNO2(1 ) + 1 / 2 0 2 (1) a product are highly favored thermodynamically,
hence these same reactions must be inferred to be
2LiNO3(1 ) = Li20(s or dis) kinetically limited. Because high n, 3' radiation fields
have the ability to accelerate gas phase reactions that
+ 2NO 2 + 1 / 2 O 2 (2)
involve N 2 (via radiolytic production of " h o t " atoms
LiNO2(1 ) + N O 2 = LiNO3 (1) + N O (3) and/or ion molecules), o~ and because fusion reactor
blanket materials and coolants will be exposed to a
2LiNO3(1 ) = Li20(s or dis) high radiation field at relatively high temperatures,
our view is that equilibria involving molecular N 2
+ N 2 + 5 / 2 02 (4) must be considered in any conservative evaluation of
nitrate coolant "thermal" stability.
2LiNO2 (1) = Li 20(S or dis) + NO + NO 2
(5)
3. METHOD AND APPROACH
Li20(s or dis) + 2NO 2 = LiNO2(1 ) + LiNO3 (1) (6)
2LiNO2(1 ) = Li20(s or dis) In principle, knowing the Gibbs energies of for-
mation of all reactants and products as functions of
+ N 2 + 3 / 2 02 (7) temperature, and subject to certain compositional
Lithium Nitrate
constraints for the condensed phase, the equilibrium
composition of a multiphase, multicomponent system
may be calculated at a specified temperature. (11'16)
This Second Law method yields equilibrium partial
pressures for gaseous constituents and chemical ac-
tivities for condensed phase constituents. Often, the
total pressure, or one or more partial pressures or
condensed phase activities, are prespecified. Our ap-
proach was to apply this method to the LiNO 3-
LiNO2, NaNO3-NaNO2, and KNO3-KNO 2 systems
and then compare predicted decomposition pressures
for comparable degrees of decomposition at a repre-
sentative temperature. On the basis of the recent
Blanket Comparison and Selection Study, (3~
700~176 was selected as the threshold for use-
ful high temperature operation, and 800~176
was assumed as a realistic upper operating limit.
Selected equilibria were computed over a somewhat
wider range--600 to 900~ properly evaluate
the effect of temperature.
Since the available thermodynamic functions for
M N O 3 and MNO 2 (M = Li, Na, and K) only refer to
low temperatures, and in certain cases are estimated,
we chose to neglect heat capacity corrections for
these species in the equilibrium calculations. Instead
we used the approximation AG~176
TAS~ to describe the T-dependence of the Gibbs
energies of formation AG~ This approximation
has been shown to be acceptable in a variety of
calculated gas-condensed phase equilibria in nuclear
fuel systems, (12'13~ even at temperatures as high as
1200~ (It is acceptable in the sense that uncertain-
ties for condensed phase reactants and products tend
to cancel out.) The principal sources of thermody-
namic data used for our calculations were the JANAF
Tables, (14) NBS Technical Note 270-8, (15~ and refs. 7
and 11.
Two approaches were taken in calculating de-
composition pressures over MNO3-MNO 2 systems:
(a) allowing the formation of molecular N 2 as a
gaseous reaction product, and (b) not allowing its
formation. As will be seen, allowing N 2 to form as a
product has a rather dramatic effect on the predicted
decomposition pressure. For calculations on MNO 3-
M 2 0 - M O H - H 2 0 equilibria, which were used to
evaluate the reversibility of tritium dissolution and
release, the activity of hydroxide reaction product
(aMolO was determined as a function of water activ-
ity (aH2o) at two representative temperatures. The
magnitude of the constant relating aMoH and aR~o
is a measure of the relative stabilities of MOH (dis)
and H 2 0 (dis).
249
Equilibrium calculation were performed both
manually and on an IBM PC using a floppy disk
version of the computer code SOLGASMIX-PV. (15'16)
Preliminary calculations showed that the pressures of
many gaseous species (for example: N, O, M, MNO,
N203, N204, N205, and N20 ) were trivially small at
T < 800~ consequently these species were omitted
in subsequent calculations. An inert diluent (argon)
was included as a species in the SOLGASMIX calcu-
lations; this served the dual purpose of fixing or
adjusting the total system pressure.
4. RESULTS AND DISCUSSION
4.1 Thermal Decomposition Pressures
Preliminary calculations performed at 800~ for
a specified composition of condensed phase (i.e., 50%
decomposition in reactions 1, 2, and 4) indicated that
the LiNO 3 decomposition pressures for "case a" (N 2
allowed) were several (> 2) orders of magnitude higher
than the corresponding "case b" (no N 2 allowed)
pressures. Stern's calculations for Li, Na, and K
nitrates refer to "case b" with special restrictions on
the condensed and gas phase compositions. In order
to compare Stern's predicted decomposition pres-
sures at 800~ we extended his calculations for
LiNO 3 to 800~ using a standard logP (or Keq ) -
1/T extrapolation. The resulting "equilibrium" pres-
sures at 800~ are compared in Table II. From these
results, it is clear that LiNO 3 is considerably less
stable than NaNO 3 and KNO~. However, it should
be noted that somewhat higher pressures were ob-
tained for "case b" decomposition using SOLGAS-
MIX free energy minimization calculations; this is
believed to be the consequence of removing Stern's
somewhat artificial compositional constraints.
For "case a" decomposition, which represents
the least restrictive equilibrium condition, N 2 was
included as an additional reaction product and the
Table II. Comparison of Stem's Calculated Decomposition
Pressures for LiNO3, NaNO3, and K N O 3 at 800~ and 50%
Decomposition
m
Partial pressure (atmospheres)
Material 0 2 NO 2 NO Total
LiNO 3 3• -3 9• -5 3.0• -3 6.3 • -3
NaNO 3 9• -6 2• -8 1.2• -s 2.1• -5
KNO 3 4• 8 7• 5.0• 9.0• 10-8
m
250
Table IlL Comparison of " C a s e a" Decomposition Pressures for Molten Li, Na, and K Nitrates
at 700 and 800~
Material
LiNO 3
NaNO 3
KNO 3
total decomposition pressures ( -- Po2 + PN2 + PNo +
PNo2) recalculated for each nitrate. In the absence of
reliable phase equilibrium data it was assumed that
MzO reaction product dissolves in the MNO3-MNO 2
melt, a condition which tends to maximize the de-
composition pressures. The resulting uncertainty is
the primary contributor to the estimated absolute
error on our calculated decomposition pressures; this
error has a maximum value of + 50~ However, it
should be pointed out that comparisons of calculated
decomposition pressures are subject to considerably
lower uncertainties (+ 5 to 10%). The results of "case
a" calculations performed at 700 and 800~ are
summarized and compared in Table III.
Pressure ranges are shown in Table III for each
material because in these systems the decomposition
pressure is not uniquely defined by temperature
(according to the Phase Rule, the number of degrees
of freedom F equals 5-P, where P = 2 or 3). Com-
plete definition requires specification of at least one
compositional parameter--in this case either the fi-
nN composition of the condensed phase or the sys-
tem mass :volume ratio. In Table III the highest
pressure results from > 1.5% decomposition and the
lowest pressures from 50% decomposition.
The "case a" results confirm that LiNO 3 is
considerably less stable than NaNO 3 or KNO 3 and,
although the relative pressures parallel those predic-
ted for "case b," the absolute pressures are consider-
ably higher. In fact, for LiNO 3 the decomposition
pressure is predicted to lie in the range 20-70 atm
(2-7 MPa) at 800~ Pressures of this magnitude are
generally undesirable in flowing liquids--especially
highly oxidizing liquids--because they dictate im-
position of stringent mechanical and safety require-
ments on the containment.
The temperature dependence of the "case a"
decomposition pressure of L i N O 3 w a s alSO calculated
at a constant percent decomposition ( - 1.5%). These
maximum decomposition pressures are summarized
in Table IV.
Adamson et al.
(Upper and Lower P Limits)
Decomposition pressure, P% + PN~ + PNo + PNo2(atms)
700~ 800~
11.6 to 30.7 22.5 to 69.5
2• -3 to 0.17 0.15 to 1.12
1 X 1 0 - 4 to 3 • 1 0 - 3 4 • 1 0 - 4 to 0.02
Table IV. T e m p e r a t u r e D e p e n d e n c e of the " M a x i m u m "
Decomposition Pressure of LiNO 3 (% Decomposition = 1.5 +_.1)
i
Temperature (~
600 700 800 900
Pressure (atms) = 21.4 30.7 69.5 246
Table IV shows that the relative advantage of
reduced total pressure upon lowering temperature
appears to decrease with temperature; from 700~ to
600~ for example, the pressure drop is only mod-
erate while the absolute pressure remains quite high.
However, this relatively small advantage may be
enhanced by the expected concomitant decrease in
decomposition rate. Bleeding off decomposition gases
as they are formed could also limit the maximum
pressure established in the system for, as illustrated
in Table III, this would eventually lead to a substan-
tially reduced decomposition pressure. The resulting
build-up of Li20 product, however, would render the
liquid nitrate extremely basic and, as a consequence,
more corrosive toward its containment (see below).
4.2. Reversibility of Tritium Dissolution and Release
The stable form of H 2 (T2) in molten alkali
nitrate salts is thought to be dissolved H20 (T20),
due to the reaction (18)
H 2 + N O r (salt) = H20(dis) + N O ; (salt) (10)
According to DeVan, liquid NaNO 3 and KNO 3 can
dissolve significant quantities of H2(T2) in the
H 20(T20) form which is easily removed by inert gas
stripping. (18~ DeVan also noted that displacement of
dissolved water by stripping seems to be less effective
in the case of LiNO 3. To us, this information sug-
gests that, in liquid LiNO 3, dissolved H20 exists in a
more stable form, namely LiOH (dis). We have tested
this hypothesis by evaluating reversibility with re-
Lithium Nitrate
Table V. Calculated Values of the Constant B T in the Relation
aMO H = BT(aH20) 1/2 for M = El, Na, and K
T emperatu re (~ M = Li M = Na M = K
600 196 3.6• -3 1.1 •
800 5 x 104 14 0.16
spect to dissolution/evolution of water in terms of
the general equilibrium reaction:
2MNO3 (1) + H20(dis )
= 2MOH(dis) + N2(g ) + 5/2 O2(g )
( M = L i , Na, o r K ) (11)
Assuming the activities of 02 and N 2 to be fixed by
the composition of air at NTP, and the nitrate is
essentially undissociated (aMNo3=I), we calculated
values of the T-dependent constant B T in the expres-
sion aMO H ~ BT(aI~20) 1/2 for each nitrate at 600~
and 800~ The results are presented in Table V.
These results show clearly that dissolved LiOH is
considerably more stable than its Na and K analogs
(Li > Na > K), and that the chemically stable form
of Hz dissolved in liquid LiNOs is in fact LiOH
(dis). This appears to explain the previously noted
observation of poor H20 reversibility in LiNO3, (is)
and it certainly argues against use of the Li salt in
liquid NaNO3-KNO 3 mixtures to enhance tritium
breeding capability. The stability of LiOH relative to
its nitrate is so much greater than for the correspond-
ing Na or K salts, even LiNO 3 concentrations as low
as 1 mol% would not prevent preferential formation
of LiOH (LiOT). It is also worth noting that the
stability of MOH (dis) relative to H20 (dis) increases
with temperature.
4.3. Corrosiveness of Molten LiNO3-LiNO 2
Mixtures
In a recent review of exreactor corrosion data
for various Fe-base structural steels in contact with
liquid Na and K nitrates, DeVan(18) concluded that
corrosion rates appeared acceptably low ( _<13/tm/yr
alloy conversion to adherent oxide) at temperatures
up to 600~ However, he also indicated how subtle
interactions between salt "acidity" (as represented by
the log inverse 0 2- ion concentration in the equi-
librium NO 3 + 2e = NO~- + 0 2. ), impurities such as
251
CO 2 and H20, and MHD-induced external polariza-
tion effects, could dramatically influence the corro-
sion rate.
-s Although the extant literature on corrosion by
LiNO3/LiNO2 molten salts is sparse, two related
effects are considered particularly relevant in assess-
ing its corrosion behavior:
1. the relatively low thermal stability of LiNO 3
coupled with radiolytic decomposition will
lead to significantly higher oxygen activities
than in mixed K, Na salts (i.e., decreased
"acidity," increased "basicity');
2. b u i l d u p of H 2 (T2) will decrease
"acidity"/increase "basicity" via the genera-
tion of L i O H / L i O T described in the previous
section (note that molten alkali metal hydrox-
ides can be particularly corrosive toward
austenitic stainless steels(t9)).
From this brief survey we conclude that molten Li
nitrate coolant will exhibit greater corrosivity toward
structural steels than Na and K nitrates; however, at
T < 750~ the resulting reduction in wall thickness
may fall well within current design allowances. Un-
fortunately, more quantitative statements cannot be
made without the benefit of additional test data.
5. SUMMARY AND CONCLUSIONS
The foregoing assessment suggests that due to
thermochemical limitations molten LiNO 3 or
LiNO3-LiNO2 mixtures may not be suitable for ap-
plication in current fusion breeder reactor designs.
Although features such as stability and corrosivity
may be tolerable at temperatures currently consid-
ered too low for serious interest ( < 650~ say), the
material's tendency to retain tritium is not signifi-
cantly improved at these temperatures. Specifically,
we reach the following conclusions:
9 with respect to decomposition to gaseous
reaction products in a reactor environment,
LiNO 3/LiNO 2 will be considerably less sta-
ble than its K and/or Na counterparts;
9 coupled thermal/radiolytic decomposition of
LiNO3/LiNO 2 in a closed system is ex-
pected to lead to the development of (02 +
N2) pressures as high as 70 arm (7 MPa) at
800~
9 in the intense radiation field of a fusion
reactor blanket, the LiNO3/LiNO2-O2-N2
252
system is expected to behave reversibly at
temperatures higher than - 750~
9 tritium dissolved in liquid LiNO 3 will not be
easy to remove by inert gas stripping due to
the strong tendency for dissolved T20 to
exist in the chemically stable "tritoxide"
( O T - ) form; LiOT is so stable that tritium
may be extremely difficult to remove from
LiNO3-NaNO3-KNO3 salt mixtures contain-
ing as little as 1 mol% LiNO3;
9 liquid LiNO 3 is expected to be more corro-
sive toward structural alloys than its Na and
K counterparts.
In closing, it must be stressed that questions
remain concerning the influence of temperature and
radiation field on the magnitude of liquid LiNO 3
decomposition pressures and the salt's corrosivity
toward particular structural alloys. Although the pre-
sent evaluation suggests L i N O 3 is nt a promising
candidate from either standpoint, final resolution of
these and related technical issues would require a
program of carefully planned tests in an appropriate
radiation environment. Such a program would in-
clude the following key measurements: (a) the rate of
decomposition, final decomposition pressure, and
identities of the corresponding gaseous decomposi-
tion products, of liquid LiNO 3/LiNO 2 at 600-900~
in n, 7 radiation fields on the order of 2 • 1014 and
5 • 10 TM n or photons/cm2-sec, respectively; (b)
long-term corrosion, i.e., wastage rate and mecha-
nisms, of candidate structural alloys by flowing
LiNO 3 at 700-900~ in representative n, 3' radiation
fields (in-reactor pumped loop experiments); (c) re-
versibility of T 2 / H 2 dissolution in liquid LiNO 3 and
concomitant effects of T2/H 2 dissolution on the
salt's corrosivity towards structural alloys (ex- and
in-reactor loop experiments; similar conditions to
(b)).
ACKNOWLEDGMENTS
The authors thank colleagues at Pennsylvania
State University (K. E. Spear) and Oak Ridge
National Laboratory (T. M. Besmann and T. B.
Lindemer) for advice on the application of
SOLGASMIX. Professor K. E. Spear kindly supplied
the PC version of the program.
Adamson et al.
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