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8334372
8334372
P. C. Souers, C. K. Briggs.
J. W. Pyper and R. T. Taugawa
m LAWRENCE
L1VERMORE
LABORATORY
UniversityotCaltomb/UvenriQn
NOTICE
Dommtic Domwtlo
Pag, Rang, Prica Pig, Rang, PrJea
L3
LAWRENCE LIVERMORE LABORATORY
UrmBisity of CaWbrnia. Uvermore, California, 94550
UCRL-52226
piPTrilWIT!"..
Contents
Abstract 1
Introduction 1
The Clausius-Clapeyron Equation 2
The Saturated Liquid-Gas Vapor Pressure 3
Virial Coefficients 9
Saturated Solid and Liquid Densities 13
Saturated Vapor Pressure of the Solid Hydrogens 15
Binary Hydrogen Mixtures 1?
Acknowledgments 23
References 24
Appendix. List of Symbols 30
-iii-
HYDROGEN VAPOR PRESSIRES FROM 4 TO 30 K:
A REVIEW
Abstract
Introduction
(#)/'* (fl | PH
(5)
H)
dT"
ZRT
(
3G\
dP +
(C dT
g
(1)
f9
dT
RT
l V, (2)
-2-
From a practical point of view, we
H (eff) = (7) would like to know what H (eff) or
H) v
H (eff) look like. We may, therefore,
s
take experimental data points that
and also, are close together and use a varia
tion of Eq. (8);
2
H (eff) - RT 4iSE f8) / lnP
2 - l n P
l\
v dl H (eff) = R(T)' (9)
T T
\ 2 - l /
For solids and gases in equilibrium, The subscripts 1 and 2 refer to the
we use the corresponding solid den data points in a pair. The T is an
sity, p , and the heats of sublimation, average between T and T . If (T. -
H and H (eff). We consider only the T.) is small (i.e., a Kelvin or less),
s s '
solid-liquid equilibrium and just at a linear average may be used without
the triple point. Again, we may use great error. (After presenting our
the Clausius-Clapeyron equation with sources of data, we use Eq. (9) for
-3-
any degree into the 1968 temperature their accuracy. The T value is
scale. Moreover, the 1575 temperature- listed as normal but. could be equi
measurement conference" includes even librium because it could have been
less of the work of the Dutch. The converted during the experiment by
J8 '9
nH, data are not repeated and there beta-particle catalysis.
are no vapor pressure curves. Three Now, we consider the form of the
fixed points from 13.8 to 30.3 K are effective heat of vaporization,
listed for eH,; these are obviously H (eff), as a function of temperature.
from the 1968 temperature scale. We have taken the data on H, HD, and
Returning to the 1968 temperature D_ from the sources listed above and
scale work for our hydrogen vapor have processed pairs of adjacent data
24
pressures, we conclude that, from points according to Eq. (9). Figure
the triple point to 23 K, the eH 1 shows the resultant H (eff) vs
v
data are valid. They are almost
temperature curves from the triple -.
certainly as good as enybody else's points to 30 K.
up to 30 K because they are a close At first glance, the form of
derivative of the triple point to 30-K H (eff) appears to be linear with a
equation of the famous 1948 Woolley quadratic component,
review. The nH, data, only slightly
different, are listed to apply from 2
H (eff) = R[-B + B'T + C T ] , (10)
24
the triple point to 30 K. These,
too, are similar Co the old Woolley where B, B', and C are constants and
equation. B is a negative number. We substitute
For the HD data, there are only for H (eff) in Eq. (8) and integrate
12 to obtain
two choices available and we select
the 1948 data of Woolley. For the
D. data, we select the 1951 data of lnP A + | + B'lnT + CT , (11)
Grilly. The later review of Prydz
does not seem to us to be internally where A is the constant of integra
22 tion. The term P denotes the sat
consistent. For T_, we select some
1975 data by Sherman and Grilly of uration liquid-gas, pure-component
27 vapor pressure. This equation pro
Los Alamos. These are partly re- duces a fairly self-consistent set of
measured data by Sherman and partly26 constants for H, HD, D, and T
the readjusted 1951 data of Grilly
(see Ref. 3 ) .
The D data are normal and the dif
ference between these and the equi However, liquid-gas vapor pressures
librium form is probably less than have not been cast in the form of
1 T r
~W Triple
15 point
14
''!# v
t? 13
SP Triple * oo
point # . 0 0
12
HD
<P
11 0cd&
o o
o Triple
Solid point . &o 0
w 10
<^P o
o ft*
Liquid
8 - waso
J I 1 I I I
5 10 15 20 25 30 35 40
Temperature K
from many sources. Most of the strings of points contain unknown amounts
of smoothing. Here, * = eH,, 0 = nH,, HD, and v = D . ?
-5-
Eq. ( 1 1 ) . From Woolley's 1948 review values as well as constants A ami B
to the present, the accepted form has follow a smooth sequence through the
of equations.
2
lnP = A + | + CT + D T ; (13) The equations of Table 1 m u s t , of
Hydrogen
Isotope A (Pa) A(Torr)
these values arc taken from different Mittelhouscr and Thodos analyzed the
sources, they are not comp'.^ely con data of tiie day and decided that -in.
sistent as a set. The H and T 7 tem (15) is true to within 0.52, although
peratures are set to the 1968 tempera here is a 1.1? deviation at 19 K.
ture scale; the HI) and D values have They used Eq, (15) to find the normal
not and could be 0.01 K higher. boiling point of the unknown species,
Now the problem arises: What XY. Then they plotted a normal
their vapor pressures have never been temperature, Eq. (15) gave them the
o
^
CD +3
rtJ
1-3
t-l
CD <U
S- 03
3 E
10 15 20 25 30
Temperature K
Fig. 2. Deviation of vapor pressures from the rule of the Geometric Mean. The
HD data are taken from Table 1; other daca are estimates.
estimated an HT value from the rela DT, the effect will be smaller,
tive difference of H-T and H.,-n perhaps IX or less. This effect is
triple-point temperature differences. important when analyzing mixtures
We find a possible deviation of 4.5% of isotopes where nonidealities of
which could change the triple-point mixing are expected to be a few
temperature by as much as 0.2 K. For percent.
Virial Coefficients
-9-
-0.5
20 24 32
Temperature - K
-10-
Table 2. Second virial coefficients of the hydrogens from 14 to 30 K.
Estimates, as derived from a triple-point temperature plot, are
in parentheses.
n
B - B /T
g 0
Hydrogen _, ,
Isotope B , 10 m K /mol n
H, -11,178 .1.44
HD -16,170 1.53
HT (-20,468) (1.59)
D -25,168 1.64
DT (-29,310) (1.705)
T 2 (-33,189) (1.765)
These estimates are obtained by plot and the data extend in two opposite
ting the constants vs the triple-
directions. The Woolley data are
it
point temperature and extrapolating. probably the more correct. However,
The third virial coefficient has we need only concern ourselves with
been measured for eH_ and nH (Refs. the high-temperature end of the satur
11,33,35). We do not include the ation curve. He use the C -limiting
22 - 1 3 2
Prydz review data for D, for either value of 1600 x 1 0 " (m /mol) ; at
virial coefficient. The third virial 30 K, both sets of data approach this
coefficient data are shown in Fig. 4 value. At lower temperatures, the
saturation pressure falls so rapidly
*This empirical method accounts for
the saturation of a given property, that the effect of the third virial
progressing from H2 to T2. It also coefficient, whatever its value, may
accounts for the probable differences
expected (from the vapor pressure) be ignored. Thus, we have calculated
for HT and D2. It is, actually, the compressibility and gas density
almost equivalent to plotting a
property vs the reduced mass of the at the triple points of the hydrogens
isotope. and present the data in Table 3.
-11-
Table 3. Hydrogen heats of transformation at the triple points. Estimates are
in parentheses. For purposes of calculation, more digits than the
true accuracy are given.
Hydrogen
isotope T (K) ITorr) iraol/tn )3
U *,:!) \ J
eH, 13.810 52.73 62.213 0.9841 923.85 0.9S25 907.7 117.3 102 5.11 0.982.' 104 1.0
nH, 13.956 54.00 63.043 0.9842 935.76 0.9826 919.5 ['.2 1(136.7 0.9K26 (054.H
rlD 16.604 92.8 91.498 0.9799 1133.78 0.9777 1110.5 155.4 1769.9 0.9779 1246.6
HT (17.62) (109.5) (101.87) (0.9782) (1246.57) (0.9758) (1216.4) (176) (1192.4) (0.9761) (1426.5)
nD, 18.731 128.6 112.67 0.9768 1314.63 0.9742 1280.7 Wh.6 1477.S 0.9745 1516.0
DT (19.71) (145.7) (121.20) (0.9780) (1417.31) U).975)) (1382.5) 1215) (1597.)) (0.9>56) U 6 J 7 . J)
T
20.627 162.0 (128.56) (0.9796) (1497.59) (0.9768) (1462.8) 12J2) (1694.8) (0.97711 (1714.6)
2
1 1
- -
4-
- -
A
D
D
D ([ ]
D
D
1 1 1
10 15 20 25 30
Temperature K
-12-
Saturated Solid and Liquid Densities
As we can see in Eq. (7), the next deviate from 0.5% above 26 K and is
item needed (in addition to gas com off by 5% at 30 K. The other measured
pressibility and density) to relate isotopes should have densities to 0.5%
H and H (eff) is the liquid (or up to 30 K. We have interpolated for
v v ^
solid) density. The available liquid- HT and DT by plotting p (at constant
ably good to 0.5%. We use the fol The density data for solid H, HD,
Table 4. Equations for saturated solid and liquid densities of the hydrogens.
Estimates are in parentheses.
SOLID LIQUID
3
B T
p
s =
'I- s H * - v
A 2
Hydrogen Ps 43
B
s
3 3
4 3 H 3 2
Isotope (10 mol/m ) (mol/m -K ) (10 mol/m ) (mol/m <K )
-13-
10
Temperature - K
Densiity
3
(10 mol/m ) Density Ratios
see that the HD and T, curves basi desirable to have better experimental
cally are estimates, to say nothing values for all these isotopes.
of the HT and DT values. We have, In Table 5, we have collected the
therefore, used the same triple- equation-derived densities for the
point temperature plot, fixed mainly solid hydrogens at 0 K, 4.2 K, and
on H and D_ values, to obtain all at the triple point as well as for
solid density curves. It would be the liquid at the triple point.
We can now consider the deviation point heat of fusion to find the heat
of the solid-hydrogen vapor pressures. of sublimation. We use the measured
We start with the effective heat of values of e H 2 = 117.3 J/mol, nH. =
55
vaporization, H (eff), for the liquid 117.2 J/mol, HD 159.4 J/mol, * 11
does not produce a good sequence of point is not of the quality of Lee's
data but it is all we have for HD.
constants B and C for the measured
For eH,, we assume the same slope
isotopes H,, HD, and D . The reason
as nH,, i.e., we expect a value
can be seen in Fig. 1, which plots
of 806.2 J/mol at 4 K. For HT, DT,
the good solid-gas data (Refs. 11, 57,
and T,, we must use our usual
58) with the obsolete references for
triple-point temperature estimates.
eH 2 (Refs. 11,14), n H 2 (Refs. 11, 59-
As an aid, we have Grilly's
61), and D 2 (Refs. 11,26), We have triple-point T, values for H (eff)
not included the solid-T, data in and H (eff) of 1700 and 1500 J/mol
the plot because the scatter is 26
(each 50 J/mol, respectively.
considerable.
Next, we integrate Eq. (8) to
The good data in Fig. 1 are the
two clusters about 4 K by Lee for obtain the pressure,
57 58
nH, and nD, . The precision of
these points is outstanding, even con lnQ = A + ^ + B'lnT (11a)
sidering the smoothed data nearby. It
-16-
Table 6. Saturated solid-gas vapor pressure of the hydrogens. Estimates are
in parentheses.
lnQ = A
+ h B' InT
Hydrogen
Isotope A(Pa) A(Torr) B B'
All work with mixtures of hydrogens Soviets, mostly on eH-eD , but partly
has been done with binary combinations. on H -HD and H D - D . "
2 2
6 4 6 7
Much of
The first substantial work concerned this work also involved the three-
the liquid-gas equilibria of H.-HD and phase region.
H.-D, mixtures. Some H_-L/ liquid- The three-phase eH-eD phase dia
solid work was done, primarily to de gram is shown in the temperature-
monstrate the absence of a phase sep composition plot of Fig. 6. '
aration down to 8 K. This was fol The solid-line data were taken by
lowed by considerable work by the melting a slowly-frozen sample, i.e.,
-17-
19
I i 1 i I i I i I i I
0 0.2 0.4 0.6 0.8 1.0
Mole fraction of D,
-18-
one that fractionated away from the H.-HD and HD-D , respectively. If we
known input composition. Hence, the correlate these with the difference
experimental values were extensively in triple-point temperatures of the
corrected to produce those shown in pure components, 6, - ., we find
Fi>;. 6. The gas line is our that the temperature spread increases
Raoult's-Law calculation. as approximately the 2.2 power. The
gram resembles a "cigar" that closes 1.2 to 1.5 power. All mixtures are
perature, ''). (for the ith species). Assuming that these mixtures are
U'e use the center line, connecting essentially ideal, we consider the
the two triple points, as our refer following relations. Raoult's Law,
ence. For a two-phase system (e.g., generalized for three equilibrated
liquid and gas), about half of the phases with components i and j ,
cigar is above and half is below this becomes
center line. We may imagine two such
two-phase cigars, liquid-gas and (20)
h^l
solid-liquid (from the melting curve),
overlapping almost completely. The and
liquid line then moves almost onto
the center line. For H -D , the _i
po
(21)
vertical-temperature spread of the
liquid-solid cigar at 0.5 mole frac
where
tion, AT , is 0.6 K with less than
20% of this above the center line.
The corresponding horizontal- LP! (22)
x I
composition spread occurs at the tem i=l
perature where the center line and
Here, the mole fractions of component
the AT line intersect (point 0 in
i in the gas, liquid, and solid
Fig. 6 ) . This spread, (s. - I ) ,
phases are g., I., and s.. Also, P
I I I i
for H -D is 0.12. Similar liquid-
is the ith pure-component, liquid-
solid cigars have been measured for
vapor pressure, derived in the last
64
H -HD and HD-D .
2 2 It is difficult section after much effort and 0. is
to measure the cigar widths from the l
small graph, but we obtain AT_ ^ val the same for the solid code. Lastly,
ues of 0.17 and 0.10 K and (s - P. is the partial pressure of com
..). - values of 0.052 and 0.038 for ponent i in the mixture and P is the
Raoult's Law total pressure of the
-19-
mixture. We substract S..Q? from each 6
1 1
T - 7) i.e. , (25)
side of Eq. (20) to obtain the compo
sition spread at a given temperature.
and
V (H (23)
( s , - . ) = 0 . 0 6 8 IA, ( 6 .
l i i j i -v (26)
-20-
' below TP
Average of Eq. ( 2 4 )
eH above TP
2
4<
v
: n H above TP
-21-
D.-T-, (6. - 9.) is 1.90 K and we to 18.73 K. The pressure peaks at
calculate (s - l )
i Q b to be 0.043 approximately 0.83 mole, fraction D
(i.e., 50% liquid T yields 54% solid (17.90 K). The two lower curves
T ).
9 Also, we calculate AT. _ to be are for two-phase, liquid-gas equi
0.081, quite a thin phase-diagram librium, taken from the boiling-point
cigar. For H~-T 2 (providing there is table of Ref. 62 where the liquid
no phase separation) we calculate mole fractions are given. The two
(e^-6^, (s - i ) 1 0 > 5 , and A T Q > 5 to curves are isobarLC in terms of the
be 6.82 K, 0.15 mole fraction, and Raoult's-Law pressure, F. They are
1.05 K, respectively. not isothermal and the temperatures
We now turn to the percent devia are not given. Thus, it is impossible
tion of the mixture vapor pressure, I, to modify the data (or use the au
from Raoult's Law. This is defined thors' dew-point table). On each of
as the lower curves, the temperature
obviously increases with the mole
(VT) fractions of D . Also, the 2500-Torr
I(T ) = - - (100) , (28)
m P
m curve represents higher temperatures
than the 500-Torr line. There are
where P is the measured total pres-
m
two major features of the Raoult's-
sure of the mixture and I is calculated
Law, mixed-vapor pressure data. The
at the measured temperature, T . We
data are peaked towards the D side,
see that I has an empirical aspect in
about at the gas mole fraction of 0.5.
that T may be shifted from the ideal
m ' Secondly, I increases with decreasing
shows available data for H^-D,. The because the gas pressure drops rapidly
equilibrium data, taken for freezing becomes more nearly ideal in the sense
liquid where we know the composition of the Perfect Gas Law, even while it
and for freezing gas where the Raoult's is becoming more nonideal with respect
Law is used to estimate the liquid to Raoult's Law. There are also some
-22-
10
Three-phase'
7
S ^Cr" 2500 T o r r - ^ ^ \
Fig. 8. Percent deviation from Raoult's Law for H2-D2 mixtures. The two-
phase pressures are Raoult's Law values, Pf. Here, = calorimetric freezing
of liquid-gas,*>? o volume shinkage upon freezing,6? and = two-phase
boiling points.^2
Acknowledgments
-23-
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-24-
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-28-
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9
PLL/gw/vt
-29-
Appendix. List of Symbols
D Constants for vapor pressure, temperature equations.
-30-
Mole fraction of the i component of a mixture in the solid
phase.
Compressibility of gas.
3
Density of gas, liquid (mol/ra ) .
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