Dew Point/Temperature Curves for
Selected Metal/Metal Oxide Systems
in Hydrogen Atmospheres
A new dew point/temperature diagram
is developed for process engineering purposes
in metallizing, brazing and sintering
BY M. C. REY, D. P. KRAMER, W. R. HENDERSON, AND L. D. ABNEY
ABSTRACT. As an aid in determining
metallizing, brazing and sintering condi-
tions, a new dew point/temperature dia-
gram is developed for selected metal/
metal oxide equilibria in hydrogen atmo-
spheres. The new diagram constitutes an
expanded and more accurate version of
the original set of curves developed ear-
lier by W. H. Chang (Ref. 1).
Experiments carried out to check the
calculated curves show that chemical
kinetics, rather than equilibrium thermo-
dynamics, determine the temperatures of
reaction initiation for the majority of the
systems investigated. In these cases the
empirically determined dew point/tem-
perature curves supercede the calculated
ones for process engineering purposes.
Introduction
Metallizing a ceramic surface and braz-
ing a ceramic to a metal must be carried
out in atmospheres sufficiently reducing
to prevent oxidation of the system's met-
al components. Sintering of an oxide/
metal composite further requires that the
atmosphere be sufficiently oxidizing to
prevent reduction of the desired oxide
and to facilitate the removal of any
organic binders present. The necessary
atmospheric conditions are commonly
provided by gas mixtures consisting of
hydrogen and water vapor in appropri-
ate ratios. Measurement of a gas mix-
162-s | M A Y 1984
ture's dew point is easily done and pro-
vides a convenient, if indirect, measure of
the hydrogen-to-water ratio.
In order to provide a direct correlation
between dew point and metal/metal
oxide equilibria, Chang (Ref. 1) devel-
oped a diagram based on widely known
thermodynamic data for several metals
important to metallizing and brazing
operations —Fig. 1. The authors exam-
ined Chang's calculations with the inten-
tion of extending the range of the dia-
gram, but they arrived at results different
from Chang's for several of the metal/
metal oxide systems represented in Fig. 1.
The authors proceeded to recalculate
and to extend all of Chang's curves and
undertook a program of measurements
to provide an experimental check of the
calculated results.
Method of Calculating Dew Points
The reaction between a metal oxide
and hydrogen can be represented by an
equation of the form:
M m O n (c) + nH2(g) =
mM(c) 4- n H 2 0 (g) (1)
where M is the metal and c and g denote
where
M. C REY. D. P. KRAMER, W. R. HENDERSON,
ANDL D. ABNEY are with Monsanto Research
Corporation, Mound Facility, Miamisburg,
Ohio. To calculate AG n e t , the reaction (1) is
condensed and gaseous states, respec-
tively. The equilibrium constant for this
reaction is given by the expression,
K = (PH2o/PH2)n (2)
where PH2O and PH2 are the partial pres-
sures of water vapor and hydrogen,
respectively, and the activities of the
condensed phases are assumed to be
unity. The net free energy change associ-
ated with the reaction is obtained from
the relation,
AG n e l = -RT 1nK (3a)
where R is the gas constant and T is the
absolute temperature in Kelvin. If calories
are the units specified for AGnet and
logarithms to the base ten are employed,
equation (3a) assumes the form:
AG n e t (calories) = -4.576 nT Logio
(PH 2 O/PH 2 ) (3b)
The total pressure in the system is
assumed to be one atmosphere, so that
PH 2 = 1-PH2O-
Making this substitution in equation (3b):
10-Q
PH2o(atm) = (4)
1 4- 10_Q
Q = AG net /4.576nT (5)
 80 t h e literature (Ref. 2b) and solving f o r A
FeO^^^ a n d B.
60 Selection of d i f f e r e n t t a b u l a t e d values
f o r substitution into e q u a t i o n s (9a) a n d
u_ 40 (9b) will result in slightly d i f f e r e n t values
FE 3
o

11i
DC
?n V^ f o r the t w o constants. A judicious choice
o f n e a r - e x t r e m a f r o m t h e tables will m i n -
LU
nz 1 imize the e r r o r inherent in t h e a p p r o x i -
D_
0
CO
O
1—
<
-20 ' / 2 m a t e relation given b y equations (9a) a n d
(9b). T h e values selected f o r A a n d B in
c o m p u t i n g the equilibrium d e w points
w o 2 ^ ^^1/lo02
X -40 -J- 7N$i021/ in this p a p e r are: A = -2387.718, B = -
11 6.401.
o
h- -60 T h e H 2 0 partial pressures calculated
zn(
} / vinoy / / f o r the various m e t a l / m e t a l o x i d e equilib-
ria are such that m a x i m u m d e v i a t i o n o f
/Cr2037 - t h e c o m p u t e d d e w p o i n t values f r o m
/ /'' tables in the literature (Ref. 2b) is less than
-100
^ /
L-Li...
1 /Ti0 2 >
/ / / I
4 ° C (7.2°F). T h e discrepancy is greatest
/
-120 f o r equilibria at the l o w e r t e m p e r a t u r e s

-140
Fig. I — After Chang (Ret. I). Used with permission
w r i t t e n as t h e sum of t h e t w o chemical
reactions;
M m O n = m M 4- V 2 n 0 2 (-mAG-t)
nH2 + Vi n 0 2 = nH 2 0 (+nAC2) (7)
o o o o o
o o o o o
//'/....,_T o o o
o o o
( < 5 0 0 ° C , i.e., 932°F). For m e t a l / m e t a l
oxide equilibria at t e m p e r a t u r e s higher
CD N cocno CO L O CD than 5 0 0 ° C (932 C F), t h e discrepancy
co co ^r b e t w e e n calculated a n d t a b u l a t e d d e w
TEMPERATURE. °F
points is less t h a n 2 ° C (3.6°F) a n d , in
m a n y cases, less than 1 ° C (1.8°F). Thus,
the a g r e e m e n t is best in the t e m p e r a t u r e
range applicable t o t h e processes o f
metallizing, brazing a n d sintering.
pressure w h i c h is essentially the Clausius-
C l a p e y r o n e q u a t i o n . Values o f the c o n -
Discussion of Calculations
stants A a n d B are o b t a i n e d b y selecting
(6)
t w o n e a r - e x t r e m e values f r o m the H 2 0 Results of t h e a b o v e calculations are
v a p o r pressure vs. d e w p o i n t tables in s h o w n in Fig. 2. T h e r e g i o n o f the g r a p h

T h e n AG n e t is equal t o t h e e n e r g y differ- TEMPERATURE, °C

ence given by the expression, o CO
o Oo O
oO o
o o o o o CD O ooo
n A G 2 - mAG-i. o o o o CD O ooo CNJ -sr c o c o
C\J oo o LO CD r— X>CT>T—
T h e t w o f r e e energy changes !\G^ a n d 160 i l i 'i 1
-JM r 1 1 1 i- 70
A G 2 are o b t a i n e d f o r t h e a p p r o p r i a t e
o x i d a t i o n reaction f r o m t h e e q u a t i o n 140 60
(Ref. 2a):
120 50
A G = H 0 + 2.303a T log 1 0 T + 40
b X 10~ 3 T 2 4- c X l O ^ " 1 + IT (8)
100
- 30 o
w h e r e H D is the standard enthalpy o f 80 0
f o r m a t i o n o f t h e o x i d e ( M m O n , o r H 2 OJ 20 UJ
and T is t h e absolute t e m p e r a t u r e in 60 rr
UJ

Kelvin. T h e f a c t o r s multiplying t h e t e m - - 10 Q_

p e r a t u r e in e q u a t i o n (8) are t a b u l a t e d f o r
m a n y m e t a l / m e t a l oxide reactions in the
literature (Ref. 2a). T h e e q u i l i b r i u m partial
tn
o
40
20
F e O ^
f
Fe 3 (\A . . . -ll\/lr |0:
(1
-10
cn
o
:>

pressure of w a t e r v a p o r is t h e n o b t a i n e d 0
f o r a g i v e n reaction t e m p e r a t u r e b y " -20
Fe203 y
11

-20 o
applying t h e c o m p u t e d value of A G n e t t o -30 1
—
e q u a t i o n (5) a n d substituting t h e resulting 7»
value of Q into e q u a t i o n (4). o -40 2 10 i -40 n
CL /si0 2 L^

The d e w point corresponding to the

-60 ^ M o O , y -50 •5
111
calculated P H 2 O is o b t a i n e d f r o m t h e Q
equation: -80 -60

A -100
^W02 J--70
D e w point = L r2 3 IJ -A2U3
-80
logio (PH2O) +B
-120
273, in ° C (9a) - -90
-140
A o o CO CO O O OOOO o o o co CO
= 32 + - (- o o o O CO CO o o o o o CO CO o o
CNJ CO LO CD r^oocno LD CO LO
5 log10(PH2o)+B CO CNJ CO CO
(9b) CNJ

-273), in °F TEMPERATURE. °F
Equation 9 is an a p p r o x i m a t e relation Fig. 2 —Newly calculated curves for selected metal/metal oxide equilibria in hydrogen atmo-
b e t w e e n d e w point and water vapor spheres

W E L D I N G RESEARCH S U P P L E M E N T 1163-s
above each curve is the region of oxidiz- diffraction. All reactions were carried out ARGON SOURCE
(PURGE!
ing conditions for the metal affiliated with using a DuPontt, model 990 thermal ana-
the curve, while the region below a given lyzer control module in conjunction with
curve comprises the region of reducing either a Dupont model 951 thermogravi- GAS
SATUHATOR
conditions for the corresponding oxide. HYDROGEN
metric analysis (TGA) cell or a DuPont SOURCE =Bn 3S7 DEWAND HYGROMETER
POINT
Figure 2 does not include curves for
copper, nickel, cobalt or silver, because
high temperature differential thermal CONTROL
J]
n
analysis (DTA) cell connected to a model
DEW POINT p
these metals are too noble. Their curves 910 differential scanning calorimetry MEASURING! CHART
RECORDER
would lie well outside the low tempera- (DSC) cell base. For reactions carried out HEAD

ture/high dew point limits of the graph. at temperatures lower than 1050°C
In the high temperature/low dew (1922°F), the TGA apparatus was used
point region of Fig. 2, several of the and the specimen weight was continu- INERT

curves are in good agreement with the ously monitored. UU REFERENCE

MATERIAL

corresponding ones in Chang's diagram, Typically, a specimen was heated in

particularly for Al 2 03, Si0 2 , and Cr2C>3. the TGA cell at a rate of 5°C/min (9°F/ GAS EXHAUST -
The curves for M n O and ZnO match min) until a significant weight change was
Chang's at very low dew points, but observed, then cooled several hundred X-Y CONTROL
diverge with increasing equilibrium tem- degrees below reaction temperature, RECORDER CONSOLE
perature. For the Zn-ZnO equilibrium at and heated again. This process would be
1500°F (2732°F), Chang's curve gives a repeated three to six times in the course Fig. 3 —Schematic of experimental apparatus
dew point of —5°F (—21 °C), lower by of a heat treatment. used for differential thermal analysis (DTA)
40°F than the corresponding dew point Isothermal reactions were also carried
shown in Fig. 2. out using the TGA apparatus. Oxides
The disparity between Fig. 2 and were rapidly heated to set point temper- high temperature DTA cell was used to
Chang's diagram is most striking for those atures in dry hydrogen and isothermally carry out isothermal reactions at temper-
equilibria which are represented in the reduced. With temperature held con- atures higher than 1050°C (1922°F). The
low temperature/high dew point region stant, the dew point was then increased DTA traces could not be used to deter-
of the graph. For example, the dew point in order to re-oxidize the specimen, and mine reaction initiation temperatures,
for W - W 0 2 equilibrium at 100°F decreased again. In this way a calculated since deflections were also caused by
(37.8°C) is 90°F (32.2°C) according to curve of Fig. 2 could be bracketed. The melting, volatilization, annealing and sin-
Fig. 2, but - 2 8 ° F (-33.3°C) according to tering. This circumstance necessitated the
Chang's diagram; and the difference fE.I. DuPont De Nemours & Co., Inc., Instru- heating of numerous specimens of the
becomes larger with increasing equilibri- ment Products Div., Wilmington, Del. same species in order to obtain data.
um temperature. Generally, for the sys-
tems which fall in the low temperature/
high dew point region, Chang's curves
are shifted to higher dew point values TEMPERATURE. °C
than the corresponding curves of Fig. 2. CO
CD O O O O
o o o
CD
CD
O
CD
O O OCDiO
CD CD C D O C D
CD
OJ
CD O O
"St" COCO
The source of the discrepancies o CO
CNJ
CO "^ LTO ( A N COODi— 1— 1—

between Chang's curves and the newly 160 1 1 r 1 1 1 r 1 i 1 1 1 \\ \- 70

calculated curves is not known. The 140 60
present authors have checked their
results against Richardson plots (Ref. 3), 120 50
and agreement with these has been satis- 40
factory. 100
The curves of both diagrams are based
30 CO
0
80
on the assumption that the metal and its 20 LU

oxide are completely immiscible. The 60 cc

LU

validity of this assumption extends to only CL 10 Q_

a limited number of systems, necessitat-
CO 40 - - • —

"Td cn
o 0
ing experimental confirmation of the cal- 0 o>
20
culated curves.
r Z 1 -10 <c
0 1 -20 3_
Experiments 1J
O
-20 -30
High purity powders of the metals or
their oxides were heated in flowing, con- o -40 -40 o
trolled dew point mixtures of hydrogen CL

and water vapor. Dew points were mon- -60 -50

itored and controlled to ± 1°C ( ± 1.8°F)
. -60
-80
using a Panametrics* model 700 hygrom- Cr 2 0 3 / - -70
eter and Panametrics model 101 moisture -100 >
generator. The powder specimens were - -80
weighed both before and after heating, -120
and were contained during heat treat- A - -90
ment in either platinum or alumina cups. o CO CO CD CD CD O O O O co co co co co
CO CO CD co co 0 0 0 0 CO CO CO CO CO
CO CO
Phase identification of the reacted CNJ uo CD r~-oocx>o LO
T—
CO
CNI
LO
CNJ
CO LD
CO CO
material was made by means of x-ray
TEMPERATURE. °F
*Panametrics, Inc., Waltham, Massachusetts Fig. 4 — Experimental data for Cr-Cr203 system superimposed on calculated curve

164-slMAY 1984
 600 A Fe203
Calculated /
• FeO
• Fe304

"of 5 5 0
y ^
3

Measured^,^-"^
i 500
t-
- /

450

i i i i i i
-20 -10 -10 0
Dew point, ' C Dew point, °C

Fig. 5 —Reduction initiation temperatures vs. dew points for ZnO in Fig. 6—Measured reduction initiation temperatures for Fe2Oj, FejO^
H2/H20 gas mixtures and FeO in H2/H20 gas mixtures

700 •
• First heating
my
/%
650 • Subsequent heatings •
^m
600 - JL-——"•" * ***
m
£
| 550
a. x^***
E

500
-

450 " *"

i i i
-30 -JO -10 0 -20 -10 0
Dew point, C Dew point, C

Fig. 7-Measured reduction initiation temperatures for Mo02 in H2/ Fig. 8-Measured reduction initiation temperatures for W02 in H2/H20
H20 gas mixtures gas mixtures

X-ray analysis alone was used to deter- that equilibrium thermodynamics ade- unity, the resulting water-to-hydrogen
mine if reaction had occurred during a quately describe the behavior of this ratio consistent with the equilibrium is
DTA run. A schematic of the DTA exper- system. greater than it would be if K were given
imental configuration is shown in Fig. 3. The Zn-ZnO system exhibits marked by equation (2). Therefore, the calculated
The TGA configuration used was, except deviation from ideal behavior —Fig. 5. dew points for the Zn-ZnO equilibria are
for the furnace module, the same in all Zinc oxide is reduced at temperatures too low, as Fig. 5 shows. Efforts to detect
respects. much lower than the thermodynamic oxidation of zinc in wet hydrogen were
calculations predicted. Zinc has a low unsuccessful; the zinc specimens vola-
melting temperature and the liquid has a tized when heated. The empirical Zn-
Results and Discussion
high vapor pressure, boiling at 907 °C ZnO curve in Fig. 5 was generated by
Figure 4 shows the results for the (1665°F) (Ref. 2c). The effects of having reducing zinc oxide powders.
Cr-Cr 2 03 system. The solid curve is taken both liquid and gaseous phases of the Figures 6, 7 and 8 show oxide reduc-
from Fig. 2. The error bars bracketing the zinc present is to reduce the activity tion temperature vs. dew point data for
curve represent the limits of deviation of ac(Zn) of the condensed phase to some oxides of iron, molybdenum and tung-
the empirical data from the predicted value less than unity, and to introduce the sten, respectively. The observed reaction
results. The data confirm that the thermo- activity ag(Zn), also less than unity, of the initiation temperatures are, in all cases,
dynamic model described previously is gaseous zinc phase into the expression considerably higher than the correspond-
valid for the Cr-Cr 2 03 system. The for the mass action constant. Conse- ing metal/metal oxide equilibria tempera-
assumption made in the calculation that quently, equations (1) and (2) are more tures shown in Fig. 2. The phase diagram
the t w o condensed phases, chromium correctly written as follows: for the systems Fe-O (Ref. 4b), M o - O
and chromic oxide, are completely immis- (Ref. 4c), and W - O (Ref. 4d) indicate that
cible and, therefore, have unit activity — ZnO(c) 4- H2(g) = xZn(c) + none of these metals is soluble in its
equation (2) — is consistent with the Cr-O oxides. Furthermore, reaction tempera-
(1-x)Zn(g) + H 2 0 (10)
phase diagram (Ref. 4a). In addition, for tures are well below the melting temper-
dew points higher than - 4 0 ° C (-40°F) where 0 < x < 1 , and atures of all three metals. Therefore, the
the equilibria temperatures for the Cr- assumption of unit activity for the con-
Cr 2 03 system in hydrogen atmospheres K = (P H 2 o/PH 2 )-a c (Zn).a g (Zn) (11) densed phases participating in the reac-
exceed 1000°C (1832°F). At these high Since the mass action constant K is a tions should be valid.
temperatures the reaction kinetics appar- function only of temperature, and the It remains that reaction kinetics are too
ently proceed at rates sufficient to ensure product of ac(Zn) and ag(Zn) is less than slow for equilibrium to be attained over a

WELDING RESEARCH SUPPLEMENT 1165-s

period of several hours for the systems
that lie in the low temperature/high dew
point region of Fig. 2. It is to the domi-
nance of chemical kinetics over equilibri-
um thermodynamics that we attribute
our inability to oxidize tungsten, molyb-
denum or iron in wet hydrogen during
heats of up to seven hours duration.
Figures 7 and 8 show that, for M o 0 2
and W 0 2 , the reduction initiation tem-
perature observed during the first heating
of a specimen was higher than for the
subsequent reheatings. The reaction start
temperatures observed in the second
and following cycles were repeatable, so
that t w o distinct reaction start tempera-
tures were to be considered.
The authors attribute the observed
differences between initial and subse-
quent reduction initiation temperatures
to one or both of t w o unrelated
causes:
1. Contaminants adsorbed onto speci-
men surfaces can form protective barri-
ers between the specimen particles and
the surrounding atmosphere until the
contaminants are thermally desorbed or
are themselves reacted to form porous
or delaminated products which permit
the passage of gaseous reactants and
products to and from the specimen sur-
face.
2. Partial reaction of a crystalline spec-
imen can greatly increase the degree of
disorder in the crystal by an increase in
the number of vacancies or interstitial
ions, or the formation of non-equilibrium
phases; increased disorder serves to
make the specimen material more reac-
tive, effectively lowering the tempera-
ture at which the specimen will further
react in a given chemical environment.
The process engineer should be aware
of these possibilities and of those cases
for which their effects are significant.
Figures 7 and 8 clearly demonstrate this
significance for the reactions of M o 0 2
and of W 0 2 with hydrogen/water gas
mixtures.
Summary
The equilibria curves for metal/metal
oxide systems in H 2 / H 2 0 atmospheres
originally constructed by Chang have
been recalculated, their range extended
and their accuracy improved. A program
of measurements carried out to check
the validity of the calculated curves has
shown that chemical kinetics dominate
equilibrium thermodynamics in the low
temperature/high dew point regime. For
the metal/metal oxide systems thus
affected, the empirically determined tem-
perature/dew point curves may be
referred to for process engineering pur-
poses.
References
1. Chang, W. H. 1956. A dew point-
temperature diagram for the metal-metal
oxide equilibria in hydrogen atmospheres.
Welding Journal 35(12):622-s to 624-s.
2. Weast, R. C , ed. 1978. Handbook of
Chemistry and Physics, 59th ed., (a) —pp. D45
to D50, ( b ) - p p . D231 to D233, ( c ) - p . B65.
Cleveland: The Chemical Rubber Company.
3. Darken, t. D., and Gurry, R. A. 1953.
Physical Chemistry of Metals. N e w York:
McGraw-Hill Book Company, Inc.
4. Samsonov, G V. 1973. The Oxide Hand-
book, ( a ) - p . 4 7 2 , ( b ) - p . 4 7 4 , ( c ) - p . 4 7 6 ,
(d) - p.492. New York: IFI Plenum Data Corpo-
ration.

WRC Bulletin 289

November, 1983

Hot Cracking Susceptibility of Austenitic Stainless Steel Weld Metals

by C. D. Lundin and C. P. D. Chou

This comprehensive report describes the influence of the alloying elements and multiple t h e r m a l
cycling on the hot cracking resistance of austenitic stainless steel weld metals. In addition, the effect of
composition and multiple t h e r m a l cycling on the hot ductility is also determined and correlated with the
hot cracking tendency.

Publication of this paper was sponsored by the Subcommittee on Welding Stainless Steel of the High
Alloys Committee of the Welding Research Council.

The price of WRC Bulletin 289 is $16.50 per copy, plus $5.00 for postage and handling. Orders should
be sent with payment to the Welding Research Council, Room 1 3 0 1 , 345 East 4 7 t h St., New York, NY
10017.

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