AFWAL-TR-81-41 77

Volume I

OFIC1IAL ,FILE, COPY

THE KINETICS OF POLYMER CURE BY DIFFERENTIAL

SCANNING CALORIMETRY

W. W. Adams
I. J. Goldfarb

Polymer Branch
Nonmetallic Materials Division

May 1982

Final Report for Period 1 July 1976 - 30 June 1981

"jApproved for public release; distribution unlimited.I

MATERIALS LABORATORY
AIR FORCE WRIGHT AERONAUTICAL LABORATORIES BESTAVAILABLE COPY
AIR FORCE SYSTEMS COMMAND
WRIGHT-PATTERSON AIR FORCE BASE, OHIO 45433

oq04 057
AFWAL-TR-81-41 77
Volume I
NOTICE

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This report has been reviewed by the Office of Public Affairs (ASD/PA)
and is releasable to the National Technical Information Service (NTIS).
At NTIS, it will be available to the general public, including foreign
nations.
This technical report has been reviewed and is approved for publication.

Project Scientist R. L. VAN DEUSEN

Chief, Polymer Branch

FOR THE COMMANDER

F. D. CHERRY, Chief_
Nonmetallic Materials Division

The computer software reflected in Volume II is limited to

dissemination to DOD Agencies only. Other requests for the
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(DOD Dir 4160.19, dtd Apr 73). Requests must be
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REPORT DOCUMENTATION PAGE READ INSTRUCTIONS
BEFORE COMPLETING FORM
1.REPORT NUMBER
AFWA
RE L-TR-81-4177
O T N M EI , Volum e
2. GOVT ACCESSION NO. 3. RECIPIENT'S CATALOG NUMBER

4. TITLE (and Subtitle) 5. TYPE OF REPORT & PERIOD COVERED

THE KINETICS OF POLYMER CURE BY Final
DIFFERENTIAL SCANNING CALORIMETRY 1 July 1976-30 June 1981
6. PERFORMING ORG. REPORT NUMBER

7. AUTHOR(s) 8. CONTRACT OR GRANT NUMBER(s)

W. W. Adams and I. J. Goldfarb

9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT, PROJECT, TASK
Materials Laboratory (AFWAL/MLBP) AREA &WORK UNIT NUMBERS
Air Force Wright Aeronautical Laboratories (AFSC) 24190415
Wright-Patterson Air Force Base, Ohio 45433
Ii. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE
Materials Laboratory (AFWAL/MLBP) May j1982
Air Force Wright Aeronautical Laboratories (AFSC) 13. NUMBEROlPAGES
Wright-Patterson Air Force Base, Ohio 45433 201
14. MONITORING AGENCY NAME & ADDRESS(if different from Controlling Office) 15. SECURITY CLASS. (of this report)

UNCLASSIFIED
15a. DECLASSI FICATION/ DOWNGRADING
SCHEDULE

16. DISTRIBUTION STATEMENT (of this Report)

Approved for public release; distribution unlimited.

17. DISTRIBUTION STATEMENT (of the abstract entered in Block 20, if different from Report)

18. SUPPLEMENTARY NOTES

19. KEY WORDS (Continue on reverse side if necessary and identify by block number)
Cure Kinetics Reaction Windows
Polymer Cure Resins
DSC (Differential Scanning Calorimetry)
Thermal Analysis
20. ABSTRACT (Continue on reverse side If necessary and identify by block number)

The need for providing processing information for new resins requires obtaining
the reaction kinetics for polymerization of these resins. The kinetic param-
eters can be used to generate reaction window plots. Because of the exothermic
nature of these reactions, differential scanning calorimetry (DSC) was utilized
to obtain the kinetic parameters. Multiple-scan DSC curves at several heating
rates were utilized applying the Friedman method of kinetic analysis, This
method, which obtains activation energies at each extent of conversion, allows

DD , JAN 7 43 EIINO O 5I 1SLT Unclassified

SECURITY CLASSIFICATION OF THIS PAGE (When Data Entered)
 Uncl assifi ed
SECURITY CLASSIFICATION OF THIS PAGE(WhWn Data Entered)

kinetic parameters to be evaluated without having to assume any apriori

functionality for the rate dependency. The kinetic parameters so obtained are
then utilized to predict the behavior of reacting systems under a variety of
isothermal conditions. This behavior is displayed in reaction window plots.
The method is described, and includes descriptions of computer programs with
illustrated data from the cure of new resins.

Unclassified
SECURITY CLASSIFICATION OF Tu,• PAGE(When Data Entered)
AFWAL-TR-81-4177
Volume I

FOREWORD
This report was prepared by the Polymer Branch, Nonmetallic
Materials Division. The work was initiated under Project No. 2419,
"Structural Materials", Task No. 241904, Work Unit Directive 24190415,
"Structural Resins." It was administered under the direction of the
Materials Laboratory, Air Force Wright Aeronautical Laboratories,
Air Force Systems Command, Wright-Patterson Air Force Base, Ohio, with
Dr. F. E. Arnold as the Project Scientist. Co-authors were
Mr. W. W. Adams and Dr. I. J. Goldfarb. This report covers research
conducted from 1 July 1976 to 30 June 1981.

The authors gratefully acknowledge the technical assistance of

Ms. Marlene Houtz, Mr. Gary Doll, and Mr. Thomas Grossman, especially
in the areas of programming and experimental testing of the method.

We also acknowledge the permission granted by Perkin Elmer Corporation

(Dr. Bruce Castle) for reprinting several subroutines.

LBest Available Copy

AFWAL-TR-81-4177
Volume I

"TABLE OF CONTENTS

SECTION PAGE

I INTRODUCTION 1

II THEORY 2

1. Kinetic Analysis 2
2. Differential Scanning Calorimetry 5

3. Kinetic Analysis of Differential Scanning

Calorimetry 12
III EXPERIMENTAL 14

1. Instrumentation 14
2. Calibration 14

3. Data Collection 14
4. Data Reduction 15
5. Computer Programs 15

a. KINETIC 15
b. CURE 18

c. CALIB 18

IV RESULTS AND CONCLUSIONS 21

REFERENCES 26
APPENDIX A PROGRAM CALIB 27
1. Sample Data File 27
2. Sample Output 40

APPENDIX B PROGRAM KINETIC 95

1. Sample Data File 95

2. Sample Input Cards 100

3. Sample Output 102

4. Sample Output Plot 184
AFWAL-TR-81-4177
Vol ume I

TABLE OF CONTENTS (Concluded)

SECTION PAGE

APPENDIX C PROGRAM CURE 186

1. Sample Input Listing 186

2. Sample Output 188

3. Sample Output Plot 192

vi
AFWAL-TR-81-4177
Volume I

LIST OF ILLUSTRATIONS

FIGURE PAGE

1 Differential Scanning Calorimeter, Simplified

Diagram (Modification of Drawing in Reference 8) 6

2 Simplified Differential Sc nning Calorimeter Sample

Cell: SaMple and Holder S , Thermal Energy Source
or Sink

3 Differential Scanning Calorimeter Simulated Curves for

"a Sharply Melting Standard. Slopes of two finite heat
rate curves (Cl, ½C1 ) are equal to CI/R
, ldT
LTTor d and ½CI/R (or -• 11R respectively, where R
(od{ t an C1 R t
is the thermal resistance. 10

4 Differential Scanning Calorimeter Simulated Curve for

Non-Sharply Melting Sample (or Any Other Broad
dT 1
Thermal Phenomenon). Slope of OB is -.•, TA is measured
temperature at peak height, TB is actual temperature. 11

5 Typical Differential Scanning Calorimeter Curve.

Indicated is the Partial Peak Area, a; the Total Area
Is Equal to the Heat of Reaction, AH. T5 , T5 0 , and T9 5
are respectively the temperatures for 5%, 50%, and 95%
completion of the reaction. 13

6 DSC Curves for Acetylene Terminated Sulfone Specimen and

Background (Strip-Chart Recording). Scan rate 200 minute.
range 10 mcal/sec, curves are arbitrarily shifted vertically.
a. Curing Curve, b. Baseline for a (taken of an empty
sample pan before a was run), c. Cured sample, rerun
after a. 16
7 DSC Curves for Acetylene Terminated Sulfone Resin Cure 22

8 Arrhenius DSC Curve Plot for ATS Resin 23

9 Reaction Window Plot for ATS Resin 25

vii
AFWAL-TR-81-4177
Volume I

SECTION I
INTRODUCTION

The need for providing processing information on new resins in this

laboratory requires obtaining the reaction kinetics for polymerization of
these resins. The kinetic parameters can then be used to generate
reaction window plots. Because of the exothermic nature of these
polymerization reactions, differential scanning calorimetry (DSC) is an
effective method to obtain the kinetic parameters.

A number of methods have been reported in the literature for deter--

mining reaction kinetics by DSC. Many of these attempt to obtain the
kinetic parameters from a single DSC scan. A review of some of these
has appeared recently (Reference 1). Single scan DSC kinetic analysis
has inherent difficulties especially when the reaction order is not
known or if the reaction rate data do not justify the use of a reaction
order function. The consequences of the use of single scan kinetics
were well described by Flynn and Wall (Reference 2) for the analogous
case of thermogravimetric analysis. In this report, the use of the
Friedman method of kinetic analysis of thermogravimetry (Reference 3)
is applied to DSC measurements of resin cure.
AFWAL-TR-81-4177
Volume I

SECTION II

THEORY

1. KINETIC ANALYSIS

Let us define a variable a, the conversion factor (0 -<a - 1), which

is the amount or fractional conversion of reactants to products. In
general, r, the rate of the process can be considered to be a product of
factors involving both a and temperature:

r r-dt _do
k(T)f(a) (f)

The rate is also a function of pressure, but for our purposes pressure
is a constant and will be neglected. k is called the "rate constant"
and is independent of the concentrations of the reactants but is a
function of temperature.

The dependence of k upon T is usually given by:

d(ln k) EA (2)
dT RT2

where T is the temperature, R is the usual Gas Constant, and the activation
energy EA is constant. Hence, the familiar Arrhenius equation arises
upon integration:
EA

k = A eRT (3)

and the activation energy is interpreted as the energy needed for a

molecular species to become reactive. In a reacting system an equilibrium
exists between ordinary and active molecules. EA is the difference
between the average energy of the active molecules and the average energy
of all the molecules. The two averages must have the same temperature
dependence for the Arrhenius equation to be valid (Reference 4).
Substituting Equation 3 into Equation 1 yields

da = Ae- E/RTf(a) (4)

2
AFWAL-TR-81-41 77
Volume I

The other factor in the rate equation, f(c), is generally derived

experimentally by plotting different functions of a against time. As an
analogy to many chemical reactions in solution one might consider f(a)
to be of the form:

f(c) = _,)n (5)

where n is called the order of the reaction, In this case since con-
version is used rather than the usual kinetic form which utilizes some
form of concentration of reactant(s), this should be more appropriately
called the "apparent" order. If the volume change during reaction were
known, conversion units could be converted to concentration units.

The simplest case of Equation 5 is when n = 1 or a first order

reaction. Then, if temperature is constant, Equation 1 reduces to

da/dt = k (1-a) (6)

or the rate of change of conversion decreases proportionally with the

concentration of reactant(s).

While an expression of the form of Equation 5 is not always valid,

particularly in bulk reactions, it still represents a useful starting
point for describing experimental reactions. In the case of solid state
or viscous state reactions, however, any kinetic analysis of experimental
data should not initially require a reaction "order" form of rate
dependency.

Consider experiments conducted under different conditions, e.g.,

different heating rates, such that a certain constant degree of
conversion (a) is attained for each experiment at different temperatures.
Then assuming that f(a) is not a function of temperature, i.e., the
mechanism does not change over the temperature range considered,
Equation 1 can be rewritten:

In d-a - E 1 + In Af (a) (7)

dt RT

3
AFWAL-TR-81-4177
Volume I

Since a is a constant, f(a) is also constant and the second term on

the right side of Equation 7 is a constant. Thus, a plot of in da/dt vs. I/T
for the several experiments should yield a straight line with a slope
equal to -E/R and an intercept equal to ln Af(a). An activation energy
can be obtained without making any assumption as to the reaction "order"
or rate dependency. Repeating this process at different values of a
can verify that the activation energy is indeed constant during the
course of the reaction. If not, it indicates that Equation 4 is not a
valid representation of the reaction and alternate expressions should
be tried.

Having determined an average Ea over the whole reaction as described

previously, values of da/dt and T at various values of a can be substituted
into Equation 6 giving Af(a) as a function of o. The rate dependency can
be determined in this manner without having to assume any a priori
functionality. If a plot of ln Af(a) vs. ln(l-a) results in a straight
line then the slope of that line gives the reaction order n of Equation 5
as well as the pre-exponential factor A. If the plot is not a straight
line either some other functional form can be tested or a numerical
table of Af(a) vs. a may have to suffice, as described below.

Having obtained the kinetic parameters, one can utilize them to

predict the behavior of the reacting system under a variety of isothermal
reaction conditions. This is displayed in a so-called "reaction window
plot," the source of which can be described as follows:

If temperature is held constant, Equation 4 can be rearranged and

integrated to yield aT

MdA eE/RT f dt (8)

0 0

The left-hand side of Equation 8 is a function of a which we can

call g(a) and, if the functional form of f(a) is known, can be

4
AFWAL-TR-81-41 77
Volume I

expressed analytically. If not, g(a) as a function of a can be obtained

by numerical integration of I/Af(a) as a function of a. Thus, Equation 8
becomes
g(a) = te-E/RT (9)

or rearranging and taking logarithms of both sides,

ln t = 1 n g(a) (10)

which relates reaction time to extent of conversion for each temperature.

Plots of ln t vs. l/T will give parallel straight lines for each extent of
conversion. These are called reaction window plots since they indicate
how long one can process reactants before any appreciable reaction has
occurred and how long one must heat them at any given temperature before
the reaction is essentially complete. It is for this reason that our
reaction window plots show lines for a = 0.05 (5% conversion) and
a = 0.95 (95% conversion) as well as a = 0.5 (50% conversion), to show
the extremes of the reaction. It should be emphasized that while l/T
is plotted on the abcissa of the reaction window plots, the plots display
times for isothermal reactions.

2. DIFFERENTIAL SCANNING CALORIMETRY

Differential Scanning Calorimetry, first described in 1964 (Reference 5),

is a scanning thermal analysis technique utilizing insulated sample and
reference holders maintained at the same temperature by a closed loop
electrical system (Figure 1). The energy per unit time absorbed or
released by the sample is exactly compensated by a corresponding increase
or decrease in the electrical power to the heaters, such that equivalent
temperature of the two holders is maintained. The measure of the
electrical power applied is equivalent to the heat flow of the system
to the sample. Thus, the DSC is an energy measuring device, while other
familiar thermal analysis instruments (such as differential thermal
analysis, (DTA)) are temperature measuring devices.

5
AFWAL-TR-81-41 77
Volume I

Temperature
-• Averager

Temperaatture
•_ •Progrmmermmer
CL T

E E.
D a M Programmer
o)
6.
Diferetia
PwrInput s
Holder 4-
(V

Figure 1. Differential Scanning Calorimeter, Simplified

Diagram (Modification of Drawing in Reference 8)

6
AFWAL-TR-81-4177
Volume I

A simplified view of a thermal analysis cell is shown in Figure 2.

The sample and its holder are at temperature T , the thermal energy
source is at temperature Tp, and the total resistance to the heat flow
dq/dt is R, a sum of resistance between the pan and the sample, and the
resistance of the sample itself. If care is taken to insure good thermal
contact between the sample, the pan, and the heater, the thermal
resistance can be minimized, but it is an effect which must be compensated
for in DSC measurements.

If we assume that the temperature of the sample and pan are uniform
and equal, and that the heat capacity of the sample and pan and the
thermal resistance R are constant over the range of interest, then:

dh =C dTs d(q
dt s dt dt
dt
where the sample produces heat d-t in an exothermic reaction (dh/dt is

considered positive for an exothermic reaction). Heat flow dq/dt to the

sample is taken as positive, and Equation 11 indicates that heat either
produced by the sample or absorbed from the energy source must increase
the sample temperature or be lost to the surroundings. The heat loss is
controlled by the value of R, and in an analogy with electrical circuits,
the heat current is equal to the potential difference (temperature)
divided by the resistance:

dt R(12

This is Newton's Law, the thermal analogy of Ohm's Law. If we take the
time derivative of Equation 12

dT~ cIT
_!t=
- (13)
dt R R

and if we consider a sharply melting standard material such as indium,

dT =- 0 during melting. Hence, during melting, the slope of the curve
dt

7
AFWAL-TR-81-41 77
Volume I

h R
d

Figure 2. Simplified Differential Scanning Calorimeter Sample

Cell. Sample and Holder (D, Thermal Energy Source
or Sink (E)

8
AFWAL-TR-81-41 77
Volume I

generated, , is equal to the programmed temperature rate dT divided

by the thermal resistance R. This provides the correction method

commonly used in DSC analysis: a value of R is calculated for each heating
rate used in scanning a sharply melting standard (indium), as shown in
Figure 3.

This value of R is then used to calculate the actual temperature at

any point on an actual data curve of interest. For example, in Figure 4,
the true temperature at the peak height is not TA, but is actually found
dT1 from the peak height at A
to be TB by constructing a line of slope T
to the intercept on the temperature axis. This correction typically
ranges from 0.20 for an ultra pure, sharply melting material to several
tens of degrees for other less pure materials with broad melting curves
or curves showing other thermal phenomena (Reference 6).

Obviously, the greatest accuracy in temperature measurements is

achieved with small sample size, proper encapsulation in the sample pan
(i.e., no bending of the flat pan bottom), and slow heating rates. A
balance between sensitivity, which increases with scan rate, and accuracy
is possible by reducing thermal resistance by experimental techniques
and performing a correction for thermal lag and scan rate error.

Another error considered is that of absolute calibration error and

scan rate/temperature nonlinearity. The usual method of correcting for
the latter effect involves measuring melting points of a number of standard
materials and calculating a polynomial fit between the Tm's and the
indicated temperatures (Reference 7). The correction was not accomplished
in this study since over the limited range of temperatures involved, the
error is not large, and a linear correction was applied instead. The
error due to inaccuracy in the calibration points and the scan rate error
can be described by
Ttrue = Tobs - C dT/dt + D (14)

where the coefficients can be evaluated from two melting points.

9
AFWAL-TR-81 -41 77
Vol ume I

4-) 5

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Si - Gi
0- 0 *0 4-

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00

01
01
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0i m u 14-0

4- = 4
0o!

... oi va)E
Ir..

I- (Dr-

4--. U)
cL,-' * 5
AFWAL-TR-81-4177
Volume I

5- a
40-
E 0 E

oJ4-)

4-)
oS-

4-)

4-)

.1-0 0
W. S- 4- M
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d) 0
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to= to
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AFWAL-TR-81-4177
Volume I

3. KINETIC ANALYSIS BY DIFFERENTIAL SCANNING CALORIMETRY

The Differential Scanning Calorimeter (DSC) produces a plot of dH/dt

versus time t (or temperature T), where dH/dt is either the rate of heat
input (endotherm) or heat output (exotherm) in millicalories/second.
The total area under the thermogram curve (Figure 5) defines the heat of
reaction AH. The area of a small section of this peak, a, corresponds
to the fractional heat evolved up to time t (or temp T) and is proportional
to the extent of conversion (a),

a (15)
AH
or more generally
t
a() f L dt (l16)
AH dt
t
0

where to is the time for the onset of the exotherm or endotherm.

12
AFWAL-TR- 81-41 77
Volume I

dH

I I
I I

I I I

T5 T5 0 T95 Temperature

Figure 5. Typical Differential Scanning Calorimeter Curve.

Indicated is the Partial Peak Area, a; the Total Area
Is Equal to the Heat of Reaction, AH. T5 , T50 , and T95
are respectively the temperatures for 5%, 50%, and 95%
completion of the reaction.

13
AFWAL-TR-81-4177
Volume I

SECTION III

EXPERIMENTAL

1. INSTRUMENTATION

Thermal data were obtained using a Perkin Elmer DSC-2 differential

scanning calorimeter with analog output display on a Perkin Elmer
Model 56 strip chart recorder. BCD temperature output and heat signal
from the DSC were recorded on punched paper tape by means of a Hewlett-
Packard Model 2570A Coupler/Controller, a Hewlett Packard Model 3480B
Digital Voltmeter, and a Teletype Corporation Model 33 teletype.
Computer calculations were performed on the WPAFB-ASD Computer Center
Cyber 175, and all programs were written in Fortran Extended.

2. CALIBRATION

The DSC was calibrated in the manner described in the operations

manual (Reference 8). Cooling rates were carefully controlled to avoid
super cooling of the standards. Absolute temperature calibration was
checked by examining the melting points of high purity indium and lead at
different heating rates, and constructing a temperature correction curve
for each heating rate, the intercept and slope of which were calculated
in program kinetic (Appendix B). Program CALIB (Appendix A) was used
to determine the value of the thermal resistance factor (TR) for each
scanning rate. This program performs a peak analysis of the melting
endotherm for the standard, and prints out the values of TR and the
observed melting point (Appendix A.2). CALIB is a modified version of
a standard program provided to DSC users by The Perkin Elmer Corporation
(Reference 7).

3. DATA COLLECTION

Data for each material was collected for a set of at least four heating
rates. The coupler/controller was used to initiate the temperature
program of the DSC, and measurements of the signal voltage were made by

14
AFWAL-TR-81-4177
Volume I

the DVM at intervals of 0.8 seconds or longer (limited by the maximum

punching rate of the teletype). For each specimen, three runs were made.
First a scan of the empty sample pan was performed to provide a back-
ground level, then the sample was introduced into the pan and data was
collected through the temperature program. The background scan was
subtracted from the peak data scan to produce a corrected data set
(Reference 9). After completion of the curing scan, the sample was
rescanned to determine if cure was complete and to determine a glass
transition temperature (Tg). Samples were weighed before and after
scanning, and all samples were scanned under a nitrogen atmosphere.
Sample DSC scans are shown in Figure 6.

4. DATA REDUCTION

Punched paper tapes were either converted into punched cards using a
utility program or were read directly onto a disk file by remote terminal.
After checking the data to eliminate any obvious errors, the program
KINETIC in Appendix B was executed. Sample data, required data cards,
and typical output of KINETIC are listed in Appendixes B.l, B.2, and B.3,
respectively.

5. COMPUTER PROGRAMS

Several computer programs have been utilized to perform the kinetic

analysis. Each will be summarized briefly and the main subroutines will
be listed and their functions described. Those subroutines which are
identified with an asterisk are unmodified or slightly modified versions
of standard Perkin Elmer routines, and are printed with the permission
of the Perkin Elmer Corporation, Norwalk, Connecticut (Attn:
Dr. Bruce Castle).

a. Program KINETIC (see Volume II for program listing)

This program is a general data reduction program for transforming

raw data from the DSC into conversion rate versus time or temperature
data for kinetic analysis. Kinetic parameters are ultimately

15
AFWAL-TR-81-41 77
Volume I

0
C)

4.0

to
4.0) a),.-.

r,- o....
-o 4=.C)c. E
FESo
v0 ,. > M

C Ln>
C\ 'a--
g *r 4 - ,
EC E-
(a a)-
0) L) 4~)C
a)0::-, >0-

0-
to..- a4w
LJ a)
S- $- ca
a)
C-. u"00.
4-
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CC• E E

>~ C4) r_

a(D
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C) Lntom
pa r4- 4

C ) ca
CI .0M4nt

o
6a a)

L/ oa - -a

C)C-

16E
AFWAL-TR-81-4177
Volume I

produced, including activation energy and reaction order. Each subroutine

will be summarized briefly to indicate its function.

KINETIC - Calls individual subroutines depending upon mode of

operation, repeats for multiple data sets. Comments list all data
formats.

PRELIM - Initializes control constants, reads input cards to select

options and to set values of thermal resistance and scan rate temperature
correction factors.

INREAD - Reads data file for scan rate, range, initial temperature,
and data rate information followed by raw data for each curve. Calls
INPUTT for actual reading of the raw data. If background subtraction
option used, calls SUBBAK which in turn uses INPUTT to read background
data. Calls COUPLR to analyze each peak.

COUPLR - Peak processing subroutine, applies thermal resistance and

scan rate corrections, senses the peak, truncates if desired, applies
baseline correction, fills the two main data arrays (DHDT and TEMP),
and copies the data to the output data file if desired.

CVPLOT - Calcomp plotting routine for the set of up to six curves

for a graph.

PREKIN - Calculates area under a curve and cumulative areas

dc for 0.01
intervals of conversion. Data is interpolated to calculate i-, c, time,
and temperature for each value of c from 0.01 to 0.99. Calls subroutine
TGA3 for kinetics analysis.

TGA3 - Modified subroutine TGA3 from Reference 10.

POSTLM - Reinitializes to the main program or terminates execution

if job is complete.

FITY - Utility for FT.

FT - Performs a three-point fit and interpolate operation.

17
AFWAL-TR-81-4177
Volume I

NUCO05 - Controls page skips and numbering and title printing for
printer control.

NUCO08 - Writes benchmarks, elapsed running or execution time and

time since last call.

PRPLOT - Calls subroutine GP to produce a one page printer plot of

data when requested by various calls in the main subroutines. Provides
the proper heading for the plot depending upon the value of N in the call.

SUBBAK - calls INPUTT to read the background data, and subtracts point
by point since the data are required to be at the same starting temperature
and data rate.

TEMPTR - Corrects a given temperature for thermal resistance and

applies the scan rate correction.

TK - Utility for FT.

KINETIC - also uses some utility routines listed under program CALIB.

b. Program CURE

This program uses the output kinetic parameters from program KINETIC
to produce a processing window plot. This plot indicates time-temperature
factors for various degrees of cure desired. The program consists of
only one main routine (CURE), which reads kinetic factors from the
teletype or g(c) data from a file (from KINETIC). The temperature -
cure time - cure amount (degree of conversion) relationships are then
calculated and plotted in a convenient graphic form on the plotter.
(See Appendix C for input and output).

c. Program CALIB

This program is a modified version of a Perkin-Elmer Co. supplied

routine to calculate the calibration constants for the DSC. It locates
the melting peak of the standard employed after subtracting baseline
curvature, calculates a least-squares background on either side of

18
AFWAL-TR-81-41 77
Volume I

the peak, integrates the peak (to find heat of fusion), and locates the
true melting temperature for that peak. Subroutines included in this
program are:

CALIB - Main routine, reads sample identification, and other data

about the standard, calls INPUTT to read peak and background data,
locates the maximum (calls IMAX), beginning and end of the endotherm
(calls PEAK twice), and integrates (INTGRA). The leading edge of the
peak is considered to be indicative of the thermal resistance (TR) of
the system at that scan rate, and subroutine DER is used to obtain the
maximum slope of that edge. The area heat constant which converts
encoder readings (ordinate values from the coupler-controller) to cal/sec
in absolute units is obtained from the area of the peak and the heat of
fusion of the sample. TR is applied to the peak maximum to obtain the
true melting temperature for the standard. A printer plot of the data
and all values of constants are then printed. The program cycles through
as many data sets as desired.

INPUTT - Reads the input file for raw data and fills array Y or YB
with M or MM points.

The following utility routines are used by either KINETIC or CALIB

or both:

*BASE Calculates the value of the baseline at a point given the

intercept and slope of the baseline function.
*DER Calculates the derivative at a point in an array.
*GP Produces one page line printer plot of the data requested.
*IMAX Finds the maximum value of an array.

*INTGRA Performs a Simpson's Rule integration.

*INVT Finds the data point index for a given temperature (not valid
after thermal resistance correction is applied).
*PEAK Locates the beginning of a peak in an array of ordinate data.
*SLOPE Applies a least squares fit to ordinate data to obtain a
straight line approximation.

19
AFWAL-TR-81-4177
Volume I

*TEMPT Calculates the temperature of a data point knowing the initial

temperature and the scan rate.
*TEMPTR Calculates the thermal resistance corrected temperature of a
data point.
*YAV Finds average values of an array.

20
 AFWAL-TR-81-4177
Volume I

SECTION IV
RESULTS AND DISCUSSION

DSC curves for the reaction of an acetylene terminated sulfone resin

(Reference 11) are shown in Figure 7. The values have been corrected
for baseline and only show deviations from the baseline.

It should be noted that the integration of the DSC curves is as a

function of time, not temperature, so that the abscissa actually used
for the integration is the elapsed time from the beginning of the exotherm.
Integrations are accomplished utilizing computer programs that interpolate
the integrated values to integral percent conversions, i.e., for Aa = 0.01,
The data for da/dt are plotted on a log scale vs. l/T in Figure 8. The
numbers beside each curve refer to the heating rate in degrees per minute.
Points on each curve at a constant value of a should describe a straight
line in accordance with Equation 7. Two such lines are drawn on Figure 8,
one for a = 0.5 and the other for a = 0.8. The computer program evaluates
the slope of the straight lines for each value of a thereby determining
the activation energy as a function of extent of reaction. If all the
lines are essentially parallel as in the case for this example, a single
reaction is assumed whose activation energy is given by the average
obtained from the slopes of the straight lines. Lack of constancy of
activation energy as a function of conversion (and also temperature) is
evidence for a more complex reaction scheme, and a warning not to
proceed further with this method. In this case the slopes are quite
constant giving an average activation energy of 25.06 kcal/mole. It
o should be noted that data on Figure 8 for early stages of reaction
(i.e., the right side of each curve) are essentially superimposable and
parallel to the constant conversion straight lines. That is because, at
early extents of reaction, there is little loss of reactant and the
reaction curve follows the Arrhenius function. Only after significant
reaction has occurred do the curves start decreasing in slope due to loss
of reactant.

21
AFWAL-TR-81 -4177
Volume I

3.50
0 HEAT RATE = 80.0
A HEAT RATE =40.0
S3.00 * HEAT RATE = 20.0
3.00 A HEAT RATE= 10.0
"w a HEAT RATE= 5.0
CO
4
< 2.50

~ 2.00
w
w
•, 1.50
0

o 1.00
w
I--

0.50

0.00
440 480 520 560 600 640
TEMPERATURE (DEGREES KELVIN)

Figure 7. DSC Curves for Acetylene Terminated Sulfone Resin Cure

22
 AFWAL-TR-81 -4177
Volume I

-1.60

* -1.80
-80
o a=0.5
-2.00
A a= 0.8
-2.20 4

D -2.40
20
v -2.60

. -2.80 10
0
-3.00

-3.20 5

-3.40

-3.60
1.60 1.80 2.00 2.20
I/TOK x 103

Figure 8. Arrhenius DSC Curve Plot for ATS Resin

23
AFWAL-TR-81-4177
Volume I

Having obtained an activation energy, it can be substituted into

Equation 7 along with the appropriate experimental values to obtain the
log Af(c) as described previously. If log Af(a) vs. log (i-ot) is a
straight line the slope gives n, the apparent order of the reaction, In
this case the values are log A = 8.3530 and n = 1.21. These values are
substituted into Equation 10 yielding the reaction window plot given in
Figure 9. This plot can be utilized to guide processing of resins as
described previously.

24
 AFWAL-TR-81-4177
Volume I

2.80

* 100
, 2.60 2

0, 160
N 2.20 180
CL
W 200
2.0 220
240
-J
260
0 1.80 280
0r_ 300
w5 320
~ 160REACTION
1.60 WINDOW PLOT 340
360
380
* 400
1.40 9
*100 10, 102- 103 10
LOG TIME (MINUTES)
Figure 9. Reaction Window Plot for ATS Resin

25
AFWAL-TR- 81-4177
Volume I

REFERENCES
1. T. H. Grentzer, R. M. Holsworth, and T. Povder, ACS Org. Coatings
and Plastics Preprints, 44, 515 (1981).
2. J. H. Flynn and L. A. Wall, J. Res. Nat. Bur. Stds., 70A (6),
487 (1966).
3. H. L. Friedman, J. Polymer Sci. 6C, 183 (1965).
4. H. Eyring and E. M. Eyring, Modern Chemical Kinetics, Reinhold
Publishing Co., New York, 1963.

5. E. S. Watson, M. J. O'Neill, J. Justin, and N. Brenner,

A Differential Scanning Calorimeter for quantitative Differential
Thermal Analysis, Analytical Chemistry, 36, 1964.

6. A. Lucie and M. Tamanini, "An Investigation on Lattice Reorgani-

zation in Copper," Thermochemica Acta, 13 (2), 147 (1975).
7. A. Gray and R. Scott, Thermal Analysis Computer System, The Perkin
Elmer Corporation, Norwalk, Connecticut, June 1970.

8. Instructions, Model DSC-2 Differential Scanning Calorimeter, The

Perkin Elmer Corporation, Norwalk, Connecticut, April 1974.

9. A. P. Gray, "Polymer Crystallinity Determinations by DSC,"

Thermochemica Acta, 1, 563 (1970).
10. AFML-TR-68-181, Part II.

11. G. A. Loughran and F. E. Arnold, Polymer Preprints 21, (1),

199 (1980).

26
AFWAL-TR-81-4177
Volume I

APPENDIX A.1

PROGRAM CALIB

SAMPLE DATA FILE

27
AFWAL-TR-81-4177
Volume I

U dLI.o0 7.2 INDIUM

elO.0
310.00
0j. ts
3339 0331 0337 0337 0337 0336 0336 0335
D335 0334 0334 0335 0334 0333 0333 0333
)333 0333 0D33 0331 0332 0331 3331 0331
0330 0331 0331 0331 0329 0330 0330 0331
329 0329 3329 03Z9 0329 0329 0329 0328
5329 0329 03Z9 03Z9 0329 0329 0329 0329
3328 03Z9 0328 0328 0328 0328 0328 0328
)32? 0327 0327 0327 0308 0L9§-0021-0290
-js52-0554-0339-0087 010> 0222 D8d* 0312
0323 0326 0344 0324 0323 0322 0322 0321
0321 0320 OZO 0320 0320 0320 0320 0320
3320 0320 0320 0310 0319 0319 0319 0318

0 81.10.7.3 INDIUM
b. 8
9.1

60.0

341 0340 0340 0339

0339 0338 0338 0338
3337 0337 0337 0336
0336 0335 0335 0335
ýj36 0336 0335 0335
0335 0334 0333 0333
j333 0333 0333 0333
0332 0333 0333 0333
3333 0332 0332 0332
0332 0332 0332 0332
3J31 0332 0331 0332
0331 0331 0331 0331
03i31 0331 D33l 0331
0330 0329 0329 0329
J329 0329 03290317
0329 0217 0013-0251
"-0515-057-0370-0115 0088 0213 0280 0311
332' 0327 0328 0327 0327 0326 0325 0325
)324 0324 0324 0324 0324 0323 0323 0323
3323 0323 0323 0323 0322 0322 0322 03ZO
3321 0321 0320 0321

0 81.10.7.4 INDIUM
bed
9.L
Z090
40.0
380.0
08
0290 0290 0290 0293 0290 0289 0289 0290
0289 0289 0289 0289 0289 0289 0289 0288
0288 0288 0288 0288 0287 0288 0287 0Z87
0267 0287 0287 0287
0 087 0287 0281 0287
3287 0287 0287 0287 0286 0286 0287 0287
0287 0287 0286 028b 0285 0286 0288 0286
0285 0286 0Z86 028b 0286 0286 0255 0285
3285 0185 O25 0285 0285 0285 0285 0285
Ue85 0285 0285 0285 0285 0284 02• 028J
028' 0284 O28 0285 0284 0284 0285 0284
Dz28 0184 OZ4 0284 028q 028, 0284 Oz4
.j2bd OZ4 02833 02d3 0284 O28 0283 0123
0283 0271 0229 01Z9-0002-0149-029q-0428
-Jt57-0303-U094 007o 0183 0241 Obg8 0279
0ZdZ 0282 08Z2021 0279 0280 0280 0279
3179 0279 0219 0279 0279 0279 0279 0279
0219 0279 0Z79 0179 0218 0Z78 0278 0178

28
 AFWAL-TR-81-4177
Volume I

JZlS 0Z78 0278 0278 0Ž79 0278 0276 0277

0Ž77

I. 81.10.7.5 INDIUM

9.1
40.0
LOod .U
360
350.0
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0t88 0Z88 0Ž58 0289 0288 0Z88 0Z88 0288
0DZ8 0Z88 OZ7 0Z87 0288 0Z87 0Z86 0Z87
0Z87 0287 0Ž87 0287 0Ž87 0Z87 OZ8 OZ87
0256 0Ž56 0Ž87 OZb 0Ž87 0287 0286 0287
0z8b 0285 Ozb00286 0286 0Ž56 0285 0Ž85
0285 0Ž85 0285 02Ž5 0285 0285 0Ž84 0285
0Žz5 0285 0285 0255 0285 0285 0284 0Z84
0Ž54 0283 0U84 0Z84 0Ž84 0284 0ZS4 OZ85
0Ž55 0285 0Z84 0264 0253 0284 0284 0284
0264 0Z84 0284 0283 0284 0283 0Ž84 0284
0Ž84 0Zd3 0Z83 02d4 0284 0283 0283 0283
0Žs3 0283 0Ž83 0283 0283 0Ž53 0283 0283
0253 OZ76 OZZ6 01Z5-0013-0153-0Ž97-0431
-3453-0Z95-0087 0051 0187 0243 0271 0281
0283 0283 0283 0Ž82 0282 0282 028Z 0252
0251 0281 0251 0281 0281 0Ž80 0281 0281
0Ž80 0280 0280 0280 0280 0Ž50 0?19 0280
0Ž80 0Ž80 0279 0281 0279 0279

0 81.107.16 INDIUM
608
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3321 0320 0320 0320 0319 0320 0321 0320
3320 0319 0320 0320 0319 0319 0320 0319
3Z0 0320 0319 0320 0320 0321 0318 0318
0318 0318 0318 0318 0318 0318 0319 0319
3319 0321 0319 0318 0317 0317 0317 0317
03188 03L. 0318 0318 0317 0317 D317 0317
0318 0318 0318 0318 0318 0318 0318 0318
3317 0318 0317 0318 0318 0318 0318 0317
0318 0318 0318 0318 0318 0317 0317 0318
3318 0318 0318 0318 0317 0317 0318 0318
0318 0317 0317 0317 0317 0317 0317 0317
0317 0318 0317 0315 0317 0318 0317 0317
0317 0317 0317 0317 0317 0317 0317 0317
3317 0317 0319 0319 0318 0317 0316 0313
0257 0D07 0088-0051-0197-0344-0488-0627
-075b-0645-07L3-0410-0113 0098 OZZ0 0283
3309 0318 0319 0319 0318 0317 0317 0317
3317 0318 0318 0317 0317 0316 0316 0316
3316 031b 0317 0317 0316 0317 0317 0317
D317 0317 0317 0316 0315 031b 0315 0316
0315 0316 0317 031b 0316 0316 0317

0 51.10.7.7 INDIUM
b.8
9.12

29
AFWAL-TR-81-4177
Volume I

LOoO
1•0.0
390.0
0o8
0323 0323 0314 0325 0324 0323 0322 0323
3323 0323 0323 0323 0323 0323 0323 0323
3323 0323 0323 0324 0324 0323 0323 0323
a323 0323 0323 0323 0324 0324 0324 0323
3323 0324 0323 03Z3 0323 0323 0323 0323
)333 0323 03U3 0323 U323 0323 0323 0323
)323 0323 0323 0323 0323 0323 0323 0323
3323 0323 3323 0323 0323 0323 0323 0323
3323 0323 0322 0323 0322 032Z 0323 0322
3323 0323 0322 0323 0322 0322 0323 0323
3322 0322 0322 0322 0322 0322 0323 0322
03Z2 0321 0322 0323 0323 0323 032Z 0322
3322 0322 0323 0323 0322 032L 0322 0323
0323 0323 0322 0321 03Z2 0320 3321 0321
3322 0322 0322 0321 0322 0322 0322 0322
332JZZ032 0320 0321 0320 0321 0321 0322
33Z 0322 0321 0321 0321 0321 0321 03ZL
3322 0321 3323 0322 03Z2 0320 0320 0321
332l 0321 0319 0320 03Z0 0320 0320 0317
328Z 0195 0071-0070-0T17-0363-0D7-Obq
-0T71-0838-0b7-0354-0067 0128 0238 0293
0316 0323 0324 0323 0322 0321 0320 0319
0319 0320 0320 0321 0320 0320 0320 03L9
3JZO 0320 0320 0320 0319 0319 0319 0319
3320 0320 0320 0319 0319 0319 0319 0319

0 81o10.7.8 INDIUM
0.8
9. 1
10.3
10.0
'#00.0
0.8
028b 0287 0287 0287 0287 0287 0287 0287
02,7 0287 0287 0287 0286 OZ8b 0286 0287
OZdb 0287 0287 0287 0287 0287 0287 0287
0287 Z87 0287 0287 0287 0287 0287 0288
0288 0287 0288 0289 0288 0288 0288 0287
0287 0288 0287 0288 0287 0287 028? 0288
0288 0287 0287 0287 0287 0Z88 0288 0289
0289 0288 0289 0289 0289 0289 0289 0289
)289 0289 0289 0289 0289 0289 0289 0289
D289 0289 0289 0289 0289 0289 0289 0288
0289 0289 0289 0289 0289 0290 0289 0289
0290 0290 0290 0289 0289 0289 0289 0289
0289 0289 0290 0290 0290 0290 0239 0290
D289 0290 0290 0289 0289 0289 0289 0289
0289 0289 0291 0290 0289 0289 0289 0289
0289 0289 0289 0289 0290 0Z90 0290 0289
0289 0290 0490 0289 0Z90 0290 0290 0291
0290 0Z90 0290 0290 0290 0290 0290 0290
0289 0289 0290 0289 0289 0289 0290 0290
0289 0290 0290 0290 0Z89 0289 0291 029a
3Z90 0290 0290 0289 0289 0290 0289 0290
0290 0290 0Z89 0290 0291 0291 0290 0290
0Z90 0290 0289 0289 0290 0290 0289 0290
0289 0289 0290 0290 0290 0290 0Z90 0291
0290 0289 0289 0290 0290 0290 0289 0289
0290 0290 0290 0290 0290 0290 0290 0290
3290 0291 0291 0291 0290 0290 0289 0289
0Z90 0290 0289 0289 0289 0289 0289 0288
0284 0264 OZ9 0159 0089 001b-0057-0128

-30
AFWAL-TR-81-4177
Volume I

-0199-3 270-0341-0410-0477-0540-0590-0526
-0312-0078 0098 0203 OZ56 0280 0289 0291
3291 0290 0289 0289 0Z9 0289 0289 0289
azd9 0289 0289 0290 0290 0289 0209 0288
0288 0288 0288 0288 0289 0289 0Z89 0289
0Z88 0289 0289 0289 0289 0289 0289 0290
0?290 0290 0289 0289

3 81.10.7.9 INDIUM

5.0

4100.
0.80
0453 0253 0253 0253 0253 0253 0253 0Z53
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0D53 0Z53 0254 0254 0253 0254 0255 0254
0253 0253 0254 0254 0255 0254 0254 0254
3453 OZ54 0254 0253 0253 0253 0253 0254
3?254 02-54 0255 0255 0254 0255 0254 0253
0254 0254 0254 0255 0255 0254 0254 0254
O254 0254 0254 0254 0254 0255 0256 0257
325b 0254 0254 0253 0255 0254 0Z54 0254
0454 0255 0255 0255 0255 0255 0455 0256
3255 O254 0255 0255 0Z56 0256 0255 0255
D056 0257 0257 0257 0255 0254 0254 0254
-354 0255 0Z55 0255 0255 0255 0255 0256
0255 0256 0256 0256 0255 0255 0255 0256
3255 0256 0256 0256 0255 0256 0256 0257
0257 0257 0256 0255 0255 0255 0Z55 0254
0255 0255 0254 0255 025b 0257 0258 0257
025b 0254 0255 0256 0258 0259 0257 0255
3254 0255 0256 0256 025b 0257 0256 0256
0255 OZ56 0256 0256 0256 0257 0258 0258
0456 0255 0255 0255 0255 0257 0257 0257
3257 0257 0257 0256 0255 025b 0257 0256
0256 0256 0L57 0258 0258 0257 0256 OZ56
0256 0257 0256 0257 0257 0257 0257 0257
3,Zn7 02-57 0257 0257 0257 0257 0257 0258
3?258 0258 0258 0257 0257 0257 0257 0257
0,57 0258 0259 0259 0260 0259 0257 OZ56
D256 0257 0257 0257 0257 0257 0257 0257
3Z58 0257 0257 0258 0258 0258 0257 0259
0ZbO 0258 0257 0257 0256 0257 0258 0259
0258 0258 0258 0259 0258 0257 0257 0257
0_57 0258 0259 0259 0259 0259 0260 0259
0Z59 0259 0258 0259 0260 0259 0259 0257
OZ56 0257 0257 0257 0Z57 0256 0257 0258
0258 0259 0258 0257 0257 0257 0258 0259
0259 0259 0257 0257 0257 0257 0259 0258
0257 0257 0256 0252 0235 0200 0148 0084
0017-0052-OZ4-019O7-OZ70-0341-0.410-0479
-) 549-0b 17-Ob ,4-0750-0815-0878-0938-0994
-1024-0875-0546-0221 0013 0151 0220 0251
0261 0263 0262 026b 0260 0260 0258 0258
3259 0259 0Z59 0258 0258 0258 0259 0259
3059 0259 0259 02bO 0?259 0259 OZbI 0263
02"3 OZ61 02!59 0258 0257 0257 C258 0257
0259 0259 02-2 0264 Ob3 0262 02bO 0258
0257 0257 0259 0261 0260 0259 0259 0258

0 8L.O.7.1O INDIUM
bed8
9,0
20.0

31
AFWAL-TR-81-4177
Volume I

80.U
370.0
0.8
D99b U95 0295 0295 0294 0293 0293 0194
0293 0293 0293 0294 0293 0293 0292 0293
3292 0293 0293 0293 0293 0293 0Z92 0292
3292 0292 0291 0292 OZ92 0292 0292 OZ91
0Z9Z 0291 0292 0292 OZ9Z 0291 0292 0292
0293 0293 0293 0292 0Z92 0293 0292 0293
0293 0292 0293 029Z 0293 0292 029Z 0292
0292 0292 0292 0290 0230 001-OZbl-0317
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0293 0291 0290 0289 0289 0289 0289 0289
0289 0Z89 0289 0288 0289 0289 0289 0288
04d? 0288 0Z87

U 61,10.7.11 INDIUM
b.8
5.0
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40.0
380.0
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0234 0234 OZ4 0234 0234 0234 0233 0233
023I 0133 0233 0233 0233 0234 0233 0233
0233 0233 0233 0233 0233 0233 0233 0233
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0233 0233 0233 0233 0233 0233 0233 0233
0233 0233 0233 0233 0233 0233 0233 0233
0232 0233 0233 0233 0233 0233 0233 0233
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0232 0232 0232 0232 0232 0232 0231 0231
0232 0232 0232 0232 OZ32 0231 0232

0 81.10.7o12 INDIUM
0.8
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J393 0393 0393 0393 0393 0393 D393 0393
3393 0393 0393 0394 0393 0393 0393 0392
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3394' 0394 0394 0394 0393 0394 0393 0394
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0394 039' 0394 0394 0394 039. 0394 0394
0394 0395 0395 0394 0394 0395 0395 0394
0J94 0394 0345 0394 0394 0395 3395 0395
0394 0395 0394 0395 0395 0395 0395 0395
0A95 0395 0395 0395 039'.0395 0495 0395

32
AFWAL-TR-81-4177
Volume I

0395 0395 0395 0396 0395 0395 0395 0395

0395 0395 0395 0395 0394 0395 0393 0372
0ZdO
0l26-0059-0250-0425-0493-0294-0010
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3396 0397 0396 0397 0396

0 81.10.7.13 INOIUM
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0353 0353 0352 0352 0352 0352 0353 0352
3352 0351 0352 0351 0352 0352 0352 0352
3352 0352 0352 0352 0352

0 81.10.7.14 INDIUM
b8.
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5.0

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0307 0307 0307 0307 0307 0307 0307 0307
0307 0307 0307 0307 0307 0308 0307 0307
0307 0307 0307 0307 0307 0307 0308 0307
0308 0307 0337 0307 0307 0307 0307 0307
"0307 0308 0307 0308 0307 0308 0308 0308
3308 0308 0308 0308 0308 0308 0308 0308
0308 0308 0308 0308 0308 0309 0308 0308
0308 0308 0338 0308 0309 0308 0308 0308
0308 0308 0308 0308 0308 0308 0309 0308
0308 0309 0339 0308 0308 0309 0308 0309
0309 0309 0308 0309 0309 0308 0309 0309
0308 0309 0339 0308 0309 0309 0309 0309
3309 0309 0309 0309 0309 0309 0309 0309
D309 0309 0309 0309 0309 0309 0309 0309
0309 0309 0309 0309 0309 0309 0309 0309
0309 0309 0309 0309 0309 0309 0339 0309
0309 0309 0309-0309 0309 0309 0309 0309
3309 0309 0309 0309 0308 0306 0300 0277

33
AFWAL-TR-81-4177
Volume I

3223 0143 0049-0052-0153-0253-0351-0446

-3538-0521-0695-0732-0578-0257 0027 0201
3Z05 0317 03Z5 0323 0319 0315 0313 0311
0311 0310 0309 0310 0309 0310 0309 0310
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0310 0310 0309 0310 0310 0310 0310 0310
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031L 0311 0310 0310 0311 0310 0311 0311
3311 0311 031L 0309 0310 0310 3311 0310
0310 0310 0310 0311 0311 0309 0311 0310
3310 0311 0310 0310

0 81.10.7o15 LEAD
5.5
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0303 0303 03D3 0303 0303 0304 0303 0303
0303 0303 03D3 0303 0303 0303 0302 0302
0302 0302 0332 0302 0302 0302 0302 0302
0302 0302 0302 0302 0299 0252 0119-0038
-3082-0013 0088 0173 023Z 0266 0284 0294
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0 OL110o7.16 LEAD
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0315 0315 0314 0315 0314 0314 0313 0313
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0 8110o7.17 LEAD
5.5
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0263 0Z63 0263 0263 0263 0263 0263 0263
0263 0263 OZb3 0263 0263 0263 0263 0263

34
AFWAL-TR-81-4177
Volume I

0263 0263 0Z63 0263 OZ63 0263 0Z63 0263

O263 0263 02b3 0263 oz62 0263 0262 0257
OZ17 0135 0025-0071-0076-0003 0087 0159
0208 0236 0250 0257 OZ61 0261 OZb2 0262
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0 81.1071.18 LEAD
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0 81.10.7.20 LEAD

10.0
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35
AFWAL-TR-81-4177
Volume I

0298 0U98 0298 0298 0298 0198 0299 0297

0298 0298 0198 0299 0198 0298 0297 0298
0298 0198 0298 0299 0299 0299 0299 0299
0298 0Z98 0297 0298 0298 0298 0298 0298
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0 81.10o.722 LEAD
5.5
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36
AFWAL-TR-81-4177
Volume I

0.8
OZ43 0143 0Z42 024 Z 024
Z042 042 0241.
0241 0U41 0ZO 0240 0Z40 0239 OZ4 0239
J139 0839 0139 0239 0239 0239 0239 0238
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3Z35 0235 0Z35 0234 OZ34 0234 0234 0234
0233 0233 0233 0233 0Z33 0233 0232 0233
0232 OZ32 OZ32 0232 0228 0190 0084-0081
-32b7-0391-0342-0189-0032 0085 0157 0196
OZ16 O124 0217 02ZS 0Z18 0228 0ZZ8 0Z27
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OZZ7 0Z27 0227 0227 OZZ7 0226 0226 0226

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3163 0107 0025-0072-0174-0269-0307-0280
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3 81.10.7.25 LEAD
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013 0213 0213 0213 0213 02L3 0213 0212

0113 0?13 013 013 0213 0?13 0212 021?

37
AFWAL-TR-81-4177
Volume I

0212 0Z12 0211 OZ11 02Z 0211 0212 0211

OZLZ 0212 Z012 0212 OZ11 0212 0211 0211
0211 0212 0211 0211 0211 02L1 0211 0211
OZI 011 0211 0209 0211 0211 0210 OZI
0209 0211 0210 0211 0210 0211 0Z1L OZ1
OZO 0110 0210 0210 0210 OZI02210 0Z10
OUIO 0210 0210 0210 0209 0210 0210 0210
0210 0209 0210 0210 OZO 0210 0207 0189
0135 0053-0047-0153-0253-0317-0273-0144
-0008 0093 0154 0187 OZOL 0208 0209 0209
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0 81.10.7,16 LEAD
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0 81.10.7.27 LEAD
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38
AFWAL-TR-81-4177
Volume I

0 b1.10.7.28 LEAO
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,05

5.0
596,0

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D064 0Z63 0263 0263 0264 0263 OZ63 0Z63
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0264 0264 OZ64 0264 0264 0264 0Zb3 0264
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0259 0248 OZZ7 0194 0152 0105 0055 0004
-3047-0099-0150-0203-0254-0306-0357-0409
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-0242-0041 0133 0190 0234 0253 OZ6Z 0263
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0263 0264 OZb3 0264 0263 0264 OZ64 0263
0263 OZ64 0264

39
AFWAL-TR-81-4177
Volume I

APPENDIX A.2

PROGRAM CALIB

SAMPLE OUTPUT

40
AFWAL-TR-81-4177
Volume I

8*.L0.*7* INJIUM

NEAT OF FUSION ICALIGRAM) = 6.800

uEIGHT (MG) UF CALIBRATIUN STANUARO - 9.100

KANGE 10.000 (MILLICALISEC FULL SCALE) SCAN RATE - 80.000 (DEGREESIMIN)

PEAK DATA INPUT:

DATA KATE (SECONDSI/ATA PUINT) - .80000000

TEMPEKATURE OF FIRST POINT OF DATA - 371h067 (DES KELVIN)

PEAK BEGINS AT 434.00 DEG. K. (PEAK HEIGHT - 14,94)

PEAK ENDS AT 446*bO UEG. Ke (PEAK HEIGHT - 16.921

AREA-HEAT CONSTANT - .00090099 RANGE PER ENCODER UNIT (CON*RAN=MCALOSEC PER ENCODER UNIT)

TNERMAL RESISTANCE = .Z7i45 DEG* K.-SEC.IMILLICAL

Tn- 436.10 DEG, K.

41
AF'WAL-TR-81 -4177
Volume I

0
0
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AFWAL-TR-81-4177
Volume I

6L.10*7,3 INDIUM

ItAr OF FUSION (CALIGRAM) " boO00

WEIGHT (MG) OF CALIBRATION STANDARD 90100

K4NGE 20o'000 (MILLIAM.ISEC FULL SCALE) SCAN RATE " 80.000 IDEGREESi/IN)

PEAk DATA INPUT:

JATA RATE (SECONDS/DATA POINT) - ,80000000

TEMPERATURE OF FIRST POINT OF DATA - 371,067 tOES KELVIN)

PEAK BEGINS AT 434.•0 DEG. K. (PEAK HEIGHT - 1Z.67)

PEAK ENDS AT 446b80 UEG. K, (PEAK HEIGHT - 1b6L3)

AREA-HEAT CONSTANT - .00090L40 RANGE PER ENCODER JNIT (CON*RAN-MCALISEC PER ENCODER UNIT)

TIERMAL RESISTANCE * .27790 DEG. K.-SECoINILLICAL

MI= 435.9Z UEG. K.

43
AFWdAL-TR-81 -4177
Volume I

4,
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ARAL-TR-81-4177
Volume I

"NEAT OF FUSION (CAL/GKAM) - b.800

WEIGHT (AG) OF CALISRATION STANOARD - 9.100

RANGE - ZO.000 1I4LLICALISEC FULL SCALE) SCAN RATE = 40.000 (DEGREES/NIN)

PEAK DATA INPuT:

DATA RATE (SECUNOSIOATA POINTI - .dO00COOO

rtNPERATURE OF FIRST POINT OF DATA - 36O.533 (OEG KELVIN)

PEA& OEGINS AT 431.73 DEG. K. (PEAK HEIGHT - 1.35)
PEAK ENDS AT 439.Z0 DEG. K. (PEAK HEIGHT - O.65)

AREA-HEAT CONSTANT - .00091008 KANGE PER ENCODER JNIT (CUN*RAN-MCALISEC PER ENCODER UNIT)
|IEKMAL RESISTANCE - .ZOUTt EG. K.-SEC.IMILLICAL

TM- qS3.20 DEG. K.

45
AFIJAL-TP-81 -4177
Volume I

w9
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AFWAL-TR-81-4177
Volume I

oa.10.7.5 INUIUM

r1EAT OF FUSION (CALIGRAM) - b.600

IbG.HT (MG) UF CALI6RATIO4 STANDARD - 9.100

RANGE - 20.000 MINLLICALISEC FULL SCALE) SCAN RATE - 40.000 (DEGREESIMIN)

PEAK DATA INPUTS

DATA RATE (SECONDS/iJATA PUINT) - .60000000

TEMPERATURE OF FIRST POINT OF DATA - 380.533 (DEG KELVIN)

PEAK OEGINS AT 431.73 DEG. K. (PEAK HEIGHT - b.80O

PEAK ENUS AT 439.20 DEG. K. (PEAK HEIGHT - 7.6Z)

AREA-HEAT CONSTANT - 000V0879 RANGE PER ENCODER UNIT (CON*RAN-MCAL/SEC PER ENCODER UNIT)

tiEKMAL RESISTANCE " ZIk030 DEG. K.-SEC.IMILLICAL

Tn- 433.19 DEG. K.

47
AFbIAL-TR-81 -4177
Volume I

0
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 AFWAL-TR-81-4177
Volume I

HEAT OF FUSION (CAL/GRAN) - b.600

dEIGHT (MG) OF CALIBRATION STANDARD - 9.100

kAN"E - 10.000 (NILLICALISEC FULL SCALE) SCAN RATE - 20.000 (DEGREESIMINI

PEAK DATA INPFT9

DATA RATE (SECONDSiDATA PUINTI - .0000000

riNPERATURE OF FIRST POINT OF DATA - 390.2b7 (DEG KELVIN)

PEAK BEGINS AT 430.27 DEG. K. (PEAK NEIGHT - b.971
PEAK ENDS AT t35,07 DEG. K. (PEAK HEIGHT - b.07)

AKEA-HEAT CONSTANT - .0OO•L60 KANGE PER ENCODER JNIT 1CON*RAN-NCALISEC PER ENCODER UNIT)

THEKMAL RESISTANCE .OIZZ

Z UEG.-K*-SEC./IoLLICAL

TN- 3L*.O0 UEG. Ke

49
AIFWAL-TR-81 -4177
Volume I

0
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35 91 o.9

ooi9

o 9o
AFWAL-TR-81-4177
Volume I

hI.10.7.7 INJIUM

HEAr OF FUSION tCALIGKAM) - b.d0a

wEIGHT 4MG) OF CALIdRATIO4 STANDAKO - 9.100

KANGE - 10.000 (NILLICALISEC FUkL SCALE) SCAN RATE = 20.000 (DEGREES/MIN)

PEAK DATA INPUT:

DATA RATE (SECONDSIDATA POINT) - .80000000

rFMPERATUkE OF FIRST POINT OF DATA - 390.267 (DEG KELVIN1

PEAK dEGINS AT 430.4? DEG. K. (PEAK HEIGHT - 14L.)
PEAK ENDS AT 435.07 DEG. K. (PEAK HEIGHT - 4.0L)

AAEA-HEAT CONSTANT - .UO0JLo71 RANGE PER ENCUODER JNIT (CON*RANNMCALISEC PER ENCODER UNIT)

TrIERNAL RESISTANCE - *.0QIA DEG. K.-SEC.MNILLICAL

IN- 43L.07 DEG. K.

51
AF1JAL-TR-81 -4177
Volume ]

4.
40
0
0
0

°C *

* .4

4 el
41 e.4

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h.

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4 .4

O °4

4 1.4 I

O 4.4 )
AF'WAL-TR-81-4177
Volume I

S1.10.7.• INDIUM

MEAT OF FUSION (CALIGRAMI - b.000

wEINHT (IG) OF CALIOKATIU14 STANOAKO - 9.100

RANGE - 10.000 IMLLICA.,SEC FULL SCALE) SCAN KATE - 10.000 (DEGREESIMIN)

PEAK UATA INPUT:

dATA RATE 4SECONDSI.ATA POINTI - UOO000c

I|APEKATUKE OF FIkbT PU14T OF UATA - 400.133 (DEG KELVIN)

PEAK OEGINS AT 430.13 UE6. K. (PEAK HEIGHT - 1.04)
PEAK ENDS Ar 43#.80 UEG. K. (PEAK HEIGHT - Z.571

AKEA-HEAT CONSTANT - .00•9O40 RANGE PER ENCODER JNIT (CON*RAN-MCALiSEC PER ENCODER UNIT)

hIERNAL RESISTANCE - *Z01%1 UkG. K.-SEC.MILLICAL

fl- 130Z4 OEG. K.

53
AF'IAL-TR-81 -41I77
Vol ume !

0,
'L
0
0

• •

41. e•

* .'4

,,, * .4

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* . . I

U • . . .4 •
- *•

• .4k

45
AFWAL-TR-81-4177
Volume I

61.10.7.9 INJIUM

HEAT OF FUSION (CALIGRAMI - b. 00

WEIGHtT (MGj OF CALI1KATION STANDARD - 9.100

oo.00 (MILLICA./SEC FUL SCALE) SCAN RATE - 5.000 (DEGREES/MINJ

RANGE -.

PEAK DATA INPUT:

DATA RATE (SECONDS/JATA POINT) .80000000

T=MPERATURE OF FIRST POINT OF DATA - u10.0b7 (DEG KELVIN)

PEAK 8E6INS AT 429.47 DEG. K. (PEAK HEIGHT - 5.81)

PEAK ENDS AT 131.33 DEG. K. (PEAK HEIGHT - 'k.85)

KANGE PER ENCODER JNIT (CON*RAN-MCAL/SEC PER ENCODER UNIT)

AREA-NEAT CONSTANT = .000o42b8

THERMAL RESISTANCE - .198bO DEG. K.-SEC.IMILLICAL

T- QZ9.69 DEG. K.

55
AFWAL-TR-81-4177
Vol wne I

C"
0
e*e

L.AJ
3..
I3
3 o.1

3 .3
0
341 . l. m
2J 3*. *t. 3

U 3 . * * .

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U .
3 col

3• 0.18
3 .3 a

3• .3 -,

- 0 a .°
U. 3
- 3 3l

3 *.*•°°°•°*°°°..°***.°* . .3

4 3 35g

3 3,
AFWAL-TR-81-4177
Volume I

81.10.7.10 INDIUM

HEAr OF FUSION (CAL/GRAM) = 0.60

WEi6HT ING) OF CALIBRATION STANDARD - 5.000

RANGE - 0.000 (MILLICALISEC FULL SCALE) SCAN RATE - 80.000 (OEGREEStIHN)

PLAK DATA INPUT.

OATA RATE (SECONDS/DATA POINT) .80000000

TEMPERATURE OF FIRST PUINT OF DATA - 311.067 IOEG KELVIN)

PEAK BEGINS AT 432.V3 UEG. K. (PEAK HEIGHT - 5.30)
PEAK ENDS AT 443.bO DEG. K. (PEAK HEIGHT -

AkEA-HEAT CONSTANT - .00090978 XA4GE PER ENCUDER JNIT (CUNSKAN-MCALISEC PER ENCODER UNIT)

THERMAL RESISTANCE - .34313 DEG. K.-SEC.INILLICAL

TN- 434.4b DEG. K.

57
AF•AL-TR-81 -4177
vol ume I

0
9
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 AFWAL-TR-81-4177
Volume I

L.oO1.7.11 INDIUM

HtAT OF FUSION ICALIGRAMI b.800

wEIGHT (MG) UO CALIaRATIO0d STANDARO = 5.000

K.ANE = ZO.O00 (MILLICAL/SEC FU-L SCALE) SCAN RATE = 'O.OO0 (OEGREESININ)

PtAK DATA INPUT:

OATA RATE (SECONOSIaATA PJINTJ = .6000000G

TErPERATURE OF FIRST POINT OF DATA = 380.533 (UEG KELVIN)

PEAK EGINS Atr31.ZO DEG. K. IPEAK HEIGHT - 6.z3)

PEAK ENOS AT 43b.53 DEG. K. (PEAK HEIGHT = b.49)

AALA-HEAT CONSTANT - .O0004Z576 KAGE PEK ENCOUER JNIT (CON*RAN=-CALISEC PER ENCODER UNIT)

rIERMAL RESISTANCE - .Z1357 DEG. K.-SEC.IMILLICAL

Tn- '431.78 DEG. K.

59
AFWAL-TR-81 -4177
Vol ume I

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IA * . *O
AFWAL-TR-81-4177
Volume I

61.10.7.12 INDIUM

HEAT OF FUSION (CALIGRAMI b.603

WEIGHT (MG) OF CALISKAT13N STANUAKD 5.O0O0

AANGE - 10.000 (MILLICALISEC FULL SCALE) SCAN KATE - 20.000 IOEGREES/MIN)

PEAK OATA INPUTS

DATA RATE iSECONDSOATA POINT) - .60000000

TEAPEkATURE OF FIRST POINT OF UATA - 390.267 IOEG KELVIN)

PEAK BEGINS AT 430.Z? DEG. K. IPEAK HEIGHT - 10.973
PEAK ENDS AT 433.147 DEG. K. 1PEAK HEIGHT - B.51

RAEA-HEAT CONSTANT - .00092506 4ANGE PER ENCODER JNIT (CON*RAN-RCALISEC PER ENCODER UNIT)

TrSEKMAL RESISTANCE - *Lbl2t DEG. K.-SEC,/MILLICAL

TM- 430.81 OEG. K.

61
AF.IAL-TR-B1 -4177
Volume I

•
OII
0II,0
I)0
0D I.O
II 00
I. I D
OOI,0 0 O• 0P •O O• O• • B• O• ••
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- * . .
 AFWAL-TR-81-4177
Volume I

dl.1O.?.13 INDIUM

LEAT OF FUSIUN 4CALIGRA) - b.O3

b

WEIGHT 4MG) UF CALIBRATIU4 STANDARD - 5.000

KANGE - 10.000 (MILLICA-ISEC FULL SCALE) SCAN RATE - 10.000 (OEGREES/MINI

PEAk DATA INPUT:

DATA RATE (IECONDS/OATA POINTJ = .80000000

T[MPEKATUKE OF FIRST POINT OF DATA - 410.133 (BEG KELVIN)

PEAK 8EGINS AT 4ZŽ9.81 DEG. K. (PEAK HEIGHT - 9.151

PEAK ENDS Ar 431.13 DEG. K. (PEAK HEIGHT - 4.38)

AAEA-HEAT CONSTANT t .0009281b RANGE PER ENCODER UNIT (CON*RAN-MCALISEC PER ENCODER UNITj

i•4EKRAL RESISTANCE - .14368 DEG. K.-SEC.IMILLICAL

TA- 430.00 DEG. K.

63
AFWAL-TR-81 -4177
Volume I'

o a:

"* .1 * £
*U41 . i.

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 AFWAL-TR-81-4177
Volume I

LI.1O.7.I4 INDIUM

HEAT OF FUSION (CAL/GRAM$ - 6.600

UEIGHT (MG) OF CALIORATION STANDARD - 5.000

KANGE - 5.000 (MILLICA6ISEC FULL SCALE) SCAN RATE - 5.000 (DEGREES/MIN)

PEAK DATA INPUT:

DATA RATE tSECONDS/DATA POINT) - .d0000000

- TEMPERATURE OF FIRST POINT OF DATA - 420.067 (DEG KELVIN)

PEAK WEGINSAT g29.boDEG. K. IPEAK HEIGHT - 16.17?

PEAK ENDS At 430.80 DEG. K. (PEAK HEIGHT - LZ.28)

AKEA-NEAT CONSTANT - *00093993 RANGE PER ENCODER ONIT ICON*RAN-MCALISEC PER ENCODER UNIT)

THERMAL RESISTANCE - *L4136 DEG. K.-SEC.IMILLICAL

TM- 429.71 DEG. K.

65
AFWAL-TR-81 -41 77
V01ae I

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AFWAL-TR-81-4177
Volume I

dL.10.7.15 LEAD

?:AT OF FUSION (CAL/GRAfl) = o.500

aEIGmT ING) OF CALI8RATI34 STANDARD 18.900

KANGE - ZO.0OO (fILLICA_/SEC FULL SCALE) SCAN RATE - 80.000 (DEGREES/MIN)

PEAK DATA INPUT:

DATA RATE (SECONDSIDATA POINT) . d000000

TEMPERATURE UF FIRST POINT OF DATA 5h41.O7 (DES KELVIN)

PEAK 8EGINS AT bOo.00 DEG. K. (PEAK HEIGHT - 0.19)

PEAK ENOS AT bl4.b7 DEG. K. (PEAK HEIGHT - ZO.33)

A'EA-HEAT CONSTANT - .OO0O3078 RANGE PER ENCODER JNIT (CON*RAN-MCALISEC PER ENCODER UNIT)

rIE•RAL RESISTANCE ..971,7 DEG. K.-SEC./MILLICAL

TA- b05.4•7 UG. K.

67
AFIIAL-TR-81 -4177
V/ol ue !

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AFWAL-TR-81-4177
Volume I

8L.1O.7.1b LEAD

HEAT OF FUSION (CALIGRAM) - 5.500

wEIGHT (MGI OF CALIBRATION STANDARD- 4.'00

RANGE - ZO.O00 (MILLICALISEC FULL SCALE) SCAN RATE - 0.000 (OEGREEStNIN)

PEAK DATA INPUT:

UATA RATE ISECONOSIDATA POINT) = .60000000

TEMPERATURE OF FIRST POINT OF DATA S4I.0b7 (DEG KELVIN)

5
PEAA BEGINS AT 6o.O00 DEG. K. (PEAK HEIGHT - 1.30)
PEAK ENDS AT 614.67 DEC. K. (PEAK HEIGHT - 16.91)

AgEA-HEAT CONSTANT - .00100984 RAIGE PER ENCODER JNIT ICON*RAN-MCALISEC PER ENCODER UNIT)

TlExMAL RESISTANCE .Z374

S DEG. K.-SEC./MILLICAL

TA- 605.44 DEG. K.

69
APWAL-TR-81 -4177
Volwge I

0
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70
AFWAL-TR-81-4177
Volume I

6i.1Oo?.L7 LEAD

HEAT OF FUSION (CALIGRAM) - 5.500

wEIGHT (MG) Of CALIBRATION STANDARD - 4.900

RAN6E - 0.000 (NILLICACJSEC FULL SCALE) SCAN RATE 40.000 (DEGREES/NIN)

PLAK DATA INPUT:

OATA RATE (SECONOS/DATA POINT) .80000000

FENPERATUkE OF FIRST POINT OF DATA - 5O.533 (bEG KELVIN)

PEAK BEGINS AT 602.bi DEG. K. (PEAK HEIGHT - Z.7T)

PEAK ENDS AT hOBo00 DEG. K. (PEAK HEIGHT - 7.82)

AREA-HEAT CONSTANT - *0OL307d3 RANGE PER ENCODER JNIT (CON*RAN-NCAL/SEC PER ENCODER UNIT)

TAEkNAL RESISTANCE - .313o9 DEG. K.-SEC./MILLICAL

T1- b03.Zl DEG. K.

71
AF'IAL-'rR-81 -4177
vol ume I

4.
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 AFWAL-TR-81-4177
Volume I

81.10.7.18 LEAD

HEAT OF FUSIUN (CALIGRAI) 5.500

*EIGHT (MG1 OF CALIBRATION STANDARD 4*.900

RANGE - Z0.0OO (MILLICAidSEC FULL SCALE) SCAN RATE - 40.OOO (DEGREESIMIN)

PEAK DATA INPUT:

DATA RATE (SECONDSIDATA POINT) . 0DOOOOO

TENPERATURE OF FIRST POINT OF DATA - SbO.533 (DEG KELVIN)

"PEAKBEGINS AT bOZb7 DEG. K. (PEAK HEIGHT - 3.$L4

PEAK ENDS At b08.O DEG. K. (PEAK HEIGHT - 9.471

AREA-HEAT CUNSTANT - *OODL27,k

RANGE PER ENCODER UNIT (CONORAN-NCALISEC PER ENCODER UNIT)

THERMAL RESISTANCE - .i1419 DEG. K.-SEC./MILLICAL

t4- b03.13 DEG. K.

73
AFWAL-TR-81
Voltmie I -4177

0
9
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74
AFWAL-TR-81-4177
Volume I

dL.1L0.7.19 LEAD

,EAT OF FUSION (CALIGRAM) 5.J00

EIGHT (MG) OF CALIdRATIO4 STANDARD - 4.900

RANGE - 10.000 (MILLICAL/SEC FULL SCALE) SCAN RATE 0.000 (DEGREES/MIN)

PEAK DATA INPUT:

DATA RATE (SECONDS/DATA POINT) - do000OO00

TEMPERATURE OF FIRST POINT OF DATA - 58O.Zb7 (DEG KELVIN)

PEAK BEGINS AT 601.60 DEG. K. (PEAK HEIGHT - 5.93)

PEAK ENDS AT 604.80 DEG. K. (PEAK HEIGHT - 9.30)

AREA-HEAT CONSTANT . 0034951 RA4GE PER ENCODER JNIT (CON*RAN-MCAL/SEC PER ENCODER UNIT)

TIERMAL RESISTANCE aZZbbb DEG. K.-SEC.IMILLICAL

TA- 60L.88 DEG. K.

75
AFWAL-TR-81 -4177
Vol iwe I

41

w
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OI. I!• oo I. •D D I.0 • •o O •• • • • •J •o• • ••
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 AFWAL-TR-81-4177
Volume I

8I.LO.7TO LEAD

HEAT OF FUSION (CALIGRAR) - 1.500

WEIGHT 1MG) OF CALIBRATIO4 STANDARD - 4.900

RANGE - 10.000 (NILLIGALISEC FULL SCALE) SCAN RATE " 10.000 iDEGREES/MINI

PEAK DATA INPUT:

DATA RATE ISECONOSIDATA POINT) - .80OOO00

TEMPERATURE OF FIRST POINT OF DATA - 590.133 (DEC KELVIN)

PEAK BEGINS AT 600.93 DEC. K. tPEAK HEIGHT - 2.531

PEAK ENDS AT 60Z.0 DEC. K. tPEAK HEIGHT - b.3Z)

AREA-HEAT CONSTANT - .00100649 RANGE PER ENCODER J)IT (CONORAN-MCALISEC PER ENCODER UNIT)

THERMAL RESISTANCE - .ZOJ23 UEG. K.-SEC.IMILLICAL

TN- 601.06 DEG. K.

77
AFWAL-TR-81-4177
Volume I

'A
a
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0
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AF'WAL-TR-81-4177
Volume I

tl.10.71.Z LEAD

HEAT OF FUSION (CALIGRAN) 5.500

aEI6HT 4MG) U= CALIBRATIO4 STANDARD - 4.900

RANGE = 5.000 (NILLICAL/SEC FULL SCALE) SCAN RATE - 5.000 (DEGREES/MIN)

PEAK DATA INPUT:

DATA RATE (SECONDSIJATA POINT) = dO000000

TEMPERATURE OF FIRST PUINT OF DATA - 595.067 (DEG KELVIN)

PEAK OEGINS AT 600.47 DEG. K. (PEAK HEIGHT - 6.421

PEAK ENDS AT 601.80 OEG. K. (PEAK HEIGHT - 5.86)

ACEA-HEAT CONSTANT - .00049bI5 RANGE PER ENCODER JNIT (CON*RAN-NCALISEC PER ENCODER UNITI

TIERNAL RESISTANCE - .19851 DEG. K.-SEC./MILLICAL

TM- 600.63 U•G. K.

79
AFdAL-TR-81 -4177
Volume I

C
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IL
0

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tl, o41
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41, o lt

41, e I

ses0 5.sssss•ss S ssS5 5ssssssOss

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5 04.5

4 * ~580
AFWAL-TR-81-4177
Volume I

d1.L0.7.ZZ LEAD

"NEAT OF FUSION (CAL/GMANII 5.500

ueIGHT ERG1 OF CALIBRATIO4 STANDARD 68.500

RANGE - 2O.OOo IMILLICALISEC FULL SCALE) SCAN RATE 60.000 (DEGREES/MINI

8

PEAK DATA INPUT:

DATA RATE ISECONOSIDATA POINT) - .80000000

TEMPERATURE OF FIRST POINT OF DATA - 541.0b7 (DEG KELVIN)

PEAK BEGINS AT 604.00 DEG. K. (PEAK HEIGHT - L1.531

fPAK ENDS Ar 616.60 DEG. K. (PEAK HEIGHT - ZZ.04)

AKEA-HEAT CONSTANT - *DO 9,53e RANGE PEK ENCODER JNIT tCON*RAN-RCALISEC PER ENCODER UNIT)
TdERMAL RESISTANCE - *37LL4 DEG. K.-SEC.IMILLICAL

IN- bOb.02 DEG. K.

81
AFHdAL-Th-81 -4177
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6L.LO.7.23 LEAD

"NbAT
OF FUSION ICALIGRAMI - 5.03

.*EIGHT INGO OF CALISRATIOV STANOARD - d.O0

RANGE - 20.000 (NILLICALISEC FULL SCALE) SCAN RATE - 80.000 tDEGREESININ)

PEAK DATA INPUTs

OATA RATE (SECONDS/DATA POINTA .80000000

TERPERATURE OF FIRST POINT OF DATA - 5e1.067 (DEG KELVIN#

PEAK GEGINS AT b04.30 DEG. K. IPEAK HEIGHT - It.$8W

PEAK ENDS AT b1b.60 DEG. K. tPEAA HEIGHT - 2S8.52

AtEA--MkAT CONSTANT - .00095949 RANGE PER ENCODER JNIT (CONORAN-NCAL/SEC PER ENCODER UNITI"
TrIERMAL RESISTANCE - .3?412 DkG. K.-SEC.IUILLICAL

"TN- 6Ob.0b DEG. K.

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OL.IO.7.d4. LEAD

.4tAT OF FUSION (CALI6kAN) 5- 0

STANDARD 8 .500
:E16"T 4MG) UF CALI "RATIJN
AAnGE - 4OOOO (MILLICA.JSEC FULL SCALEI SCAN RATE 40-000O (DEGREES/At
IN)

PE& DATA IN4PUT:

IjArA NATE IOECOHDSIDATA PU1NTf .d0O00OO0

TEMPERATURE ti.FIRST POINT OF UATA 5b0~.53.u (ED( KELVINI

PEAIL SEGIV4S AT 603.20 DEG.. K. II'EAA HEIGHT - .)

PEAK E1N05 AT 609.60 UL6C. K. tPLAK IIELG.T - Ib.141

AAEA-HEAT 4C0W~ANT - *000'007do RANGE PER ENCUDER JNIT (CUNNkAhNCAL/SEC PER ENCODERi UNIT)
J.IE.CNAL kESI$TANCE - .2415b DEG. K.-SEC.IMILLICA,

TM- 60J.5?. UEG. K.

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8L.1.7*.la LEAD

HEAT OF FUSION ICALIGRAMI 5.500

aEIGHT (Ma)
OF CALIBRATION STANUARD - 8.500

RANGE - LOOO0 (MILLICALISEC FULL SCALE) SCAN RATE - 40.000 (DEGREESIMIN)

PEAK DATA INPUT:

OATA KATE (SEGONDSlOATA POINT§ - .60DOOOOD

TEMPEKATURE OF FIRST POINT OF DATA - bO.533 (DEG KELVIN)

PEAK BEGINS AT 602.67 DEG. K. (PEAK HEIGHT - 4.851

PEAK ENDS AT 609.07 DEG. K. (PEAK HEIGHT - 7.03)

AAEA-HEAT CONSTANT - .0O0045bZ RANGE PER ENCODER JNIT (CON*RAN-MCALiSEC PER ENCODER UNIT)

TIERMAL RESISTANCE - .Zd499 DEG. K.-SEC./NILLICAL

T4- 603.02 DEG. K.

87
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51.0.7.Zb LEAD

HEAT OF FUSION (CALIGRAM) 5.500

wEIGHT (MG) OF CALIURATIU% STANDARD - ."O

KANGE - 10.000 (MILLICALISEC FULL SCALE) SCAN RATE - ZO.OO0 (DEGREESIMIN)

PEAK DATA INPUT:

DATA RATE ISECONOSIDATA POINT) - .60000000

TEMPERATURE OF FIRST POINT OF DATA - 580.267 4DEG KELVINI

PEAK BEGINS Ar bOI.07 DEG. K. tPEAK HEIGHT - 3.7)

PEAK ENDS Ar 605.33 DEG. K. iPEAK HEIGHT - 5.761

AAEA-HEAT CONSTANT - .0009i433 RANGE PER ENCODER JNIT tCON*RAN-MCALISEC PER ENCODER UNITS

THERMAL RESISTANCE - .268B3 DEG. K.-SEC.MINLLICAL

TN- bOI.45 DEG. K.

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8L.i0.7.Z7 LEAD

"NEAT OF FUSION (CALIGRAM) - 5.500

WEIGHT (MG) OF CALIBRATIO4 STANDARD U.500

RANGE - 10.000 (MILLICALISEC FULL SCALE) SCAN RATE - 10.000 (DEGREESININ)

PEAK DATA INPUT:

DATA RATE (SECONDS/3ATA PJINT) .80000000

TEMPERATURE OF FIRST POINT OF DATA = 590.133 (DEG KELVIN)

PEAK BEGINS AT 600.53 DEG. K. (PEAK HEIGHT - 5.30)

PEAK ENDS AT 602.9J DEG. K. (PEAK HEIGHT - 8.08)

AKEA-HEAT CONSTANT = .00047209 RA4GE PER ENCODER UNIT (CON*RAN-MCAL/SEC PER ENCODER UNIT)

TIERMAL RESISTANCE .L593b

Z DEG. K.-SEC.IMILLICAL

TM- 60D.61 DEG. K.

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Volume I

81.10.7.28 LEAD

HEAT OF FUSION (CALiGRAN) - 5.500

WEIGHT (MG) UF CALIORATIJN STANDARD = 8.500

RANGE * 5.000 (NILLICA;..SEC FULL SCALE) SCAN RATE - 5.000 (DEGREES/MINi

PEAK DATA INPUT:

DATA RATE (SECONOSIDATA POINT) = .80000000

TEMPERATURE OF FIRST POINT OF DATA - 595.067 (DEG KELVIN)

PEAK dEGINS AT 600.00 DEG. K. 4PEAK HEIGHT - 4.24)
PEAK ENDS AT 601.73 DEG. K. (PEAK HEIGHT - #.491

AREA-HEAT CONSTANT - .00095500 RANGE PER ENCOUER JNIT (CON*RAN-MCAL/SEC PER ENCODER UNIT)

THERMAL RESISTANCE - *•b9!8 DEG. K*-SEColNILLICAL

TM- bOO.13 OEG. K.

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APPENDIX B.l

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-2 Oo9-00 69-0 059-007 1-0071-007 1-00 73-007
-3073-0071#-0076-0076-0077-0077-0077-0077
-0077-0077-0079-0077-0079-0079-0079-0074
-0079-0079-0079-0079-0082-0079-0082-0083
-J 083-00 83-008 3-008 3-00 83-00 83-0 0 83-00 86
-20835-0087-0086-0086-0087-0087-0087-0007
-3067-0089-0087-0087-0069-0089-0389-00ii9
-2089-0089008d90089-0089-0089-0089-0089
-2091-0092-0092-009Z-0092-0093-0093-0093
-0093-0093-0093-0043-0093-0095-C093-0094
-00j93-0095-009 5-0096-0095-0097-009 7-009?7
-209 7-0097-0091-0097-0097-0097-0047-0097
-J097-0097-0097-0097-0097-0047-0099-0097
-D007-0099-0099-0097-0099-0097-DO,)1-02917
-3047-u099-0047-0097-0097-0097-0099-0099
-ý009-0099-0099-0099-0099-0099-0099-0099

99
AFWAL-TR-81-4177
Volume I

APPENDIX B.2

PROGRAM KINETIC

SAMPLE INPUT CARDS

100
AFWAL-TR-81-4177
Volume I

100- KINETIC SERIES FOR GULF ATS (50 GRAM EVALUATION)

110= 0.30920 0o21155 0.19110 0.17285 0.18999
120= 0.44179 0.29991 0.24575 0.22965 0.23405
130= 435.24 432.49 430.94 430.12 429.70
140= 605.75 603.22 601.97 600.84 600.38
150=0.000905490.000917600.000920920.0009?4?90.0O091141
160= 0.000986960.000995400.000971770.000990290.00097558
170=
180=11110001100 390 670 340 650 399 680 374 5P5 353
600

101
AFWAL-TR-81-4177
Volume I

APPENDIX B.3

PROGRAM KINETIC

SAMPLE OUTPUT

102
 AFWAL-TR-81 -4177
Volume I

Lk
&IitTC Stt<ItS
4.v6'INETIU FUR Gjkr 4Tj (!)0 GRAM EVALUATION)

PMCJG.A~I CONTROL CARD

I.LIEUJOIIOI00000000L) 38~J 610 340 baU 396 be) J7% 5b5 353 bo0 0 0

LALIVRATIUN DATA

MLLT1NG POINTS:
(u4ITS OF A(ELVINS)

HEAT KATE fM4(INUJIU'iD DELTA TM(LEAO) DELTA

nsu.voo f3.zqe' 5.4'. eO5.75 5.10

'.0.0000 4.3Z.49 Ž.69 o03.Z2 Z.57
'30 . 9#
It.00 1. 1,4 t01.tl 1.02*
1.oo430.12 .3z 600.64 .19
to 000 #29.1/, -. 10 bO0.36 -. Z7
e.!?000 e*19.dO 0.00 600.es 0.00
1.z500 '.t9.n0( G.00 600.65) 0.00
. 6 ?5 0 %e1.49.80 0.00 boo. b5 0.00
.415 49.uo 0.00 630.t5 0.00

CA-COLATEO THERMAL CORRECTION FACTORS

STRAIGHT LIN- SHONING TRUE TEMPERATURE
VERSOS JaSERVED TEflPE4ATURE

HEAT RATE IN4TERCEPT SLOPE

nO.0000 -0.30706 1.00199

40.0000 -Z.99398 1.00070
20.0000 -1.44c69 L.00070
10.U0000 -. b4?53 1.O0700
ns.0000 -. 32.799 1.00100
Z.to0c0 .00000 1.00000
1.250C .00000 1.00000
.bzt50 .U0000 1.0000
.3125 .00000 1.00000

fHERMA.. RESISTANCE (LAG CORRECTIONI

(IN UNITS Of KELVINSI(MCAL/SEI)i

MEAT RATE TRIIN'JIUi) TR(LE&O) TR(AVERAGEI

- 6.0030 .s09z0 .,'.t.1?9 .37550

140.0000 .21155 .29491 Z25573
20.0000 .10113 Z,457ti .21313
10.0U04 .172o5 Z24365 .20115
5.0000 *Lb9r9d .23405 .20202
Z.50.-0 U.00000 0.00000 0.00000
1.4s5" L.03333a 0.00003 0.00000
.60 0.00330 0.OOOGu 0.00000
.32 O.00000 0.00003 0.00000

103
AFWAL-TR-81 -4177
Volume I

KIN=rIL *.4IfttNTIC St:,(:S FUJR 6JLF ATS 4'5J 6R.- tVALUArIUN,

ARE~A t1EAr CONSTANT

(UNITS JF INVcA~k ENCOUUE UNITS

I1EAT R~ATE CUN(INOIL1,4 CUN(LEAJ)) CLJNIAVEbiAbtI

00.0001) .00O93ý-%' OOUY6666 .000947L*
140.O0jJ *OOCVIb.J qO09~d54U .0OOOY5L50
zC.Ouý;) .00092jl .0OU47177 .0cfjqibj3,
10.00J. .00Jv334z .0004,Y? .0C911
2.5,ao COM a 1.0oJU.,30 0.co~u
i.250. ;,.OOOL033j 0.00030ij3u O.OQCOO('.0)
.6150 0.,0OOjUO)0) 0.000006
OOJ(auO~
.31e, 0.00000,C0)5 0.0000ý (J.O0cu"LuO

icLIr4TtlG) Uf, SAMlPLE- L.50

AAN~rEMILLIC4LISEC F~ULL !O;ALfiJ-, 0.0

rF1lVrATtkLREwG KELVINI UF F~iks eutNr UN LIATA TAPE- 3/%.C.7

OATA KATE ISE."ONDS PER JATA pIr- .6000

x TE?¶I'EKATU-(L Ji1IN~AL Y
(SECUNU~i tKELWI'4~ 1cu.

*dý 3Z4*.,J -L10.

i JZ53.L3 -jib.

3.eo sdiale -ILL.

4.dO 32y4a3 -IL.

5.ba 33u.,%J -LO.
1L..45J -10.t.
k1ed 347.b. -90.
ie'j
340.01 0

.1304 r3
Jilt.

kL.zJ 344.933-.
1.2.03 isq-)

104
AFWAL-TR-81 -4177
Volume I

i G**8L
t to L').L1 I(J)

e.. 3 o! . 13 .

46v 300.33 -Wo .

341.00 461 . du

S ife'.01 -10.

3..) 313.L3. -7,e.

'#I.bO 379..41-.
43.t.J sdo.ot) -7cs.
41.'..)j Jd1.bt -7d.
~4d) 3dZ.73 ~ d
q.!).oO 36d3.dU -11.

d47. ZJ JdD.93--.
'f.U.J0 3ts70J -to.
',6.8) 30d..)I -ii

'4900 IO.C1 -71.

Dc,. -ti *90.13 0 -17.
PO.u. t7.'L -?7.

54,4 395.113? -7b.

55.zý 39b.0o2 -1b.
5o.uj. 397.01 -77.
5b. ts 34d. 13 -I
57.ao 39V.80 -1o.
D9.40. '40.93.8 -11.
60.3.) #0.vsoO -11.

bL.60 %05.b.J -o.

105
AFWAL-TR-81 -4177
Volume I

A14trIN *o.51.4. LL T

bq4J 1409. let -77.

05.tJ( 40M.I3S -11.
O6eu I L .30
.0 -71).

bbf.J 4 Ls. I -1b.

b8.d0 41''..13 -71.

I U.4I 0416.8? -1b.

7Z0 tzo.ai -7b.

7o.MJ he . 4U -75.

17. b5 4ZO. -7 -75.

60.00 44J. 73 -~
81.63 43L.6? 73
Be . fl 11U.67 -73.
a 4 .Uvf 435. 00 -3
64.6.,6 3(3.07 -73.
D5.bj 437.1L4
66.40 4438.z0 t4
07. ZC 1439.,e -7#..
#d5.00 1#1#0.3 -7s
dab 4~4
#19.00
90 .,# 43.!03 -74..
91.aj '4441.60 -73.
9,c. O I 100. b -74.
Yz.6.j It46.4 -73
93.60 -147.0 do4

95.zo 1#49.93 -7,.

96.00 %S1.01, -74.

9 1. 6. #5 3.1L3 -73.
98.,#) 54~ -7s.
99~a0 -74.
100.0) ft50. 11 -73.
1uo00 451.4to
't -73.

L1e . 40 459. 23 -73.

1o3 .4e1 460,. 6 0 -73.
104#.00 41.
* b7 -U1.
L04.83 #oz. 13 -7z .
L0.OS.b # Jo.8do -7,e.
l0b.13f 464t.81 -7e.
107.eL, to5. 4 - It.

106
AFWAL-TR-81-4177
Volume I

•KNTITC **81.L5.l0.14.1 GULF ATS

108.00 4b7.00 -71.

108.83 468.07 -71.
109.6b0 4o9.13 -71.
110.40 140.zo -71.
111.10 4IL.2? -70.
112.03 472.33 -69.
11.d83 413.40 -69.
113.63 474.47 -b9.
114.4#0 475.13 -68.
115.ZO 47b.0o -66.
116.03 477.67 -b8.
116.80 47d.13 -67.
111.o3 479.80 -66.
118.40 480.87 -65.
119.23 481l.93 -64.
120.00 't83.00 -64.
1Z0.83 48I.07 -63.
12L.o0 4o5.13 -6z.
tez.40 6db.ZO -61.
1Z3.ZO #87.Z7 -60.
124.00 488.33 -59.
124.60 469.40 -58.
125.63 %90.47 -5b.
126.13 491.53 -54.
1Z7.23 492.bO -53.
i1d.03 493.67 -5Z.
1z2.80 494.73 -50.
1Z9.60 495.80 -49.
130.40 '9b.87 -41.
131.20 497.93 -4,
132.03 499.00 -43.
13Z.O0 500.07 -4L.
133.60 501.13 -39.
134.40 sOZl.ZO -3b.
135-.0 503.27 -34.
136.03 504.33 -32.
136.83 505.40 -Z9.
137.oO 506.47 -zb.
138.40 501.53 -23.
139.Z0 50d.60 -20.
140.00 509.67 -17.
140.80 5L0.73 -14.
141.63 51L.80 -LO.
#? .14 51Zd7 -8.
1*3.Zo 513.93 -3.
144.00 515.00 L.
144.80 5L6.07 5.
145.b0 517.13 9.
146.4U 518. ?0 13.
147.10 519.27 18.
148.0D 5O.33 Z4.
148.80 .
2160 Z9.
149.b3 5Z.47 35.
150.40 5Z3.53 40.
151.ZU 5Z4.oO0b.
15Z.00 5Z5.67 53.
152.80 5z.173 59.

107
 4177
AFWIAL-TR-81-
Volume I

KINETIC .w8.51.41GULF ATS

153.60 !)Z7.80J66
L564.410 7za.87 72.
155.210 529.93 79.
156.00 631.00 8eb.
156.b0 5632.07 YJ .
L57.63 63-3.13J 100.
L511.443 634. ZQ 108.

160.00 !06.33 124. -

160.80 537.,40 13.i.
161.0O 538.47 141..
162.1#0 L3.649.
163.ZO 640. 60 1:)8.
164#.00 641.6 7 L6b.
1184.80 542.7s Oj.
L65.60 543.60 183#
166.1#3 54I,#.81 19;j.
167.20 546.93 197.
166.00 547.00 2014.
166.00 548.01 Z09.
169.60 549.13 Z1i.
170.40 s5u*Z0 216.
171.20 ssiaL~ Z17.
172.00 562.13 a16
172.80 !03.40o M1.
173.ba 55,#.47 206.
0174.40 665.63j 91#?
176.20 556.60 Ldb.
176.00 55 I.b1 114.
176.63 !08.73 159.
117.60 569.80 L144.
178.4#0 560.87 129.
179.Z0 561.93 113.
180.00 563.00 9Id.
180.80 66b4.07 83.
181.6D 66b5.13 69.
182.40 !i66.20 66b.
103.Z0 561.27 44t.
184.00 568.13 32.
184.80 5b9.410 Z3.
185.60 to70.4#7 13.
186.4#t !71.53 6.
187.20 572.b0-2
185. 00 673.6 -9.
188.80 674#.73 -6
169.60 57to.80 -20.
190.40 !i76.87 -26.
191.20 !077.93 -30).
192.00 679.00 -33.
192.83 680o.07 -37.
193.60 581.13 -4#0.
194.40# 682.20 -004.
196).,0 683.27 -46.
196.00 584.33 -49.
19b6.0 585.410 -5L.
197.60 686.4t? -541.
198.40 687.53J -56.

108
AFWAL-TR-81 -4177
Volume I

k.1NETIC *#.L.011 GULF ATS

199.20 586.00, -56.

200.00 5 89.6b? -!)9.
200.80 590.71 -61..
20i.bo 591.80 -61.
201#40 59Z.87 -Olt.
203.Z0 s193.93 -b6.
Z04.00 no95. 0U -6?.
204.80 !090.01 -b6).
205.60 597.13 a9
204).40 596. Z0 -71.
207.20 ý,99.z? -71..
.20a.00 *00.33 -7z.
206.80 bUL.-40 -73.
?09.ao 6002.41 -14.
Z10.40 603.53 75
ZLI.ZO taOt.bo -75.
212.00 605.67 -71.
2Z1..80 60b.73 -7?.
Z13.60 bO7.dO -19.
Z14W.40 b08.87 -19.
215.20 b09.93 -d0.
21b.00 611.00 -80.
216.bO biZ.07 -al.
217.60 1613.13 -82.
218.,43 614.Z0 -83.
219.23 b1.5.ZI -83.
220.00 616.33 -alt.
2e20.60 61.7*40 -85.
221.60 618.47 -80.
2i22.4#0 b19453 -07.
223.g20 620.60 -88.
224.00 bil.67 -89.
Z24.80 b22.7zs -89.
225.60 623.80 -89.
"£6.43 bz24.87 -y0.
2Z7.z0 o25.93 -91.
Z28.00 627.00 -9L.
2283.80 628.07 -92.
229.60 bOZ9.13 -9s..
230.4#3 630.10 -93.
231.Z0 631.27 -93.
Z32.00 632.33 -4
232.80 633.40 -94.
233.60 b34.47 -95.
234.,40 63ti.53 -9b.
235.20 63b.b0 -96.
23b.00 637.o1 -95.
236.80 638.73 -9b.
237.6D 639.80 -12b.
23$8.40 640.07 -93.
239.20 641.93 -9b.
240.00 b43.00 -91.
240.80 64#4.07 -97.
241.60 645.13 -97.
24Z.40 646.20 -96.
243.20 641.7oz -96.
24#4.00 648.33 -96.

109
AFW4AL-TR-81 -4177
Volume I

KINE4TIC 9**061.15.10.14.L GULF ATS

24#4.60 b49.900 -96.

245.60 650.47 -b
24.d40o b5L.53 -96.
i't7o.20 b5z.60 -96.
V46.00 653.6? -9b.

i49oou b55.80 -9!).

250.40 b5b.67 -95.
251.20 65 7. 93 -95.
Z51.00 659.00 -95.
252.60 660.07 -95.
&03.0~ b61.13 -94.
15,4.40 bo2.20 -94 .
255.20 663.27 -94.
256.00 664.33 -94.
Z56.60 b65.40 -93.
257.60 b66.4#7 -93.
258.4#3 5)67.53j -43.
259.20j 666.oU -93.
Z60.00 b69.67 -92.
260.0a b73.73 -92.
261.60 671.60 -2
262.40 672.67-91
263.20 673.93 92
264.00 675.00 -2
264.oOa b7b.07 -92.
265000 b77.13 -91.
266.4#0 67d.20 -9z.
267.?0 sF?9.2? -yz.
Z6om.0 680.31 -92.
26d.60 661.40 -92.
269.60 682.4? -920
210.,#0 663.53 -93o
2,11.23 664.60o -93.
272.00 665.67 -93.
272.60 666.73 -93.
273.60 687.60 -93.
274.o,0 666.67 -93.
275.20 669.93 -930

110
AFI4AL-TR-81 -4177
Volume I

•ew
oF0

- 0o

II'

* ...---

*41 4 4I.

*N,

S• : * .4

I * 0

1 *
AFWdAL-TR-81-4177
Volume I

K INETIC *9@~1.15,1O.1,.1 GULF ATS

MAXIMUM ORDINATE- eL7.0 OCCURS At 551.£7 DEG KzLVIN.

PcAK SkARCH LIMITS: START PT.- 119.5 STOP PT.- bb9.? DEG. KELVIN

THE PEAK ENDS AT 25 POINTS FROM START. THE Y AT THIS POINT IS -7t.77
THE BASELINE EQUATION IS Y- -.3J?40E*.0*X* L,0J5OE*0e

T*E PEAK STARTS AT 155 POINTS FROM THE START. THE Y AT THIS POINT IS -bi.17
THE BASELINE EUJATIUN IS Y- LZJ'f5E*O(X+ -. tbJOeE.OZ

PEA( BEGINS AT 488.33 OEt. KELVIN 4PEAK HEI6HT - -o7.171 IDATA PT. 155)
PEAK ENDS AT 595.00 DIG KELVIN (PiAK HEIGHT - -75,.71 (DATA PT. Z55)

NJM8ER OF POINTS IN PEAK- 100

BASELINE SHIFT CUMPENSATEi IS -3.88

ItMPERATURES HAVE NOn dEEN CORRECTED FUR THERMAL LAG9 SCAN RATE EFFECTsANO CALIORATION EkRO(.
MAGNITUDE OF THE COKKECTIJN AT MAKIMUM ORDINATE IS: -J.15

..... ,**,.W 81e15.IO.14.2 GULF ATS w*

urIGHT4NG) OF SAMPLE- t.07

AANGE(MILLICALISEC FULL SCALE)-, 20.0
SCAN kATEIOEG PER NINUTE(- 40.0
TEIPEKATUREIDEG KELVIN) OF FIRST POINT ON DATA TAPE- 24.00

DATA RATE (SECONDS PER DATA POINT)- 1.5000

X TEMPERATUKE ORIGINAL V
(SECONDS) (KELVINS) 4E.U.1

L.53 324.00 -10o.

3.00 325.0Uj -160.
4.50 3Z6.00 -159.
6.03 327.00 -Lb6.
7.50 328.00 -L67.
9.00 329.00 -Lbo.
10.50 330.00 -164.
12.03 331.00 -163.
13.)0 33Z.00 -16z.
15.03 333.00 -1be.
16.50 334.00 -162.
18.00 335.J0 -1bJ.

112
AFWAL-TR-81-4177
Volume I

KINETIC ***dL.15.10.14.2 GULF ATS

19.5; 336.00 -1b3.

Z1.00 331.00 -164.
2Z.5u 338.00 -164.
ZIt.0 339.00 -164.
25.50 40.0 -lb
Z7.0 i31.00 -1to5.
Z!.O 342.00 -Lob.
30.00 343.00 -1b6.
J1.70 344.00 -1b6.
33.03 345.00 -1b.
310•0 34o.O0 -160.
36.03 341.00 -17.
37.50 348.UO -".8.
3Y.03 349.00 -L69.
40.!2 350.00 -1b9.
4z.O) 351.00 -110.
'3.53 35Z.00 -L70.
45.00 353.00 -169.
46.5D 3b4.00 -L18.
48.03 355.00 -1o0.
4y.53 356.00 -168.
51.0 357.00 -lob.
5Z.50 358.00 -168.
54.03 3,39.00 -168.
55.50 360.00 -L67.
57.03 361.00 -LoI.
58.!0 361.00 -168.
60.03 364.00 -168.
61.53 364.00 -166 .
b3.03 3t5.00 -168.
64.50 3bb.00 -Lo8.
66.00 367.00 -L69.
67.5) 368.00 -169.
69.00 3b9.00 -169.
70.50 310.00 -169.
72.03 371.00 -170.
73.5" 372.00 -110.
75.00 373.00 -170.
76.0 371#.00 -170.
78.03 375.00 -170.
79.50 376.00 -LL.
U1.00 377.00 -1TL.
8Z.50 37s.00 -L71.
8,4.03 319.00 -171.
5.50 800.00 -L7I.
87.03 381.00 -172.
88.50 382.00 -072.
90003 383.00 -11.
91.50 384.00 -LIZ.
93.03 35.00 -M71.
94W0 386.00 -M17.
9b.03 38?.00 -17s.
97.50 388.00 -172.
99.03 389.0U -M71.
100.53 390.00 -17Z.
102.03 391.00 -172.
103.53 39z.00 -173.

113
AFWAL-TR-81-4177
Volume I

%INMTIC ***d.1,.1 4a GULF AT4

105.03 3J.30 "17z.

LOb.3 394.00 -1i1.
10U8.u 395.00 -02.
L09.53 34b.00 -172.
LL.0) 397.00 -O7z.
i1.50 396.00 -172.

115.50 400.00 -LM.

117.05 401.00 -171.
I1d.50 40Z.00 -1,1.
120.00 403.00 -171.
121.50 404.00 -Le.
123.3J 401.00 -171.
1Z4.50 40b.00 -017.
126.0a 401.00 -17L.
127.53 400.00 -171.
19.00 409.00 -M72.
1s0.50 410.00 -LU.

133.50 41Z.0.) -171.

L35.03 #3J.00 -170.
136. I 414.00 -170.
18.03 410.00 -171.
139.50 46Lb.00 -100.
0)
L-hO. #O.O -171.
14Z.50 415.00 -110.
144.30 419.00 -703.
145.50 4#0.00 -170.
147.02 421.00 -110.
14d.,0 42z.00 -173.
150.0) 4zi.00 -L69.
15.,25 4Zt.00 -170.
153.0 44:.00 -169.
15,.50 42B.00 -169.
1b6.00 407.00 -169.
157.50 428.00 -169.
159.00 4Z9.00 -169.
160.50 -30.00 -169.
162.00 431.00 -169.
130.53
lbz.ca 432.00
#3k.00 -Lb.
--L6#.
165.00 433.00 -Lod.
16b.50 434.00 -L16.
165.02 435.00 -166.
169.5 431.00
1 -166.
171.03 437.00 -1b6.
172.50 438.00 -L65.
174.00 439.00 -Lbt,
175.50 440#.00u -165.
177.0 f441.00 -lb5.
178.53 44Z.00 -Ib6.
150.02 4#43.00 -L64#.
151.53 0 4144.00 -163.
183.02 445.00 -L64#.
154.53) 4416.00 -163.
186.03 #441.00 -163.
187.52 1448.00 -162.
18Y.0a 449.00 -- 161.

114
AFWAL-TR-81-4177
Volume I

K NETIt *I*d .CSO.. GULF ATS

19Z.03 #51.00 -0id.

193.50 45/.00 -Ibl.
195.03 0.3.o0 -160.
196.53 4054.00 -109.
196.03 4)5.00 -156.
199.53 456.00 -159.
Z01.0j .#57.00 -158.
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115
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Volume I

KINETIC *C981.15.10,14.2 GULF ATS

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116
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Volume I

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KINETIG •oI.,.IG,. GULF ATN

MAXIMUN ORDINATE- 23L.U JCCURS AT 5JO.OC UEG KELVIN.

PeAK SEARCH LIMITS: START PT.- 340.0 STOP PT.- b5O.O OEG. KELVIN

THE PEAK ENDS AT L POINTS :n START. THE f AT THIS POINT I5 -1b5.,e

THE BASELINE EDUATION IS Y- -.J3#Ija÷OC*X+ -.104i4E+0Z

THE PEAK STARTS AT 13b POINTS FROM THE START. THE Y AT THIS POINT IS -lbS.12
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PEAK BEGINS AT 45u.30 DEG KELVIN (PEAK HEIGHT --1o5.L7) (DATA PT. 1351
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TEMPERATURES HAVE NUw tEE4 CORRECTED FUR THERMAL 4AG, SCAN RATE EFFECTAND CALIBRATION ERRUK.
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AFWAL-TR-81 -4177
Volume I

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AFWAL-TR-81-4177
Volume I

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123
AFWAL-TR-81-4177
Volume I

KI NTIt **9•Lts.I5 .14.J GULF ATS

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124
AFWAL-TR-81-4177
Volume I

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125
AFWAL-TR-81-41 77
Volume I

KLiNETIC @8.5.O1. GULF iTS

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126
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Volume I

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L008.00 b59.00 -343.
1011.00 bo0.00 -34•.
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1017.0) b56.00 -341.
100.O0 bb3.00 -336.
LO3.00 bb4.00 -s36.
LOZ6.00 b65.00 -334.
1029.00 560.00 -333.
1032.O0 b67.00 -334.
1035.00 b68.00 -331.
1038.00 669.00 -333.
L041.00 670.00 -331.
L044.00 571.00 -329.
SL0#7.00 b6z.00 -328.
1050.00 573.00 -330.
1053.00 b14.00 -329.
1056.00 61>.00 -3Z9.
1059.01 b7c.00 -3Z9.
106Z.00 607.00 -32z.

127
AFWdAL-TR-81 -4177
Volume I

KINETIC *e@81.I5.10.14.S GULF AT5

1065.00 b76.OU 330a.

1066.00 079.00 -333.
1071.00 680.00-3.
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1077.00 DOZ.00 -33?.
L060.00 b63.00 -j335.
1063.00 b84.00 -335.
1006.00 bdto.00 -336.
1,089.00 bo0.00 -330.
1092.00 667.00 -Jib.
1095.00 666.00 -335.
1098.00 b89.00 -333.
1101.03 690.00 -33:0.
1104.00 691.00 -337.

128
AFWAL-TR-81 -4177
Volume I

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AFWAL-TR-81-4177
Volume I

KINETIC *9*dL.15.10.1,.3 GULF ATS

AKXIUfUM OkUINATE- L07.0 OCCURS AT 51,j.UO EG KELVIN.

PtAA SEARCH LIMITS: STAAT PT.- $96.0 STOP PT.- b2O.0 UEG. KELVIN

TrIEPEAK ENDS AT ZJ3 POINTS FROM START. THE f AT THIS POINT IS -J05.67
THE BASELINE EwUATIUN IS Y- -. 399JOL*OUS+X -.Z7211E+03

THE PEAK STARTS AT LJO PUINTS FROM THE START. THE Y AT THIS POINT 15 -323.01
THE BASELINE EJUATION IS Y- ,'7NU9•÷OO.A+ -. 0175lE#03

rVAA BEhINS AT 452.00 OE( KELVIN (PPAK HEIGHT -- 37Z.591 IOATA PT. 1291
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NJNdEI OF POINTS IN PEAK- 104

BASELINE SHIFT COMPENNATEO IS -8.bO

TEMPERATURES SAVE NOWBEE4 CORRECTED FOR THEKRMAL LAG, SCAN RATE EFFECTANO CALIBRATION ERROK.
MAGNITUOE OF THE CURRECTION AT MAXIMUM URDINATE IS: -. 23

*99*9*W** 681.1L.B.Z1.? GULF AT$

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12.03 375.00 -103.
18.03 3o.00 -116.
74.00 327.00 -119.
30.03 3Z8.00 -1id.
36.03 379.00 -177.
4.00 330.00 -1Z7.
48.03 331.00 -1ZY.
54.03 337.00 -1Z9.
60.03 333.00 -128.
66.0 33,#00 -1Z9.
7Z.03 335.0O -131.

130
AFWAL-TR-81-4177
Volume I

PCI NET IbL e . LOZ GULP- ATS

7e°0O 33b.00 -1Z9.

84.0) 337.00 -130.
90.01 338.30 -12).
90.00 i39.00 -129.
102.03 300.00 -127.
lO.01 341.00 -130.
L14.O0 3+Z°.00 -1z9.
120.03 343.00 -131.
126.00 314.01 -130.
132.03 3 .130 -12;.
138.00 34b.00 -1Z9.
144.00 3,#7.00 -129.
150.00 346.00 -133.
15b.03 349.30 -1zd.
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168.03 351.30 -13?.
174.00 3,2.00 -- Z9.
180.00 353.00 -131.
186.O 354.00 -L2.
192.03 355.U0 -LZ8.
198.00 356.00 -130.
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210.00 358.00 -127.
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234.03 36z.00 -131.
240.00 303.00 -136.
246.00 304.00 -128.
z5z.03 365.00 -LZI.
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264.03 307.00 -131.
Z70.00, 308.00 -129.
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28a.03 371.00 -1iz.
294.O0 372.00 -Lz1.
300.03 373.00 -IZ9.
306.00 374.00 -129.
312.03 375.00 -LZ9.
318.00 376.00 -119.
324.00 377.00 -131.
330.00 378.00 -129.
336.00 379.00 -U3L.
342.00 380.00 -L31.
348.00 381.00 -130.
354.00 382.00 -131.
360.00 3d3.00 -13d.
366.00 384.00 -132.
372.00 385.00 -L33.
378.03 38b.00 -131.
384.00 387.00 -L3L.
390.00 388.00 -132.
39o.00 389.00 -133.
402.00 390.00 -13L.
#08.60 391.00 -138.
414.00 39Z.00 -131.

131
AFWAL-TR-81 -4177
Volume I

KINETIC **UdLeI.8l1.21.7 GULF AIS

#020.01 393.00 -130.

432.33 395.00 -1st.

4#31.03 39b.DO -131.
44.3 391.00 -133.
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436b.03 399.00 -133.
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534.00 411Z.00 -129.
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132
AFWAL-TR-81-4177
Volume I

KINErIL •**dL.Ijj*.o.7 GULF ATS

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174.00 452.00 -79.
780.02 1#53.00 -80.
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133
AFWAL-TR-81-4177
Volume I

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1296.00 539.00 -129.
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134
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Volume I

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KINtTIC •dj.I.C.e1.o 'ULF ATS

NAAIMUM OROINATE- I JCCUkS AT

L.O %dl.00 utG KELVIN.

P:AK ScARCH LIMITS: START PT." 353.0 STOP PT.- 599.8 OEG. KELVIN

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THt PEAK STARTS AT iLI POINTS FROM THE START. THE Y AT THI5 POINT IS -7l.94
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 AFWAL-TR-81-4177
Volume I

2. KINErI( *Ow KINETIC SEvUES FUR GJLF ATS 15U GRAM EVALUATION)

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AFWAL-TR-81 -4177
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XINETIU *4* #.INIETLC SEKI1:5 FUtK GJLF ATS (5a GR~AM EVALUATION)

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151
AFWAL-TR-81 -4177

Volume I

KINETIC ** INETIC StKIES FOR ,iJLF ATS (50 GRAM1 EVALUATION)

*~*U9#** CJRVE NUM$ER 4.

TIME TEMPi:MATUkE ODc/J C

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AV0(AGE ACTIVATIOU' ENERGY = 19.900

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&INLTIC wv kNETIG SEKIES F-Uk GJLr' ATS (DU GKA EVALUATION)

ftI UKULKf OF THlE REACTIJ4 IS: .34 THIS VALUE IS ýALCULATEA) FKUM

CIL AVEKAGE LJG F(C) V'cKSJS (I-LI

~LJb. OF eRIE-tXV'UNENTIAL FACTOR= o.544ý

AVEKiAGiE ACTIVATION ENcRGY IS: 19.'100

AVt~(ACE HEAT LIF REACTION IN: 1.04.22 STANOARD UEVtATIUN: 50zQ

SI.*Dt:VN* LUG~ IPLX STeOEY,10, AV*LUG, AFC ST.OE~V.N

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183
AFWAL-TR-81-4177
Volume I

APPENDIX B.4

PROGRAM KINETIC

SAMPLE OUTPUT PLOT

184
 AFWAL-TR-81-4177
Volume I

KINETIC SERIES FOR GULF FTS (50 QRRM EVARLURTION)

3.50- HERT RRTE=80.0(D

HEART RRTE=40.0,O
HERT RRTE=20.0 +
HERT RRTE=10.0x
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TEMPERRTURE ( DEGREES KELVIN

185
AFWAL-TR-81-41 77
Volume I

APPENDIX C.l

PROGRAM CURE

SAMPLE INPUT LISTING

186
AFWAL-TR-81-4177
Volume I

PEKCENT AFC
ZZ73 8 074E*07
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AFWAL-TR-81-4177
Volume I

APPENDIX C.2

PROGRAM CURE

SAMPLE OUTPUT

189
AFWdAL-TR-81 -4177
Volume I

WHAT TS SAMPL.E?

61.1l F ATS Rn G IA

BY WHAT FINFTIC MFTHCnh WA5 DlATA FCIIIND7

MlII-TIPI.F SCANc;/y,)q

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190
AFWAL-TR-81 -4177
Volume I

4? .31?221499P+417 A4l4! I3IE-0r-,

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AFWAL-TR-81-4177
Volume I

APPENDIX C.3

PROGRAM CURE

SAMPLE OUTPUT PLOT

192
 AFWAL-TR-81-4177
Volume I

RERCTION WINDOW PLOT

SRMPLE: GULF ATS 50 G EVAL.
MULTIPLE SCANS/DSC
E= 19.900
2.80 0.05
0.95
2.70- 0.50 -100

2.60-
S~120
0
C) 2.50.
260

C 2 140 0)
, 2.40-
U)
Lj 2.30- 160 -J

- 2.20- -180
a:
IUl -200 L
o_ 2.10- 20-
Ui -220 W
-- 2.00- _
_j -240 LUi
C:
(-- 1.90- 26
-260 :
o I--

0_ 1.80- 280 r
.. -300 o ..
ULl 1.70 -30
340
1.60- 360
380
S1.50- 400
420
0
1.40 .4
0 100
"100 101 t 1 . .100.10

LOG TIME (MINUTES)

1I93