8
MAY1943
THE CREEP CHARACTERISTICS
OF
POLYVINYLIDENE CHLORIDE
by
John F. Tormey
B. S.,
University of Notre Dame, 1941
Submitted in Partial Fulfillment of the
Requirements for the Degree of
Master of Science
at the
Massachusetts Institute of Technology
1943
Signature of Author
(Dept. Chem. Eng.-- Jafuiy T27
Signature of Professor
in Charge of Research
Signature of Chairman
of Dept. Committee on
Graduate Students
3
---
--
Graduate House, M. I. T.
Cambridge, Massachusetts
January 11, 1943
Professor G. W. Swett
Secretary to the Faculty
Massachusetts Institute of Technology
Cambridge, Massachusetts
Dear Sir:
In partial fulfillment of the requirements
for the degree, Master of Science in Chemical Engineering Practice, I am hereby presenting my thesis,
"The Creep Characteristics of Polyvinylidene Chloride".
Respectfully submitted,
John F. Tormey
258725
ACKNOWLEDGMENTS
To Dr. C. E. Reed, for assistance in
instituting this work, and to Dr. Herbert
Leaderman, for helpful suggestions during
the course of the investigation, the author
extends thanks.
TABLE OF CONTENTS
SUMMARY . . . . . . . . . .. ....
3
.....
II.
INTRODUCTION .
III.
PROCEDURE . . . . . . .
.
IV.
RESULTS .
..
V.
DISCUSSION OF RESULTS .
VI.
CONCLUSIONS
VII.
RECOMMENDATIONS .
VIII.
APPENDIX .
.......
......
A. Expanded Procedure
.
.
.
.
.
.
11
16
.
34
. . . . 40
....
41
42
......
43
B.
Summarized Original Data .
46
C.
Location of Original Dath . .
54
D.
Literature Citations
55
......
I.
SUMMARY
The time element in the stress and strain action
of natural and synthetic high molecular weight materials
has been the object of much investigation.
Because the
time element is of particular and singular significance
in these materials, attempts have been made by a study
of the relation that time has with their mechanical
action to uncover the true structure of these so-called
linear polymers.
A type of testing, wherein time is the predominant
factor, has been devised and used upon a variety of
textile materials, both natural and synthetic.
A theory
has been proposed to which these tests conform; the
object of this thesis was to employ these same tests upon
samples of oriented cordage of polyvinylidene chloride,
or Saran.
The tests consisted of stretching samples of the
cordlage under various loads for long durations of time,
releasing this load for an equal time interval,
meanwhile
making cathetometer readings of the elongations and
contractions.
Another type of test, the Superposition
Test, was also employed.
It was concluded that under the conditions established and encountered, the cordage sample of polyvinylidene chloride did not follow the established theory of
behavior.
However, there were indications that, with
some definite changes in sample size and equipment,
better correlation with theory was possible.
Recommendations covering these changes were made,
and additional testing was advocated.
II.
INTRODUCTION
In investigating the properties of most metals
for the purpose of determining their utility as materials of construction, certain established stress,
strain,
impact, and similar tests are employed by the investigator with good success in obtaining the desired information.
When these same established tests are applied to
textile fibers, either natural or synthetic, and to
certain filaments of polymeric materials, the results
are not so satisfactory, nor do they appear to tell the
complete story.
The same investigations will not suffice
to give us a clear picture of the characteristics of
these materials.
It has become increasingly evident
that time is the differentiating factor between the
action of metals and the action of textile fibers and
synthetic filaments.
It
is this time effect and its
relationship to the stress-strain action of a single
strand of synthetic "plastic", namely polymerized
vinylidene chloride, that is the subject of this thesis.
Saran
Before discussing this time effect,
some facts
about polyvinylidene chloride, or as it is called com-
mercially, "Saran", should be mentioned.
Recent patent
literature (1) states that Saran is made by polymerizing
vinylidene chloride, either alone or as a copolymer with
vinyl cyanide or vinyl chloride, adding certain filling
materials and plasticizers, fusing the mixture, dyeing
to desired color, grinding, and then extruding the
resulting thermoplastic in the desired form.
Plastic
filaments, or the oriented cordage tested in this investigation, are pulled hot from the extrusion unit and
oriented, or mechanically worked, into a wide range of
tensile strengths.
Tensile strengths can be controlled
from 4,000 pounds per square inch to 12,000 pounds per
square inch, and elastic elongation limited from ten per
cent to forty per cent (2).
Structure of Saran
This range of tensile strengths and elongations
is possible because of the unique internal structure of
Saran.
Saran has been reported, by virtue of X-ray
photographs of its structure, to possess three physical
conditions, amorphous, crystalline, and oriented, anyone
of which it may be made to assume by proper heat and
mechanical treating.
Vinylidene chloride in the unpolymerized state
is unsymmetrical dichloro-ethylene, an ethylene molecule
in which the two hydrogens on one of the carbon atoms
have been replaced by chlorine atoms.
is still present.
The unsaturation
Upon polymerization, the vinylidene
chloride molecules unite, end to end, by virtue of this
unsaturation, into long chain, linear, addition polymers
of high molecular weight (3), (4), (5).
The average
molecular weight of Saran is reported as 20,000 (2).
In the amorphous state,
it appears that these long,
linear chains exist in a haphazard,
tangled mass,
with
little or no orientation perceptible to the X-ray.
With mechanical working,
these chains may be combed out
and made to lie alongside each other, more or less parallel.
This parallel arrangement gives strength and
elasticity to the fiber by virtue of some obvious, but
not as yet recognizable, cohesive force which exists
between parallel chains.
When the molecules are so
arranged, the polymer is said to be in its orientated
state,
It
is in this state that the Saran tested in
this work existed, and it
is to the peculiar bonds,
linkages, and forces of the oriented state that Saran,
as well as the other synthetic and natural fibers, owe
their peculiar stress-strain-time relations.
The third state in which Saran is reported to
exist is the cyrstalline state, which it will assume
after heating and subsequent cooling.
This crystalline
state is peculiar to Saran, since most thermoplastics
do not display a crystalline structure.
However,
it
is
possible that the crystalline state, reported by Goggins
and Laury (2), is nothing more than a highly perfect
state of orientation and not the three dimensional
order usually associated with crystallinity.
At any
rate, the reported tendency of Saran toward perfect
orientation of its linear chains is especially noteworthy.
Commercial Properties
Saran is also highly resistant to the action of
acids,
alkalis, both weak and strong, and to most, but
not all, organic solvents (1).
It
exhibits a complete
absence of water absorption, and its rate of water
permeability is very low (2).
The other properties of
Saran, its durability, machinality, beauty, etc., not
especially important for consideration here, make it an
excellent commercial thermoplastic.
The Time Element
Whitby and Stafford (6)
in their work on the
elasticity of rubber were forded to conclude:
"Time plays an important part in the result
of any mechanical manipulation through which
these materials (rubber, organic polymers,
etc.) pass. Strictly speaking, there is no
such thing as a stress-strain diagram in
these cases, only a stress-strain-time
diagram".
They substantiate this view with time data for rubber
elongation.
The same view is also expressed1 by
Kuveshinky and Kobeko (7) and by Alexandrov (8), all of
whom report considerable work in this field.
The
former reports relationship between elasticity and
dielectric orientation, while the latter discusses the
wrelaxation" time in synthetic polymeric materials.
Leaderman (9) has conducted extensive stress-strain
time experiments on rayon, nylon, silk, and similar
textiles and has established a type of experiment,
namely the creep test of long duration, creep recovery,
and cyclical loading, to which Saran has been subjected
in this investigation.
Creep and Creep Recovery
When a fiber, or an oriented cordage of Saran,
is subjected to a constant tensile load, the material
rapidly elongates upon the applicaton of the load.
This instantaneous deflection is followed by a slower
deflection or "creep", which may continue for some
hours.
Upon removal of the load,
the material instantly
contracts to an extent closely approximating its initial
elongation.
Following this instantaneous contraction,
there ensues a gradual contraction which may result in
the materials'
attaining once more its original length.
This phenomena is called "creep recovery".
One might
speak of the instantaneous elongation and contraction
as elasticity and the creep and creep-recovery action
as delayed elasticity.
However, the term elasticity connotes complete
recovery.
In some cases of creep, the creep recovery
is not perfectly complete,
but there remains a small
non-recoverable portion, or permanent set.
Leaderman
has divided creep, therefore, into two components,
which are superimposed on each other; primary creep,
or creep to which there is complete recovery, and
secondary creep, or creep to which there is no recovery.
Inasmuch as primary creep alone is of present interest,
it seems advisable to eliminate if possible this
secondary creep.
This is accomplished by "mechanical
working" or subjecting the material to certain loads
for definite time intervals until the secondary creep
component is no longer
present.
Superposition Principle
With the ideas of creep and creep recovery is
closely related the Superposition Principle, simply
expressed by Leaderman (10) as follows:
"At any instant, the deflection of a solid
manifesting only primary creep can be separated into two components. One component
is the instantaneous elastic deflection,
proportional to the load acting at that
instant. The other component is the primary creep or delayed elastic deflection
dependent not only on the load acting at
that instant but also on the entire previous
loading history. Hence, as far as the
primary creep component of the deflection
is concerned, the material possesses a
memory of all past loading actions".
This Superposition Principle has been demonstrated
by Leaderman to hold well for single filaments of viscose nylon, and silk, and these tests on Saran wer6
conducted with the same purpose in mind, namely, to
determine whether or not Saran obeyed the Superposition
Principle.
To apply the Superposition Principle,
a creep
test under constant load, lasting for several hours,
is performed, followed by a creep recovery test of the
same duration.
versus time.
These results are plotted, elongation
The material is now subjected to a diver-
sified loading.
That is,
using the same load as was
employed in the long duration test, the experimenter
applies and removes the load at various times.
If
the Superposition Principle holds for the material, and
the memory effect is present, we may calculate and
reconstruct, from the elongations present in this latter
test, a curve et~ctly similar to the former long-duration
creep curve.
This is possible,
as Leaderman (10)
expresses it, if:
"We assume the effect of the original
load, as far as its creep is concerned,
Superimposed
to continue indefinitely.
upon this, we assume a (negative) creep
due to an equal negative load applied at
the instant of load removal...........
The effect of each load, positive or
negative, is assumed to continue indefinitely, and the deflection at any
time is simply the sum of the deflections
due to each separate loading action. Each
of these separate effects can be obtained
from the long-duration creep test".
The Superposition Principle can also be tested
by an examination of the long-duration creep and creerecovery tests.
By allowing the creep to attain its
limiting value and then removing the load, a negative
deflection will ensue, whose plot, on appropriate axes,
should reproduce the creep curve exactly.
Consequently, long-duration creep curves are
the key tool to the investigation of these creep phenomena which display themselves in such a variety of
materials.
When it has been conclusively proved that
the principles of creep and Superposition are perfectly
consistent, reproduceable, and present in otherwise
related materials, a new means will have been obtained
by which the ultimate structure of linear polymers, now
deduced only by X-ray and chemical analysis, may be
uncovered.
III.
PROCEDURE
Creep Test
The sample or oriented Saran cordage was fastened at one end to a firmly mounted bracket.
This
fastening was accomplished by clamping the cordage
between two leather-covered steel bars and screwing the
bars to a wooden base.
Details of this arrangement are
to be found in Figure II.
The oordage, .021 inch in diameter and approximately 70 centimeters in length, was allowed to hang
vertically, its other extremity being attached to a
light bronze hollow column, which was free to move
vertically but whose sidewise motion was prevented by
a double pair of rollers, which guided but did not impede the vertical motion of the column.
is sketched in Figure III.
This mechanism
By such a system of fasten-
ing, the cordage of Saran was held in the vertical plane
at all times.
Predetermined loads were applied to the
cordage by quickly and manually hooking metal weights
to a fastener at the bottom of the bronze column.
Cathetometer readings of the elongation were made at
definite intervals over the course of twenty-four hours.
Temperature readings were also noted.
The resulting
12
elongations of the Saran were plotted against the
logarithm of the time in minutes.
Creep Recovery
This test is nearly identical with the creep
test.
After a period of twenty-four hours of inducing
creep in the Saran cordage, the load was quickly removed and cathetometer readings of the contration or
recovery were made at the same time intervals as the
creep test.
These results were also plotted against
a long time abscissa, on the same graph as the creep
curve.
Cyclical Loading
In this test, a definite load was applied to the
cordage and allowed to remain for ten minutes.
then removed and the Saran allowed to contract.
It was
After
a contraction or creep recovery period of ten minutes,
the load was once more applied.
This process of load-
ing and unloading continued for sixty minutes.
Cathe-
tometer readings of the deflection were made every minute.
13
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IV.
RESULTS
The results of this investigation, comprising
creep, recovery, and superposition tests, are presented
graphically in this section.
Semi-log plots of all the creep and recovery tests
are arranged in the order in which they were performed.
In presenting these results in graphical form, it is
believed a better evaluation is possible than with tabulated data.
However,
a portion of the original data, as
it was recorded in tabular form, is to be found in the
Appendix.
Superposition points are plotted on the same
graph.as the creep curve obtained from the corresponding
srecimen and load.
Creep and recovery curves for Specimen A are
plotted on Figures IV and V.
Creep and recovery curves for Specimen B are
plotted on Figures VI, VII, VIII,
IX, X, XI, XII, XIII,
and XIV.
Creep and recovery curves for Specimen C are
plotted on Figures XV, XVI, XVII, XVIII, XIX, and XX.
Superposition tests for Specimen B are found on
Figures XIII, and XIV.
Superposition tests for Specimen C are found on
Figures XVIII, and XIX.
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V. DISCUSSION OF RESULTS
With the aim of obtaining smooth, reproducable
curves of the elongation-versus-time relationship for
Saran, this thesis was undertaken.
But, after a critical
survey of the preceding results,
is fairly obvious
it
that this particular aim has not been attained.
Several
factors were present which considerably influenced the
varied course of the results, and so serious were these
factors that no favorable conclusions as to the status
of polyvinylidene chloride in the Superposition Theory
can be hazarded.
However, certain quite definite points
may be derived from these results which may be of assistance in further work on this material.
Before discussing these conclusions, a more direct
consideration of the curves is
in order.
Specimen A
These two curves, Figures IV and V, are typical of
the action of the other two specimens, which is as it
should be if we assume the material to be of consistent
composition and structure.
The first curve shows con-
siderable permanent set, nearly half of the original
elongation, while the second curve displays only a smal;
amount of set.
Mechanioal working, or the physical pull-
ing and stretching of the cordage into tighter, more compact molecular chain bundles,
is evident.
The creep and recovery curves for this specimen
are too curved, too divergent, and too separated for any
feasible application of the Superposition Rule.
Specimen B
Figures VI,
VII,
IX, X, and XI of this group are
of little positive value in applying the principles of
creep and superposition to Saran.
In these five plots,
the points are so scattered above and below the mean line
that some factor is apparently disturbing the harmonious
elongation of th6 cordage sample.
Possible reasons for
this disturbing element will be discussed in another part
of this section.
Moreover, Figures IX and X display marked curvature,
indicating that the applied load is too light to enable the
material to display its creep qualities.
versus log time is,
concerned,
The plot of creep
so far as present investigators are
a straight line.
Figure XI, displaying a crossing of the creep and
the recovery curves, ranges so far from theoretical considerations as to be also eliminated.
In studying Figures VIII, XII, XIII, and XIV, however, some adherence to theory is noted.
The curves of
creep and recovery are parallel and reasonable close,
showing that the material is similarly responsible to
positive and negative loads, and that, with better equipment, even more similar curves might be obtained for
Saran.
Figure XIII is very good in this respect, though
the individual points are scattered to a slight extent.
Specimen C
In this group of graphs, Figure XVI is noteworthy
in that the points, for both creep and creep recovery
lie on straight, parallel lines.
The considerable load
of this test, 1100 grams, may have been of such magnitude
as to cancel those mechanical or frictional errors that
could provide scattered points.
This curve best exemplies
the Superposition Principle in Saran; and as such, shows
that the material may possibly provide some basis for
application of the superposition rules.
Figure XVIII
is also theoretically sound.
On the unfavcrable side are Figures XV, XVII, XIX,
and XX.
Here again, scattered points, diverging lines,
curved lines, and permanent set serve to make these plots
useless as far as application of the theory is concerned.
Superposition Tests
According to the data of Leaderman (10), the
superposition test points should fall nearly upon the
creep curve of long duration, if the principles of
superposition are to be upheld.
Inspection of Figures
XIII, XIV, XVIII, and XIX shows that this is not the
case for Saran.
At least, it
employed in these tests.
is not under the conditions
However, there is not reason
to conclude that superposition does not apply to the
material, polyvinylidene chloride, merely because it
is not here apparent.
Further testing under other con-
ditions of time, temperature, and strain may revetl
close harmony with the theory.
graphs,
As indicated in the
the superposition points form a family of united
and ascending convex curves and not the straight creep
curve of theory.
The regularity of this family indicates
that the failure to follow theory here is due, not to a
mechanical flaw, but to a more serious, unaccountable
property of the polymer itself.
Probably Sources of Error - General
The curved lines, the large permanent set, the
poor superposition correlation - all these indicate that
the range of loads used was not adequate to bring out
the desired properties in Saran.
loads,
The fact that at low
the curve was concave upward with a straightening
out of this curve upon an increase in load, would indicate
38
that higher loads .should be wed in -testing Saran.
Moreover, more extensive mechanical conditioning is
advisable to remove all the permanent set.
It is quite possible that the large diameter,
0,021 inch, of the specimens tested was also a factor
in producing this non-correlation of practice and theory.
Filaments of Saran, with less of a tendency for "Packing"
upon elongation, seem to offer a feasible alternative.
To establish a working range for further creep
tests, a series of stress and strain tests should be
performed on Saran.
These may then be consulted in
order to deduce that range of loads wherein the creep
properties of Saran may be viewed, free from elastic
effects.
Sources of Error-
Experimental
Two important sources of experimental error were
encounteredin the tests.
These were the frictional
resistance of the guide rollers and the error in setting
and reading the cathetometer.
The former error may be detected in those curves
in which the points are scattered.
typical example.
Figure IX is a
The points ascend in a series of
steps, rather than as a smooth curve.
Frictional
A9
resistance in the rollers, preventing differential
increases in length with differential "relaxation"
within the Saran, but allowing elongations only when
a certain force had been gathered, would produce this
step wise curve.
Only finer, more precise equipment,
or equipment of entirely different operation, will
eliminate this error.
Although readings precise to 0.005 centimeter
were possible with the cathetometer employed in this
thesis, accuracy corresponding to this precision was
not borne out in the readings.
Difficulty in setting
and sighting the cathetometer in the short space of time
between readings could not be overcome, as is evident,
in some of the data.
Timing error was negligible.
4O
VI.
CONCLUSIONS
1. Under the conditions employed and encountered in
this experimental work, oriented cordage of polyvinylidene
chloride,
or Saran, does not follow the theory of
Superposition.
2.
There are some indications that, under different
operating conditions,
a more favorable approach to the
theory can be attained.
7~.i
VII.
RECOMMENMATIONS
1. Standard stress-strain tests should be made on Saran
before any further creep or Superposition work is
attempted.
2. Heavier loads and finer cords of Saran are indicated
by the data to provide better harmony with theory.
These should be used.
3. If the roller type of attachment is used, it is
recommended that some mechanical changes be made
to minimte the frictional resistance.
4. With proper cognizance of the above points, additional
creep tests on polyvinylidene chloride are recommended.
42
PY1.
APPENDIX
18
A.
EXPANDED PROCEDURE
Material Tested
The Saran samples used in these t6sts were all
cut from the same continuous length of material.
Con-
sequently, discrepancies in theory due to compositional,
extrusion, or mechanical working differences should be
negligible.
The material was oriented Saran cordage, with an
average diameter of 0.021 inch, and a reported breakirg
load of 40,000 pounds per square inch (2).
The exact
composition of this particular Saran sample was not
available, nor was equipment available for preliminary
stress-strain tests to be conducted on the Saran.
Pretreatment and Mechanical Conditionin
The lengths to be tested were cut to approximately
70 centimeters and hung in the laboratory for from three
to six days-in order that they might attain an equilibrium with the temperature and humidity of the laboratory.
Previous to the actual testing, the cordage was
allowed to hang in the testing apparatus for twenty-four
hours, being stressed only by the weight of the bronze
column, amounting to 120.5 grams.
Moreover, the samples
were mechanically treated by subjecting them to loads
equal to or in excess of the testing loads to be used
later.
This mechanical treatment lasted from sixteen
to twenty-four hours with an equal time being allowed
for recovery.
Creep Apparatus
This has been previously mentioned in the Procedure.
Figures I, II, and III illustrate the details
of construction.
The apparatus was solidly fasteed
to a concrete pillar for complete stability.
Cathetometer
The cathetometer employed was of the standard
laboratory type with telescope and vernier scale.
The
telescope was focussed on a finely etched cross-marking
on the side of the bronze column, and this marking was
kept in view throughout the elongations and recoveries
of the attached cordage by sliding the telescope vertically along the cathetometer scale.
Positional read-
ings were taken from the vernier scale.
Tim ing
On the creep and recovery tests, cathetometer
readings were made at 1, 2, 3, 5, 7, 10, 15, 20,
30, 40,
60, and 90 minutes, and at convenient, though not necessarily fixed, times thereafter.
During. the cyclical
loading tests, readings were made with the cathetometer
every sixty seconds.
Elapsed time as indicated by a
45
clock that announced each minute with a distinctive and
audible note.
Temperature
The temperature of the surroundings immediately
adjacent to the apparatus did not go below 2400C nor
above 2700C during the course of the experiments.
In
any one particular creep test, the temperature variance
was never more than 10C.
Temperature was obtained by a mercury-in-glass
thermometer, and recorded regularly.
Humidity
Since Saran has shown a water absorption of 0.00%
over a period of twenty-four hours, the factor of humidity did not seem to be an important one.
However, the
tests were performed in a dim, artificially ventilated
and conditioned room, and it is believed a relatively
constant humidity was present.
'U,
~1
TABLE I
CREEP AND RECOVERY - SPECIMEN A - TEST III
Load - 703.1 grams
Time in Minutes
0
1
2
3
4
5
10
15
20
30
60
90
1530
Scale Position
5.460
3.895
3.850
3.770
3.730
3.670
3.665
3.625
3.595
3.575
3.490
3.405
3.025
Creep in Centimeters
0.000
1.565
1.610
1.690
1.730
1.790
1.795
1.835
1.860
1.880
1.965
2.050
2.435
Creep Recovery
Time in Minutes
Scale Position
0
3.025
0.000
1
4.555
1.530
2
4.650
1.625
3
4
5
4.680
4.720
4.725
1.655
1.695
1.700
4.805.
1.780
15
4.850
1.825
20
4.875
1.850
30
4.900
1.875
60
90
1260
1440
1530
5.020
5.040
5.270
5.300
5.300
1.995
2.015
2.245
2.275
2.275
10
TABLE II
CREEP AND RECOTERY
- SPECIMEN B - TEST VIII
Load - 858. 7 grams
Time in Minutes
0
1
2
5
5
7
10
15
20
30
40
60
90
1260
1380
Scale Position Creep in Centimeters
5.520
3.445
3.370
3.335
3.265
3.425
3.170
3.130
3.125
3.065
3.055
2.970
2.945
2.520
2.520
Scale Position
Time
0.000
2.075
2.150
2.185
2.255
2.275
2.350
2.390
2.390
2.450
2.460
2.545
2.570
3.000
3.000
Creep Recovery
0
2.520
0.000
1
2
4.500
1.980
4.580
4.625
4.710
4.715
2.040
2.105
2.190
2.195
4.785
4.795
4.995
5.350
5.350
2.260
2.270
2.470
2.830
2.830
3
5
7
10
15
100
2700
2880
48
TABLE III
CREEP AND RECOVERY - SPECIMEN B - TEST VIII
Load - 784.6 grams
Time in Minutes
Scale Position
Creep in Centimeters
0
1
2
3
5
7
10
15
20
25
40
60
90
420
1260
1440
4.550
2.585
2.525
2.495
2.430
2.400
2.365
2.310
2.270
2.270
2.185
2.160
0.000
1.965
2.025
2.055
2.120
2.150
2.185
2.240
2.280
2.280
2.365
2.390
2.460
2.570
2.715
2.760
T ime
1.090
1.980
1.835
1.790
Scale Position
0
1
2
3
5
7
10
15
20
30
40
60
90
360
1340
1530
1.790
3.695
3.770
3.800
3.880
3.940
4.000
4.000
4.040
4.085
4.150
4.185
4.295
4.405
4.525
4.535
Creep Recovery
0.000
1.905
1.980
2.010
2.090
2.150
2.210
2.210
2.250
2.295
2.360
2.395
2.505
2.615
2.735
2.745
TABLE IV
CREEP AND RECOVERY
-
SPECIMEN C - TEST II
Load - 1102.7 grams
Time in Minutes
0
1
2
3
5
7
10
15
20
30
40
60
90
400
1290
1450
Time in Mi nutes
0
1
2
3
5
7
10
15
20
30
40
60
90
1340
Scale Position
5.055
2.295
2.195
2.140
2.075
2.020
1.985
1.895
1.890
1.825
1.800
1.730
1.645
1.320
1.000
0.990
Soale Position
0.990
3.495
3.590
3.635
3.745
3.785
3.815
3.900
3.915
3.995
4.025
4.040
4.175
4.540
Creep in Centimeters
0.000
2.760
2.860
2.915
2.980
3.035
3.070
3.160
3.165
3.230
3.255
3.325
3.410
3.735
4.055
4.065
Recovery
0.000
2.505
2.600
2.645
2.755
2.795
2.825
2.910
2.920
3.005
3.035
3.050
3.185
3.550
TABLE V
CYCLICAL LOADING FOR SUPERPOSITION TEST
Specimen B - Load 784.6
Time in Minutes
0
Scale Reading
4.525
Calculated Creep
0.000
1
2
3
2.695
2.610
2.600
1.830
1.915
1.925
4
2.580
1.945
5
6
7
2.525
2.520
2.515
2.010
2.015
2.020
2.510
2.025
2.460
2.075
-
--
4.295
4.370
4.390
2.060
2.135
2.255
14
15
16
4.400
4.410
4.420
2.265
2.275
2.285
17
4.420
2.285
4.420
4.455
2.285
2.320
--
--
21
2.575
2.180
22
23
24
25
26
27
28
29
2.495
2.485
2.485
2.475
2.470
2.470
2.470
2.465
2.260
2.270
2.270
2.280
2.285
2.285
2.285
2.290
--
--
4.270
4.295
4.340
4.345
4.350
4.390
4.395
4.405
4.410
2.205
2.230
2.275
2.280
2.285
2.320
2.325
2.335
2.340
--
--
8
9
removed
11
12
13
18
19
applied
removed
31
32
33
34
35
36
37
38
39
applied
TABLE V
CYCLICAL LOADING FOR SUPERPOSITION TEST
T'ime in Minutes
Scale Reading
Calculated Creep
41
2.540
2.240
42
43
44
45
46
47
48
49
2.520
2.460
2.460
2.440
2.440
2.435
2.435
2.420
2.260
2.320
2.320
2.340
2.340
2.345
2.345
2.360
removed
51
52
53
54
55
56
57
58
59
60
--
--
4.265
4.300
4.330
4.340
4.340
4.360
4.360
4.360
4.380
4.380
2.245
2.280
2.310
2.320
2.320
2.340
2.340
2.340
2.380
2.380
TABLE VI
CYCLICAL LOAPING FOR SUPERPOSITION TEST
Specimen C - Load 703.1 grams
Time in Minutes
Scale Reading
0
4.280
3
2.485
1.795
4
5
6
7
2.460
2.440
2.420
2.380
1.860
8
2.380
9
2.375
1.905
11
12
13
14
4.070
4.115
4.160
4.160
1.945
1.990
15
4.170
16
17
4.170
4.170
2.045
2.045
18
19
4.175
4.175
2.050
2.050
1
2
removed
applied
2.545
2.500
--
2.490
2.440
23
24
25
28
27
28
29
2.435
2.380
2.375
2.375
2.370
2.370
2.340
1.820
1.840
1.900
1.900
2.035
2.035
2.045
2.000
2.050
2.055
2.110
2.115
2.115
2.120
2.120
2.150
--
31
4.035
32
33
4.080
4.090
34
35
36
4.090
4.125
4.125
37
4.125
38
4.145
39
applied
1.780
--
21
22
removed
Calculated Creep
0.000
1.735
4.145
--
2.035
2.080
2.090
2.090
2.125
2.125
2.125
2.145
2.145
-, •-
TABLE VI
CYCLICAL LOADING FOR SUPERPOSITION TEST
Time in Minutes
41
42
43
Scale Reading
2.44U
2.385
2.370
44
2.370
45
46
2.365
2.310
47
2.310
48
49
2.310
2.300
removed
51
52
53
54
55
56
57
58
59
60
4.015
4.060
4.060
4.070
4.150
4.150
4.150
4.160
4.160
4.160
Calculated Creep
.0b85
2.145
2.160
2.160
2.165
2.220
2.220
2.220
2.230
2.105
2.150
2.150
2.160
2.240
2.240
2.240
2.250
2.250
2.250
54
C. LOCATION OF ORIGINAL DATA
The original data from which the results of
this thesis have been obtained are in the possession
of the author.
Part B of this appendix presents some, but not
all, of the data recorded during the experimental
work.
55
D. LITERATURE CITATIONS
(1)
2,235,782,
U.S. Patents; 2,232,933,
2,235,782,
2,249,915,
2,235,796,
2,249,916,
2,237,315,
2,249,917,
2,238,020,
2,251,486.
(2) Goggin, W.C. and Laury, R.0. ; paper presented at
the 102nd meeting of the American Chemical Society,
Atlantic City, N. J., Sept. 1941.
(3) Lewis, W. K., Broughton, G., and Squires, L.;
"Industrial Chemistry of Amorphous and Colloidal
Materials", lst ed., MacMillan (1942).
(4) Burk, Thompson, Weith, and Williams; "Polymerization",
Rheinhold (1937).
(5) Mark, H. and Whitby, G. S.; "Collected Papers of
Wallace H. Carrothers on Polymerization",
New York (1940).
(6) Whitby, G. S. and Stafford, G.; Trans.
Rubber Ind. 6, 40 (1930).
(7) Kobeko, P. and Kuvshinsky,
U.S.S.R. 5, 401 (1938).
(8) Alexandrov, A.; Tech. Phys.
929 (1937).
E.; Tech.
Inst.
Phys.
U.S.S.R. 4,
(9) Leaderman, H.; "Elastic and Creep Properties of
Filamentous Materials", Sc.D. Thesis, Mech.
Eng., M.I.T. (1941).
(10) Leaderman,
H.; Text,
Research 10, 171 (1941).