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**Viscoelastic Behaviour & Polyethylene
**

Terephthalate

P. R. PINNOCK and I. M. WARD*

**Dynamic mechanical measurements of unoriented crystalline polyethylene
**

terephthalate fibres have been made over the temperature range of the glass/

rubber transition. The results have been conlpared with previously reported

creep data. A consistent representation of both sets of data can be obtained

using first-order approximation methods and defining the transition tenlperature

as that for which t a n 8 is a maximum.

**DYNAMIC mechanical measurements on polyethylene terephthalate fibres
**

of different physical structure have been reported in a previous publication 1

which was primarily concerned with the anisotropy of elastic and visco-

elastic behaviour in oriented fibres. The present paper deals particularly

with the frequency/temperature relationships for these fibres, and the

earlier work has been extended in several ways. First, the dynamic

mechanical measurements have been extended to lower frequencies by

construction of an apparatus with a working range of 10 -:~ to 10 c/s.

Secondly, the dynamic measurements are compared with extensional creep

data obtained elsewhere 2 and previously reported dielectric loss :~ and

dilatometric measurementsL

The previous dynamic mechanical measurements 1 were restricted to a

narrow range of frequencies, and it was found adequate to describe the

frequency/temperature behaviour as that of a constant activation energy

system. The extensional creep data 2 for unoriented crystalline fibres, on

the other hand, showed shift factors which could be fitted to the Williams-

Landell-Ferry relationshipL It also appeared that the dielectric loss and

dilatometric measurements were consistent with this representation. It is,

ihowever, not easy to distinguish between the W L F representation and a

constant activation energy over a narrow range of frequencies, particularly

at high frequencies. It is therefore of interest to examine dynamic

mechanical measurements over a wide range of frequencies for crystalline

unoriented fibres, together with the creep data, to see if a consistent

representation of both can be obtained.

EXPERIMENTAL

Preparation of samples

The fibres were made by the conventional melt-spinning process in

which molten polymer is extruded through small orifices to produce non-

crystalline fibres with a very low degree of molecular orientation. These

fibres were then subjected to a heat-crystallization process. The latter

*Present address: H. H. Wills Physics Laboratory, University of Bristol,

255

P. R. PINNOCK and I. M. WARD

**process is necessary to stabilize the samples before subjecting them to
**

the range of temperatures encountered during the dynamic mechanical

testing.

**Physical characterization of samples
**

A detailed investigation of the molecular structure of the samples was

not undertaken. However, it was of value to obtain empirical measures

of crystallinity and molecular orientation, recognizing the arbitrary nature

of these types of measurement.

The measure of crystallinity was an X-ray diffraction method devised

by Farrow and Preston 6, which compares the integrated intensity of the

sharp X-ray reflections from crystalline material with the integrated intensity

of the diffuse reflections from the non-crystalline material.

A measure of the overall molecular orientation was obtained from the

optical birefringence. This is the difference between the refractive indices

of the fibres, along and at right angles to the fibre axis, and was measured

using polarized light and a Berek compensator.

**Measurement of dynamic extensional modulus (Young's modulus)
**

The apparatus used in the measurement of extensional modulus is shown

diagrammatically in Figure 1. It is identical in principle to that described

in a previous publication I but possesses a wider frequency range (10 -3 to

Strain J Carrier

gauge I

t

Phase I Phase

Fibre [ sensitive sensitive

sample rectifier rectifier

Sine Cosine

t t

Integrator Integrator

~nchro

hi ~ etement

t f

In phase Ouadrature

L . . .

• Scotch-yoke

. . . . . J

E' Ert

mechanism Outputdisplay

Figure/--Schematic diagram of the dynamic mechanical apparatus

**10 c/s). It was also found to produce results with greater accuracy and
**

reproducibility than had proved possible using the earlier apparatus.

The sample is subjected to a sinusoidal strain of fixed amplitude, which

256

VISCOELASTIC BEHAVIOUR IN POLYETHYLENE TEREPHTHALATE

**is provided by a Scotch-yoke mechanism driven by a servo-controlled
**

motor. The stress is measured by a non-bonded strain gauge transducer

attached to the other end of the sample. Simultaneous comparison of stress

and strain is made electronically using a Servomex Transfer Function

Analyser (TFA).

The T F A provides a servo-controlled motor which, in addition to

providing a means for a sinusoidal strain, rotates a loop in a high frequency

(to~) alternating magnetic field (2kc/s). Since the loop rotates at a very

low frequency (to,D, i.e. the test frequency, this produces a carrier modu-

lated at the rotational speed of the form

K sin to,,,t cos to,,t for w, >~ w,,,

which can then be fed to the system under test. However, in our application

the mechanical signal is used and consequently the return signal presented

to the measuring system by the transducer will be of the form

K1 sin (to,,t+3)+N

where 3 is the angular phase shift produced by the system under test and

N represents unwanted elements such as harmonics, random noise, etc.

At this stage a carrier is introduced and the signal is then multiplied

simultaneously but separately by sin to,,t and cos w,,y. This multiplication

at the modulation frequency, to .... is carried out by a synchro element with

resolver type windings. This element is directly coupled to the same motor

shaft which drives the Scotch-yoke and the rotor winding is fed with the

signal from the transducer plus carrier. The two stator windings are at

90 ° to each other and from these are derived the sine and cosine functions.

These two signals after being demodulated to remove the carrier

frequency component are of the form

**Ks sin (to,d+ 3) sin to,~t+N sin ¢0,,,t
**

= ½K2 [cos 3 - cos (2tomt + 3)] + N sin to,,y

and K2 sin (to,,,t + 3) cos to,~t + N cos to~,t

= ½K2 [sin 3 + sin (2to,,,t + 3)] + N cos to,d

These signals are then integrated over a complete cycle to remove all

unwanted terms. Two steady signals are then obtained which are propor-

tional in magnitude and polarity to the real and imaginary parts of the

system output at the fundamental frequency, i.e.

I/m m 1 ,,, m

f ~K2cos 3 a t and

0

j'½K~sin3dt

0

**It is essential that the Scotch-yoke mechanism be as free from noise as
**

possible and this was largely achieved by making the eccentric collar of

Nylon which, in turn, rotates in contact with polished stainless-steel

surfaces. Provision was also made for aligning the eccentric Nylon collar

with respect to the loop thereby avoiding any constant additional phase

difference between the loop and the strain.

As in the previous apparatus a sinusoidal strain of + 0 . 2 5 m m , i.e.

257

P. R. P I N N O C K and I. M. W A R D

**,+ 0.25 per cent on the 10 cm sample, was chosen, having already established
**

that this is within the range of the linear viscoelastic behaviour. The sample

was also subjected to a static strain of approximately 0.25 mm to prevent

it going slack. The fibre is connected to both the Scotch-yoke mechanism

and to the strain gauge by German-silver tubing connections.

The fibre is surrounded by an annular copper can through which heated

air may be passed. The copper can in turn is insulated by a Thermos

jacket enabling the temperature of the fibre to be controlled to within

1 deg. C.

Creep measurements

The creep data discussed in this paper were all obtained in a previous

investigation which has been reported fully elsewhere 2. The creep measure-

ments were confined to unoriented monofilaments which had been heat-

crystallized by heating at 180°C for one hour. These samples were therefore

exactly equivalent to the unoriented crystalline fibres used for the dynamic

mechanical measurements.

The reader is referred to the previous publication for details, but to

summarize, the creep compliance of unoriented crystalline polyethylene

terephthalate was measured in the linear viscoelastic range from 65 to

115"5°C, isothermal creep data being obtained at nine fixed temperatures,

THEORY

Linear viscoelastic behaviour

There are several equivalent ways of determining the mechanical

behaviour of a linear viscoelastic system. These are broadly of two types,

the first being the response of the system to transient stress or strain, and

the second its response to dynamic stress or strain. The results of transient

measurements define a relaxation modulus or a creep compliance and the

dynamic measurements define a complex modulus or compliance.

A convenient starting point for consideration of the transient type

measurements is the Boltzmann superposition principle. For uniaxial creep,

this relates the final strain e (t) to the elemental increments of stress do-(~-)

applied at times ~-.

Thus

t

e (t) = ~-0 + J (t - r) dr

**where J (t) is the creep compliance, and similarly for stress relaxation
**

t

**where E (t) is the stress relaxation modulus, E0 is the instantaneous elastic
**

modulus and de (r) are the elemental strain increments.

From the dynamic mechanical approach, consider the system to be

subjected to a sinusoidal stress

o- = o'0 sin tot

258

VISCOELASTIC B E H A V I O U R I N P O L Y E T H Y L E N E T E R E P H T H A L A T E

**Then the sinusoidal strain produced will be given by e=e~ sin (cot-6)
**

where 6 defines the phase lag between stress and strain. The ratio between

strain and stress e/o- defines the complex compliance J * = J ' + i J ' . Alter-

natively, we may define the complex modulus E * = E ' + iE', from the

reciprocal ratio of stress to strain.

The mathematical relationships between the creep compliance, the

stress-relaxation modulus and the dynamic compliance and modulus, have

been discussed in detail by Gross 7 and others. These relationships are

complex and involve, for example, recourse to the methods of Fourier or

Laplace transforms to relate transient to dynamic quantities. Although it

is possible to compute exactly one quantity from another, provided that

a sufficient time-scale is covered, this is rarely profitable for considerations

of the viscoelastic behaviour of polymers. In the first place, the visco-

elastic behaviour can rarely be determined experimentally with sufficient

accuracy, and secondly the behaviour normally changes fairly slowly with

change in frequency. It is therefore often adequate to resort to approximate

methods, and these will be discussed in the next section.

**Use of approximate methods
**

The relaxation modulus can also be expressed as

oo

E (t)=Eo+ ( H (z)e-' ~d l n z (1)

**where H (T) is a function defining the relaxation spectrum (see, for example,
**

ref. 8, p 41).

A similar generalization for creep gives the creep compliance in terms

of a 'retardation-time' spectrum, L (z).

Y (t)=/0+ t" L (T) (1 - e-','O d In T

**where J0 is the instantaneous elastic compliance.
**

The real and imaginary parts of the dynamic modulus can also be

expressed in terms of H (7-).

E' (w)= E0 + . ~--ro-~ J d In ~- (2)

--:xz

and

oo

E" (09)=

H (r) (or ] (3)

$-~r# j d In r

--0o

**The approximations to be used in this paper all derive from approximate
**

methods to obtain H (T).

Equation (1), which has the form of a Laplace transform, can be used

t o evaluate H (z) to various orders of approximation, as has been extensively

discussed in the literature (see, for example, ref. 8, p 44).

259

P. R. PINNOCK and I. M. WARD

**The first-order approximation was proposed by Alfrey and is generally
**

known as the Alfrey approximation.

It gives

n (~')=[-dE (t)/d ln t]t=~

and can be considered to arise by approximating the intensity function

e-t/~ which goes from 0 at ~-=0 to 1 at ~- > ~ by a step function going

from 0 to 1 at r = t.

Second-order and higher-order approximations can be obtained involving

the first derivative and higher derivatives of E (t) with respect to Int.

As discussed in detail by Staverman and SchwarzP and others the first-

order Alfrey approximations hold provided that the relaxation spectrum

or retardation spectrum do not change very rapidly with frequency. In

mathematical terms this requires that the second- and higher-order

derivatives should be small compared with the first-order derivative.

The analysis of the creep and dynamic data presented here suggests that

first-order approximations are adequate. Furthermore this will be shown

to be expected from examination of the creep data alone.

Thus we shall assume that the relaxation spectrum is given by

H (r) = [ - dE (t)/d In t]t ,.

To a similar degree of approximation equations (2) and (3) can be shown

to give

[dE' (~0) ] 2 [E" (co)]1/..... (4)

**From the latter approximations it follows that
**

d In E' (w)/d In co= ( 2 / 7 0 tan 8 (5)

In a similar manner it can be shown that

d In J' (oJ)/d In w = (2/7r) tan 8 (6)

It is also noted that E(t)=E'(o)) and J(t)=J'(o)) for o)=l/t.

**Frequency/temperature equivalence and the definition of 'transition
**

temperatures'

The discussion has so far only been concerned with the variation of

mechanical properties with time or frequency at a fixed temperature. This

paper is, however, primarily concerned with the temperature dependence

of the viscoelastic behaviour. With transient measurements, it is fairly

straightforward to obtain the frequency/temperature dependence by

comparison of data obtained at different fixed temperatures. The procedure

is to obtain a 'master creep curve' or a 'master stress-relaxation curve' by

superposition of the isothermal data. The linear frequency shifts corres-

ponding to shifts in temperature are thus obtained directly.

It is, however, not so obvious how to obtain shift factors directly from

the dynamic mechanical data, obtained at constant frequency over a range

of temperatures, because each set of data for the real and imaginary parts

260

VISCOELASTIC BEHAVIOUR 1N POLYETHYLENE TEREPHTHALATE

**of the modulus or compliance does not in itself define a particular tem-
**

perature. Strictly, the measurements of E' and E " at constant frequency

over a range of temperatures should be used to construct plots of E ' and

E " at constant temperature for a series of frequencies. These plots can

then be superimposed to obtain the shift factors. A similar procedure.

of course, can be applied to measurements of J' and J" at constant

frequency, with an identical result.

A somewhat simpler procedure has been used in this paper, which will

be shown to be adequate. It is based on the following considerations.

The previous dynamic mechanical measurements ~ showed that to a

first approximation change in temperature produced a uniform shift on a

logarithmic time scale. However, the creep data show that this is not

strictly true over a wide time scale, since the so-called W L F equation

gives a better fit to the shift factors than one with a constant activation

energy. However, the difference between these two representations is not

large for a restricted time scale.

It follows from equation (4) that a peak in the relaxation spectrum

(which will correspond to a 'transition') occurs when dE' (6o)/d In ~o and

E"Io~) have a m a x i m u m value. In a system with a constant activation

energy A then time is related to temperature 0 by the equation

r ( 0 ) = r (0) exp CA/RO)

Hence for measurements at constant frequency a passible definition of

the transition temperature is the temperature at which dE'(O)/dO and

E " ( 0 ) have a m a x i m u m value. For reasons of experimental convenience,

this definition was adopted in one of our previous publicationd and used

to define transition temperatures for extensional and torsional viscoelastic

behaviour. Similarly an alternative definition can be the temperature when

d J ' (0)/d0 and J'" C0) have a maximum value. A further definition, following

from equation (5) and (6), is that the transition temperature is the tempera-

ture for a m a x i m u m value of tanS, which is equivalent to that for a

m a x i m u m in d In E' (0)/d0 and d In J' (0)/d0.

These three definitions of transition temperature give appreciably

different values for that temperature. This was remarked in the previous

paper', and shown to follow very simply from the standard linear solid

representation which was considered adequate for the previous investigation

in a very narrow frequency range. In particular, it is to be expected that

the m a x i m u m in tan 8 will occur at a temperature intermediate between

the m a x i m u m in dE' (0)/d0 or E " (0) and that in dJ' (O)/dO or J " (0).

The aim of our simplified procedure can now be defined. It is to select

one point from the E'(O), E"(O), J'(O), J"(O) or t a n 8 (0) results and

observe how this point shifts with change of frequency. Since our frequency

shifts must be identical whether we use modulus or compliance results it

would suggest the best approximation will be obtained by defining the

transition temperature as the temperature of the maximum in either tan 8,

d In E" (O)/dO or d In J ' (0)/d0.

RESULTS

Typical results for the variation of the measured quantities E ' and E " are

261

P. R. P I N N O C K and I. M. W A R D

2.5 - 0.25

2-0 - 0.20

- 0

c,,i

•EuE 1"5 -0.15

E

u

ca

r"

[2

1D

o

£ 1-0 0.I0 ~o

2

ttl

0.5 0"05

(a)

I I I I I I I I I 0

20 30 40 50 60 70 80 90 100 110 120

Temperature, °C

0.25 r-

0.20 !

0"15

r- q22

0,10 t°I EP

0.05 -

(13) I I " I (I yneslcm 2 °C)

I I I I

0.0 30 40 50 60 70 80 90 100 110 120

Temperature, °C

Figure 2--Typical measurements made at 0"1 c/s ~a) E ' and E", (b) t a n & dE'/dO

and d log U/dO

Table 1. Transition temperatures for unoriented crystalline PET fibres

Birefring-

X-ray

crystallinity

I Temperature, °C for maximum Dynamic

[requency,

ence % E" dE" / dO tan8 d log E ' / d 0 c/s

33 ---7¢- T t 92 92 0"01

33 86 88] 97 96 0"1

33 89 [93 103 100 1

33 95[95 I 110 104 10

262

VISCOELASTIC BEHAVIOUR IN POLYETHYLENE TEREPHTHALATE

**shown in Figures 2(a) and 2(b), together with the derived quantities
**

dE'/dO, tan 6 and d In E/dO. Values of the transition temperatures defined

by the temperature at which these quantities have a m a x i m u m value are

given in Table 1 for various frequencies. Table 1 also includes the X-ray

crystallinity.

DISCUSSION

Dynamic mechanical data

The results in Table 1 show that, to a good approximation, the maxima

in dE'/dO and E " occur at the same temperature and similarly the maxima

in d in U/dO and tan 6 also occur at the same temperature, although the

latter temperature is appreciably higher than the former. These similarities

in temperature substantiate to a large extent the approximations made

earlier which resulted in equations (4), (5) and (6).

The transition temperatures which are defined as the temperatures for

m a x i m u m tan 6 have been plotted as a function of log frequency in Figure 3

in a way suitable for fitting to the W L F equation. The value of T,, needed

to give agreement between these data and the equation (also shown in

Figure 3) is 79°C. As will be remembered this form of the W L F universal

equation was formulated such that the fitting temperature T, should be

similar to the dilatometrically-measured transition temperature. This is

certainly verified here where previous dilatometric measurements 4 gave a

value of 81°C for crystalline polyethylene terephthalate polymer. It should

also be noted that it was not possible to fit the temperatures for maximum

E " to the W L F equation.

**Further justification for use of first-order approximations
**

Further justification for the use of the first-order approximations can

be obtained directly from the creep data.

12

**z~ --WLF equation, log ar -- 17'~ (r-Tq)
**

51.6-(r-r9 )

(D Dynamic mechanical data

.?

0 (11 Dietectric data

CD

0

-4

-8

g~

-12 -

I I I I I 1 I I I

60 70 80 90 100 110 120 130 140 150 160

Temperature, °C

Figure 3--Temperatures for (tan 6)nl~x. at various frequencies fitted to th

WLF equation

263

P. R. PINNOCK and I. M. WARD

**The master creep compliance curve (Figure 4 in Ward ~) shows that the
**

creep compliance J (t) is, to a good approximation, a linear function of

In t over the time range l0 s to 1014sec. This range corresponds to creep

data obtained in the time interval 10 to 10' sec over the temperature range

84.4 ° to 115.5°C. Over this range it therefore follows that dJ ( 0 / d l n t is

approximately constant and that dZJ ( t ) / d l n t2 and higher derivatives are

zero, giving direct justification for the first-order approximation.

Outside this range, i.e. from 10 -4 to 105 sec on the master curve, the

first-order approximation is not satisfactory, particularly at the lowest

times. This range covers creep data obtained at the three lowest tempera-

tures only (65.0°C, 70°C and 76.6°C). It will be noted that the shift factors

from these results do not, in fact, fit on to the W L F curve (Figure 5 in

Ward2). Over the central and higher range of the creep data, however,

where the link with the dynamic data is being established, the approxi-

mation holds and a good fit is obtained to the W L F equation.

**Comparison of dynamic mechanical and creep data
**

Using the approximations described earlier it is possible to check the

internal consistency of the dynamic mechanical data and the previously

published creep data. F r o m the creep measurements (Figure 3 in Ward ~)

E ' was computed over a range of temperatures at a number of fixed

frequencies (times) by assuming that E'(oJ, O)=l/J(t,O) with t=llto.

These derived dynamic data are given in Figure 4 where log E ' (co) is shown

as a function of temperature for four frequencies, viz. 10 -4, 10 -3, 10 -5,

10 - l c / s . The transition temperatures which are defined as those at the

point of m a x i m u m d ln E'/dO are also included in the figure. Comparison

of these with corresponding dynamic data of Table 1 shows reasonable

agreement confirming the equivalence of the creep and dynamic mechanical

measurements and the validity of the approximate procedures.

Figures 5(a) and 5(b) show the shift factor a~ as a function of temperature,

these data being obtained from the previous creep measurements. The

curve shown in Figure 5(a)is similar to that obtained in the previous work

where no correction was made for changes in the unrelaxed modulus (or

the factor pT/poTo) with temperature. Although such factors are extremely

small in polyethylene terephthalate where the creep compliance changes

markedly with temperature recent work by Morris and McCrum 9 prompted

us to attempt such a correction. On the basis of the high frequency results

of Thompson and Woods I° it was estimated that the change in the unrelaxed

modulus was approximately 0-2 per cent per deg. C. New shift factors were

then obtained from the previous data, taking into account this correction

factor. The data can again be fitted to the W L F equation, and the value

of T~, is slightly reduced, to 82°C from 85°C [Figure 5(b)].

This value of 82°C is in excellent agreement with both the dynamic To

of 79°C and the dilatometric transition temperature of 81 °C. This confirms

the expectations of the theoretical discussion that definition of dynamic

transition temperature as that for the m a x i m u m in tan 6 is necessary to

produce a consistent shift factor for both creep and dynamic data.

Over this wide frequency range, there is a definite divergence of the

264

VISCOELASTIC BEHAVIOUR IN POLYETHYLENE TEREPHTHALATE

**105 F '10- second' modulus
**

'102- second ' modulus

104 ~- ID '10a-second' modutus

'104- second' mod u{ u s

103~ -{-- Temperature for maximum

d tog E

102~ de

lO-l~-

uj 1001- @

~ 9.9

9-8

i

9"7~

i

9.6F-

951 I I I 1_

6O 70 80 90 100 110

Temperature, °C

Figure 4 -Modulus measurements at different times and temperatures derived

f r o m previous creep data

**frequency/temperature behaviour of the dynamic data from that of a
**

constant activation energy system. The fit to a WLF equation for the

dynamic data alone is probably not completely conclusive, but it would

certainly appear that this representation gives a consistent fit for both

dynamic and transient data.

**Comparison with dielectric measurements
**

In the paper on creep measurements, it was noted that the dielectric

loss measurements were consistent with the WLF equation. The shift

factors were obtained by Reddish 3 from the dielectric data by measuring

the frequency at which the tan 6 maximum occurs at a given temperature

and are also plotted in Figure 3. The consistency of the dielectric and

mechanical data is further confirmed by the present work, although it may

be possible that the best fit for the dielectric data does involve a small

vertical displacement with respect to the dynamic data. This displacement

would not affect the choice of the T,,, although it is to be noted that there

is not a significant difference between the WLF equation and a constant

activation energy at high frequencies.

CONCLUSION

]it is concluded that dynamic mechanical data on polyethylene terephthalate

are consistent with the WLF equation relating time-temperature equiva-

lence. Consistency between our previous creep data and the dynamic results

265

P. R. PINNOCK and I. M. WARD

6p

4.

2 (a)

o._6

_12 / I I [ I I I

6

4

2

0

~.- - 2

(3

-4

0

-8

-10

-12 I I I [ I I I

Y3 70 80 90 100 110 120 130

**Figure 5--Shift factors obtained from creep data
**

fitted to WLF equations, (a) uncorrected data,

(b) data corrected to account for the change in

the unrelaxed modulus with temperature

**can be o b t a i n e d if the transition t e m p e r a t u r e is defined f r o m the d y n a m i c
**

d a t a by the t e m p e r a t u r e at w h i c h tan ~ is a m a x i m u m .

Research Department,

I m p e r i a l C h e m i c a l Industries Fibres L i m i t e d ,

Harrogate, Y o r k s h i r e

( R e c e i v e d D e c e m b e r 1965)

REFERENCES

1PL~NOCK, P. R. and WARD,I. M. Proc. phys. Sac. 1963, 81, 260

WARD, I. M. Polymer, Lond. 1964, 5, 59

a REDDISH,W. Trans. Faraday Sac. 1950, 46, 459

4 KOLB, H. J. and IZARD, E. F. J. appl. Phys. 1949, 20, 564

5WILLIAMS, M, L., LANDELL,R. F. and FERRY, J. D. ]. Amer. chem. Sac. 1955,

77, 3701

6 FARROW,G. and PRESTON,D. Brit. ]. appl. Phys. 1960, 11, 353

~GRoss, B. Mathematical Structure of the Theories of Viscoelasticity. Hermann:

Paris, 1953

s STAVERMAN, A. J. and SCHWARZL, F. Die Physik der Hochpolymeren, Band IV.

(F_.d.H.A. STUART),Springer: Berlin, 1956

9 MORRIS,E. L. and McCRuM, N. G. ]. Polym. Sci. B, 1963, l, 393

I0 THOMPSON,A. B. and WooDs, D. W. Trans. Faraday Soc. 1956, 52, 1383

266

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