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Original Title: Thermodynamic Properties of Polystyrene and Styrene

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R. W. WARFIELD and RiI. C. PETREE, U . S. Naval Ordnance Laboratory,

Silver Spring, Maryland

INTRODUCTION

The study of the specific heat C, and related thermodynamic functions

of a monomer and its solid polymer over a temperature range extending

down to absolute zero represents a fundamental approach toward understanding the structure and internal motion of a polymer. lcrom accurate

C, measurements on the monomer and its polymer the entropy, enthalpy,

and free energy can be calculated, as well as changes in these functions due

to glass transitions, melting, crystallization, and polymerization. Specific.

heat measurements made a t low temperatures are also useful in testing

the validity of various theoretical equations for the C, of linear polymer

chains, such as those advanced by Tarassov. More thermodynamic data

on bulk polymers are needed to establish the nature of the glassy and crystalline states and to explain the magnitude of the energy changes which

occur when polymers are heated or cooled, crystallized or melted.

Presented in this paper are calculated values of the entropy, enthalpy,

and Gibbs free energy for polystyrene and styrene. Xlm, the difference

C, - C, and the number of vibrating units per repeating unit of polystyrene are determined.

RESULTS

Specific Heats of Styrene and Polystyrene

The C, of polystyrene from (30K. to 195K. has recently betn determined by Sochava and Trapeznikova,2and Ucberreiter aiid Otto-I,aupenmuhlen3 have determined C, for polystyrene between 257K. and S9(iK

The C, of styrene has been determined by Iitzer and co-worktrs4 over the

temperature range 15K. to 300K. Thrse data are shown in lcigure 1

and in Tables I and 11. Sochava aiid Trapeznikova2 concluded that the

bulge between 60K. and 110K. in the plot of C, versus temperature

for polystyrene (Fig. 1) is due to the internal rotation of the phenyl ring

around the polymer chain axis.

Extrapolation of the C, data of Sochava aiid Trapeznikova%between

0K. and 60K. was made by means of a Tarassov function.

C,

2/dR(T/OT)

497

498

where C, is the specific heat, R is the gas constant, T is the absolute temperature, and Or is the characteristic temperature, 160.8OK. as calculated

by Sochava and Trapeznikova.2 This function has been derived by

Tarassov' for the low temperature heat capacity of a chain structure by

TABLE I

Specific Heat, Entropy, Enthalpy, and Gibbs Free Energy of Styrene

Temp., "K.

Specific

Heat Cpa,

cal./g."

10

20

30

40

50

60

70

80

90

100

110

120

130

140

150

160

I70

180

190

200

210

220

230

240

250

260

270

280

290

298.16

300

(0.002)

0.027

0.053

0.074

0 .o w

0.106

0.118

0.129

0.139

0.149

0.159

0.170

0.181

0.194

0.209

0.224

0.243

0.264

0.287

0.311

0.334

0.358

0.381

0.404

0.389

0.395

0.401

0.406

0.414

0.419

0.421

ST -

&OK,

cal./g. O

0.0022

0 .Ol60

0.0338

0,0524

0.0709

0.0886

0.1055

0.1217

0.1372

0 . I521

0.1666

0.1808

0.1947

0.2086

0.2225

0.2365

0.2508

0.2655

0.2806

0.2962

0.3121

0.3284

0.3450

0.3618

0.4814b

0.4986

0.5114

0.5259

0.54033

0.5518

0.5542

H , - HOOK.,

cal./g.

0.02

0.29

0.82

1.56

2.48

3.54

4.72

6.01

7.40

8.89

10.48

12.18

13.99

15.93

18.03

20.26

22.69

25.33

28.20

31.31

34.65

38.23

42.04

46.08

75.13"

79.08

83.09

87.15

91.29

94.71

95.50

-(FT F~K.),

cal./g.

0.002

0.030

0.194

0.536

1.07

1.78

2.67

3.73

4.95

6.32

7.85

9.52

11.32

13.27

15.36

17.58

19.95

22.46

25.11

27.93

30.89

34.02

37.31

40.75

45.22

50.04

54.99

60.10

65.40

69.81

70.76

The entropy of fusion4is 0.104 cal./g.'

The heat of fusion4is 25.16 cal./g.

presented here aiid in other papers1z2indicate that the use of this function

to estimate C, a t low temperatures iiktroduces little error into entropy,

enthalpy, and free energy calculations.

499

TABLE I1

Specific Heat, Entropy, Enthalpy, and Giblrs Free Energy of Polystyrene

Temp., "K.

5

15

25

35

45

55

65

75

85

95

105

115

125

135

145

155

165

175

185

195

205

215

225

235

245

255

265

275

285

295

298.16

305

315

325

335

345

355

365

375

385

395

cal./g."

cal./g . O

(0.004)

(0.012)

(0.019)

(0.027)

(0.035)

0.058

0.081

0.090

0.095

0.100

0.106

0.113

0.122

0.131

0.140

0.150

0. 158

0.167

0.176

0.185

(0.195)"

(0.204)"

(0.214)"

(0.225)"

(0.237)"

(0.249)"

(0.261)"

(0.2i2)h

(0.285Ih

(0.297)b

( 0 .301)b

(0.310)b

(0.321)b

(0.333)b

(0.345)b

(0.357)b

(0.393)b

( 0 .423)h

(0 435)b

(0.447)b

(0.457)b

0.0092

0.0175

0.0252

0.0330

0.0408

0.0514

0.0639

0.0759

0.0871

0.0976

0.107'7

0.1175

0.12i3

0.13iO

0 1467

0.1564

0 1660

0 ,1756

0.1851

0.1946

0.2041

0.2136

0.2231

0.2327

0.2424

0.2522

0.2620

0.2719

0.2819

0.2920

0.2952

0.3022

0.3124

0.322i

0.3330

0.3434

0.3544

0.3660

0.3776

0.3892

0.4008

cal./g.

0.04

0.16

0.35

0.62

0.9i

1.55

2.36

3.26

4.21

5.21

6.27

7.40

8.62

9.93

11.33

12.83

14.41

16.08

17.84

19.69

21.64

23.68

25.82

28.07

30.44

32.93

35.54

38.26

41.11

44.08

45.04

47.18

50.39

53.72

57.17

GO. 74

64.67

68.90

73.25

7 7 .i 2

82.29

cal./g.

0.0060

0.1025

0.2800

0.5350

0.8660

1.277

1.794

2.433

3.194

4.062

5.039

6.113

7.293

8.565

9.942

11.41

12.98

14.65

16.40

18.26

20.20

22.24

24.38

26.61

28.05

31.38

33.89

36.51

39.23

42.06

42.08

44.99

48.02

51.16

54.39

57.73

61.14

64.69

68.35

72.12

16.03

Interpolated between the data of Sochava and Trapexnikova* (55-195K.) and that

of Ueberreiter and Otto-Laupenmuhlen3 (275-395K.).

bValues of specific heat in parentheses are those obtained by extrapolation (5-45'K 1

or by interpolation (275-395K.).

500

it! 020-

rJrJrJ7---,--u

:ir

60

120

,

/

A

_

TEMPERATURE PK)

The values of the entropy, enthalpy, and Gihbs free energy of styrene

and polystyrene have been calculated from C, data by numerical integration, and are presented in Tables I and l I and in Figures 2, 3, and 4. The

values were obtained by evaluating the thermodynamic relations

320

TEMPERATURE

(OK)

360

400

501

TEMPERATURE P'K)

80

160

240

TE M PE R ATU R E,

320

400

(OK1

\\-here (Sr - & O K ) , ( H , - Hook;), and (F, - F o o I i ) are the entropy, ciithulpy, and Gibbs frre energy, rehpwtively, relative to the absolute zero of

t tmpernture.

Atactic polystyrene exhibits little teiideiicy to crystallize and would be

502

importance would be the determination of the C, of isotactic polystyrene of

known crystallinity. Such data might be analyzed to yield information

indicative of the absolute entropy of polystyrene.

The entropy of polystyrene a t 298.16"K. was found to be 30.70 cal./

mole' and that of styrene 57.39 cal./moleo. The entropy of polymerization was found by difference to be 26.69 cal./mole". These values are in

agreement with the corresponding values given by Dainton and Ivin,j

namely, 32.23, 57.16, and 24.93 cal./mole". Burnett6 gives the entropy of

polymerization as 27.9 cal./moleo.

The enthalpy of styrene a t 298.16OK. was found to be 94.71 cal./g.

(9850 cal./mole) and that of polystyrene 45.04 cal./g. (4684 cal./mole)

At the same temperature the Gibbs free energy of styrene and of polystyrene were -7260 cal./mole and -4470 cal./mole, respectively.

The molecular weight of the polystyrene used by Sochava and Trapeznikova2 is not known, while that used by Ueberreiter and Otto-Laupenmuhlen3 is given as 3650. However, Ueberreiter and Otto-Laupenmuhlen have noted that below the glass transition temperature, the C, is

almost independent of the molecular weight and is a result of transverse

vibrations. An increase in the specific heat of polystyrene occurs a t the

glass transition range a t about 355K.

Smith and Dole7 have pointed out that the function C,/T versus T ,

where T is absolute temperature, is a constant if the specific heat rises

linearly with T from a zero value a t absolute zero. The function C,/T

measures the rate a t which the entropy increases with temperature.

(dS/dT), = C,/T

(5)

Dole and Wunderlich8 have presented data on the function C,/T versus

temperature for a number of polymers and long-chain hydrocarbons over

various temperature ranges. The C,/T values for the hydrocarbons pass

through a maximum a t 60-70K., which according to Dole and Wunderlich, is to be expected theoretically if one or more modes of vibration having

the same frequency dominate in this temperature range. They further

suggest that the plots of C,/T versus temperature for polyethylene, polyethylene sebacate, and the polyamide 66 nylon should also exhibit maxima a t low temperatures. However, the lack of accurate low-temperature

C, data on these polymers prevented calculation of C,/T functions for

them.

The plot of C,/T versus temperature for polystyrene is shown in Figure

5. The C,/T values are presented on the basis of moles of repeating units.

Doleg has shown that this function is a sensitive indicator of the glass

transition temperature T , of polymers. This transition is shown clearly

in Figure 5 to occur over the range 350-365"k'.

'k

50- 100

503

EO

TEMPERATURE P K )

Also shown in Figure 5 is a plot of C,/T versus temperature for conventional polyethylene, taken from the C, data of Sochavalo for the range

17-60K., from Sochava and Trapeznikova" for the range 58-270K.,

from Dole and co-workers12 for the range 273-393K. A very slight increase is observed a t about 70K., as predicted by Dole and Wunderlich,g

and a large maximum is observed a t the melting point (380K.). The great

difference in the magnitudes of the function C,/T for polystyrene and polyethylene is due to the large difference in the molecular weights of the repeating units.

If the linear Tarassov function employed to estimate the specific heat is

correct, then the plot of C,/T versus T for polystyrene shown in Figure 5

should have zero slope. However, it will be observed that a maximum

occurs a t about 65'K. This suggests that to account for the interactions

between chains, a T 3term should be added to the Tarassov function at low

temperatures. Temperley13 has also concluded that the one-dimensional

specific heat theory must be combined with a three-dimensional Debye

spectrum proportional to T 3a t low temperatures. Tarassov' has recently

come to a similar conclusion and has proposed a two-parameter specific

heat equation which corresponds to the mathematical treatment of Stockmayer and Hecht. l4

On the basis of a number of assumptions similar to those made by

who calculated the heat capacity per vibrating unit of polyethylene, it is

possible to estimate the number of classically vibrating units a t 273K. in

the polystyrene repeating unit -CH(C,H,) CH2-.

Three assumptions

are employed. The first is that the force constant of the C-H bond is so

great that the -CH2group will vibrate as a single unit; the second is

that every group in the chain can vibrate harmonically with two degrees of

freedom along mutually perpendicular axes transverse to the chain direction; and the third, that longitudinal or stretching vibrations are negligible a t 273K. If each vibrating unit vibrates with two degrees of free-

504

dom, the expected specific heat would be 2R or 3.97 cal./moleo per vibrating unit. However, these considerations apply to C,,, not to C,.

C, can be calculated by means of the equation

cal./moleo; I'is the velocity of sound, 4'395 m./sec.15 d is the coefficient of

volume expansion, 2.33 X

per deg ;I6 and J is the mechanical equivalent of heat, 4.184 X lo7 ergs/cal.

is found to be 26.1 cal./moleo,

and C, - C, is thus 2.0 cal./moleo.

The number of vibrating units per repeating unit is found by dividing

C, by 2R, or 26.1 cal./moleo by 3.97 cal./moleo, which equals 6.57. This

implies that the pendent phenyl group is equivalent to four classically

vibrating units.

CONCLUSION

Styrene and polystyrene arc the only monomer-polymer pair for which

the C, data necessary for calculating the thermodynamic. functions are

available. Data on other systems would be of great utility for studying

the nature of the crystalline and amorphous btates, calculating kinetic

parameters for the polymerization process, studying the effects of various

degrees of crosslinking on the thcrmodj namir fun(~tions,

and investigating

the various theoretical equations for the specific heat of polymers. If data

were available on both the crystalline and amorphous forms of a polymer

the residual entropy might be determined.

The authors would like to express their appreciation to Dr. George T. Furukama of

the National Bureau of Standards for his helpful romnierits and to Mr. G. D. Blum for

checking the calculations.

References

1. Tarassov, V. V., Doklady Akad. .Yaiik S.S.S.IZ., 100, 307 (1955); J . Am. Chem.

SOC.,

80,5052 (1958).

2. Sochava, I. V., and 0. I). Trapeznikova, Vestnik Leningrad Univ., Ser. Piz. i

Khim., 13,No. 3,65 (1958);Cheni. Abslr., 53,4681(1959).

3. Ueberreiter, K., and E. Otto-Lauperimiihlen, 2. Naturforsch., 8a, 664 (1953).

4. Pitzer, K. S., L. Guttman, and E. F. Westrum, J . Am. Chenz. SOC.,68, 2209

(1946).

5. Ilainton, F. S., and K. J. Ivin, Qitart. Rev::., 12,76 (1958).

6. Burnett., G. M., Mechanism of P d y ~ i wIr'eactions, Interscience, New York, 1954,

p. 385.

7. Smith, C. W., and M. Dole, J . Polynier. Sci.,20, 37 (1956).

8. Dole, M., and B. Wunderlirh, .2falironrol. Cheni., 34,29 (1959).

9. Dole, M., Kolloid-Z., 165, 40 (1959).

10. Sochava, I. V., Doklady .-lkad. iVaiilc S.S.S.R., 130, 126 (19GO).

11. Sochava, I. V., and 0. 1.Trapeznikova, Dokladq Akad. Nauk S.S.S.R.. 113,

784 (1957).

505

20,781 (1952).

13 Temperley, H. N. V., J . Research Natl. Bur. Standards, 56,55 (19%).

14. Stockmayer, W. H., and C. E. Hecht, J . Chetn. Phys., 21, 1954 (1953).

15. Krisnamurthi, M., and G. Sivarama-Sastry, Nature, 174,132 (1954).

16. Boyer, R. F., and R. S. Spencer, Advances in Colloid Science, Interscienre, Ken.

York, 1946, p. 125.

Synopsis

A Tarassov function has been used to estimate the specific heat of polystyrene between

0" and 60K. These data, together with published C, data, have been used to calculate

the entropy, enthalpy, and free energy of styrene and polystyrene from 0" to 298.16"K.

The entropy of polymerization of styrcne a t 298.16"K. was found to be26.69 cal./mole".

The thermodynamic function C,/T versus T as calculated for polystyrene, increases to a

maximum a t 65K. and then increases again a t the glass transition temperature. The

Tarassov function, which is shown to be useful in estimating the specific heat of amorphous polymers, should be combined with a T3 Debye function to yield more accurate

c, data a t low temperatures. The number of classically vibrating units per repeating

unit of polystyrene was found to be 6.57. The difference C, - C, i ~ a scalculated a t

273K. and found to be 2.0 cal./niole".

R6sum6

Une fonction de Tarassov a 6th utilisQepour estimer la chaleur spdcifique du polystyrbne entre zero a t 60K. Ces valeurs, en mBme temps que les valeurs de C, publiBee,

utilisees pour calculer les entropies, enthalpie et Qnergie libre du styrene et du

ont QtQ

polystyrbne de 0K. B 298.16"K. L'entropie de polym6risation du styrbne B 298.16"K.

est QgaleB 26.69 cal/deg.-mole. La fonction thermodynamique C,/T vs T , telle qu'elle

est calculee pour le polystyrhe, augmente jusqu'h un maximum B 65"K, puis

augmente de nouveau B la tempdrature de transition vitreuse. La fonction de Tarassov,

qu'on a montrd Btre utile pour estimer la chaleur spQcifique de polymhes amorphes

devrait Btre combinbe avec une fonction en T3 de Debye pour donner des valeurs plus

prhcises de C, aux basses tempQratures. Le nombre d'unitds vibrant classiquement par

uniti: de la chaine de polystryitne est de 6.57. C, - C, est calculi: B 273K. et est Bgal B

2.0 cal/deg.-mole.

Zusammenfassung

Zur Bestimmung der spezifischen Warme von Polystyrol zwischen 0" und 60K. wurde

eine Tarassovfunktion verwendet. Die Daten u-urden zusammen mit veroffentlichten

C,-Kerten zur Bcrechnung der Entropie, Enthalpie und freien Energie von Styrol und

Polystyrol im Bereich von 0" bis 298,16"K. verwendet. Die Polymerisationsentropie von

Styrol bei 298,16"K. wurde zu 26,69 cal/Grad.Mol bestimmt. Die fur Polystyrol

berechnete thermodynamische Funktion C,/T steigt als Funktion von T zu einem

Maximum bei 65K. und zeigt dann einen zweiten Anstieg bei der Glasumwandlungstemperatur. Es nird gezeigt, dass es gunstig ist, die fur die Berechnung der spezifischen

Warme amorpher Polymerer brauohbare Tarassovfunktion mit einer T3-Debyefunktion

zu kombinieren, um genauere C,-Werte fiir tiefe Temperaturen zu erhalten. Die Zahl

der klassischen Oszillatoren pro Grundeinheit wurde fur Polystyrol zu 6,57 bestimmt.

C, - C, wird fur 273C. berechnet und zu 2,O ral/Grad-Mol gefunden.

Revised March 13, 1961

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