FLOW AND RECOVERY

OF DENTURE

PLASTICS

S@REN E. SORENSEN, D.D.S., M.S., AND GUNNAR RYGE, D.D.S., M.S.

Marquette University, School of Dentistry, Milwaukee, Wis. the dental profession has been confronted with the problem of warpage and systematic dimensional changes of dentures. Reports in the literature have been based upon linear measurements made across the posterior of a denture1T3 or by the use of various mechanical devices4-6 in order to determine the adaptation by comparison of dentures and models or impressions and models. Changes up to 0.5 mm. in various parts of a denture have been reported. Woelfel, Paffenbarger, and Sweeney 7 found that the warpage index was greatest for the epoxy resin (0.3 per cent) and lowest for the polystyrene (0.02 per cent). The warpage could not be detected clinically. The fact that some author9 express concern about the effects of flow of denture bases and plastic teeth after long-term stress application indicates the need for more data in this area. Tylmans has indicated that flow in acrylic resin crowns may be sufficient to break the cement union at the gingival margin. The purpose of this investigation was to study deformation and delayed elastic recovery of various types of denture-base resins. Permanent deformation refers in this article to a permanent change in shape of the specimen after ;/s hour or after 24 hours of recovery from various loads at certain test temperatures.

URING THE YEARS,

METHODS

AND

MATERIALS

The materials selected for the study are listed in Table I. Experimental Procedures.-The transverse deflection test in A.D.A. specification No. 12 for denture-base resin was used to determine whether a permanent change remained in a specimen of a given material after loading. The test described in A.D.A. specification No. 15lr for acrylic resin teeth (section 4.3.6) was used to determine indentation resistance and recovery. A specimen size of 1 sq. inch, with a thickness of g inch, was chosen in accordance with the American Society for Testing Materials (D 785-51) test for Rockwell hardness of plastic.*2 Oversized steel specimens were used for the fabrication of the molds for the heat-curing and self-curing polymethyl methacrylate specimens. The dimensions
This study was supported in part by research grant D-1057 and training grant DT.22 from the National Institute of Dental Research, U. S. Public Health Service. Portions of this paper were taken from a thesis by Dr. Serensep submitted to the faculty of the Graduate School, Marquette University, in partial fulfillment of the requirements for the degree of Master of Science. *Assistant Professor; present address: University of Buffalo Dental Srhool, Buffalo. N. Y. **Professor and Chairman, Department of Dental Materials.

1080

S@RENSEN AND RYGE TABLE I. LIST OR MATERIALS

=I

MATERIAL Experimental heat-curing resin* Experimental self-curing resin* Jectron Luxene Epoxolon

TYPE
--

BATCH 64-221-H, SR 100 SR-255 SR-253, 64-140-7 12318 SR 252, 98-48-3 SR 254, 98-48-4
52

DATE March, 1961 March, 1961 March, 1961 March, 1961 March, 1961 October, 1960 March, 1961 April, 1961 April, 1961

Clear olymer Strarg 4 t monomer Crosslinked monomert Pink polymer Straight monomer Crosslinked monomert Polystyrene Vinyl-acrylic Epoxy resin
-

resin

Gel batch

*Material furnished by Sartomer Resins, Inc.. Philadelphia, Pa. tThe crosslinking agent employed was 5 per cent ethylene dimethacrylate.

of the steel specimens were 70 by 10.67 by 3.67 mm. for the transverse deflection test specimens and 25.6 by 25.6 by 7 mm. for the Rockwell indentation test. Three deflection specimens and one indentation specimen were lubricated with a thin coat of petroleum jelly and invested in a denture flask using dental stone as a mold material. After setting of the stone, the steel specimens were removed, and the molds were flushed with three applications of hot detergent solution and rinsed with clean boiling water. The resin was packed in a mold lined with tinfoil at a temperature of 23 -L 2 C. A polymer :monomer ratio of 3 :l was used. A constant time schedule for mixing, gel formation, and packing of the molds was maintained for all specimens in which the same monomer type was used. Heat-curing specimens were trial packed twice, self-curing specimens once. The flask with the heat-curing material was held in a spring clamp and polymerized in a Hanau processing unit. The curing was carried out according to the following schedule : 73 * 1 C. for 11/z hours and then boiling for @ hour, after which the flask in the clamp was cooled in air at 23 r+ 2 C. for 30 minutes and then immersed in water at 23 + 1 C. for 15 minutes. The self-curing specimens were allowed to polymerize for 45 minutes in press and 45 minutes out of press before the flask was separated. Oversized wax specimens were used for the preparation of molds for the Jectron, Luxene, and Epoxolon test specimens. Manufacturers directions were followed in the investing procedures for these specimens. Five to six wax specimens equally spaced and one wax specimen for the Rockwell indentation test were invested in each flask. Except for the Luxene resin,* all specimens were processed by the investigator; the manufacturers directions were followed for each material.
*Processed by the courtesy of the Massey-Otto Dental Supply Company, Milwaukee,
Wis.

Volume 12 Number 6

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PLASTICS

10x1.

The Epoxolon specimens were all cured overnight at a temperature of 110 F. All specimens were marked after processing with an index number and stored in distilled water at room temperature in labeled bottles. Approximately 14 days to 3 weeks later, the transverse test specimens were machined to the following dimension: thickness 2.5 4 0.03 mm., width 10 + 0.03 mm. The cutting was performed according to A.D.A. specification No. W (section 4.3.5). The mean thickness of the specimens was determined to be 2.48 mm., with a standard deviation of 0.02 mm. ; the mean width of the specimens was 9.98 mm., with a standard deviation of 0.01 mm. The total number of specimens was 174, distributed fairly even between the seven materials. The specimens for the Rockwell indentations were sanded on all surfaces using wet 400 A aloxite waterproof Carborundum paper, with the top and bottom surfaces flat and parallel. Final thickness of these specimens was 6.28 + 0.2 mm A Hanau curing unit was used as a temperature-controlled water bath in which the transverse testing machine was placed. The transverse testing machine was provided with three stops. Two lateral aluminum stops secured the specimen in position under the metal rod through which the load was applied. The third stop provided the end stop for the specimen. In this way, it was possible to reproduce the position of a specimen. During the testing procedures, the transverse testing machine was placed against the back of the Hanau unit 20 cm. from the heating element, and the water level was kept at least 2 cm. above the specimen. Temperature readings were obtained at a distance of 2.5 cm. from the specimen. For this investigation, it was decided to study the deflection at four different loads (600 Gm., 1,500 Gm., 2,500 G m., and 4,000 Gm.) and at three temperature levels (21 C., 34 C., and 58 C.) * using the schedule of loading and reading in A.D.A. specification No. 12i (section 4.3.5). The delayed elastic recovery was recorded 30 minutes and 24 hours after removal of the indicated test load. Randomization of the order of material, specimen number, and load to be applied was carried out for each of the three temperature levels. All experiments were carried out in duplicate. Zero readings were performed for all specimens before any test was carried out. Each specimen was kept in the water bath for 30 to 60 minutes at the temperature for the performed test. After each deflection test, the specimen was removed from the transverse testing machine. The specimen was left for recovery in a vertical position in a small beaker which was placed next to the testing machine in the water bath. After the 30 minute or 24 hour storage period, the specimen was repositioned and the recovery was recorded as the deflection value under the 600 Gm. load. Indentation resistance was determined according to section 4.3.5 of A.D.A. specification No. 1511 on randomized specimens. The tests were performed at room temperature (23 3- lC.).
*The temperatures chosen were originally 21 C., 37 C., and 60 C. However, a systematic error in the temperature recording was noted, and it was found that the actual temperattlres were 21 C., 34O C. and 58O C. The actual temperatures of the experiments are, therefore, list,ed throughout this report.

1082

SZRENSEN AND RYGE

EPOXOLON LUXENE JECTRON

LOAD
Fig. I.-Deflection

IN GRAMS

x IO3

as a function

of load for various denture materials at 21 C.

RESULTS

Mean deflection and recovery values are listed in Table II. Recovery was calculated in percentage for each specimen, and the means are reported to the nearest 1 per cent. Reading error on deflection values was determined as the

SELF - CURING 34C

LOAD
Fig. 2.-Deflection

IN GRAMS x IO
of load for various denture materials at 34 C.

as a function

Volume 12 Number 6

FLOW AND RECOVERY OF DENTURE

PLASTICS

lOii3

LOAD
Fig. 3.-Deflection as a function of load for various

IN GRAMS
denture

x IO3
at 58O C.

materials

standard deviation on five consecutive readings on the same specimen. The calculated standard deviation was 0.24 mm. Variation in the water bath temperature was controlled to + 1 C. of the specified test temperature. Deflection versus load curves for the seven materials at the temperatures of 21 C., 34 C., and 58 C. are shown in Figs. 1 to 3. Table III gives the data for indentation resistance and recovery after flow. The ratio of load to projected area of indentation was calculated according io equations used by Sweeney, Sheehan, and Yost.i3 The standard deviation was calculated on mean recovery values obtained when testing four specimens of the same type of resin. The standard deviation was 0.87 per cent. It was originally planned to carry out the study using a factorial design scheme. Since some of the materials did not withstand the loads of 3,500 Gm. and 4,000 Gm. at 58 C., the resulting data did not lend themselves to a complete analysis of variance following the factorial design. Sufficient data were obtained, however, for deflections at 34 C. and 58 C. for loads of 600 Gm., 1,500 Gm., and 2,500 Gm. and for l/z hour recovery at 34 C. and 58 C. after loads of 1,500 Gm. and 2,500 Gm., and these data were, therefore, used for the analysis of variance. Table IV gives the analysis of variance computed on these deflection values, and Table V gives the analysis of variance with respect to s hour recovery. The computed figures are based on the difference measured in millimeters between the initial (600 Gm.) deflection value and the lb hour recovery value under GO0 Gm. load.

1084
DISCUSSION

S@RENSEN

AND

RYGE

Nol.*k? .

I ?;t%

the basis of the deflection values listed in Table II, the materials tested can be rated according to stiffness. At 21 C. and 34 C., Jectron gives the least deflection for any given load, followed by Luxene, Epoxolon, heat-curing resins, and self-curing resins, in that order. No significant differences were observed between deflection values for crosslinked and noncrosslinked resins. The two heat-curing polymethyl methacrylate resins and Jectron, Luxene, and Epoxolon recover completely (98 to 100 per cent) during the 1h hour storage period after all load applications at both 21 C. and 34 C. At 21 C., the self-curing resins recover completely (99 to 100 per cent) after a load of 3,500 Gm. At 34 C., these resins recover completely (98 to 100 per cent) within l/2 hour after 2,500 Gml load application. When a 4,000 Gm.
TABLE II. DEFLECTIONAND RECOVERYVALURSFORSEVRN DENTUREMATERIALS

Deflection and Recovery Values at 21 C. and 34 C.-On

=
TEMPERATURE 21 c. 34O c. I LOAD RANGE 58 c.

MATERIAL

VALUE

- _6003,500

-6001,500 _0.78 100% 101% 0.76 99% 100% 1.05 99% 101% 1.00 ;:q
0

T-

6002,500

-1

-_
Heat-curing straight monomer Heat-curing crosslinked monomer Self-curing straight monomer Self-curing crosslinked monomer Jectron Mean deflection Recovery W hr. Recovery 24 hr. Mean deflection Recovery W hr. Recovery 24 hr. Mean deflection Recovery W hr. Recovery 24 hr. Mean deflection Recovery x hr. Recovery 24 hr. Mean deflection Recovery x hr. Recovery 24 hr. Mean deflection Recovery g hr. Recovery 24 hr. Mean deflection Recovery W hr. Recovery 24 hr.

.2.33 99% 2.43 100% 2.94 99% 2.81 99% 1.75 101% 2.11 99% 2.28 99%

.1.73 98% 100% 1.70 100% 100% 2.35 100% 99% 2.30 99% 99% 1.29 100% 99% 1.60 100% 100% 1.56

6006006006004,000 2,500 %,000 1,500 _- ---_--3.17 99% 100% 3.38 99% 100% 6.29 93% 95% 5.47 96% 97% 2.38 ;;q
0 / , I , ,

1.25 97% 101% 1.24 98% 4.77

2.95 98% 103% 2.85

8.19 ;g
0

lO2Yo 88%
97% 4.37

96%
100%

7.83 94% 98%

12.31

76% 83%
12.34 90%

85%
96% 0.66 95% 99% 1.01 103% 105% 12.01

92%
2.69 96% 99% 5.16

0.58 104% 104%

1.52 99% 103% 2.36 97% 1ow?o 12.60

Luxene

3.10 100% 100%

Epoxolon

88%
93%

82% 88% f 1W.

Reading emc~ron deflection villues:

S.D. 0.024 mm., water bath temperatures

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PLASTICS

108.5

TABLE

III.

INDENTATION

RESISTANCE

AND

RECOVERY

DEPTH PiFTER 30 KG. LOAD FOR 10 MIN. DEPTH 4FTER 3 KG. LOAD FOR 10 MIS. __-__RATIO IX LOAD TO PROJECTED AREA OF INDENTATION (P.S.1.)

MATERIAL

NO. OF OBSERVATIONS --

NO. OF SPECIFICATIONS

RI? ZOVERY (%I

_-

Experimental heatcuring resin, straight monomer Experimental heatcuring resin, crosslinked monomer Experimental selfcuring resin, straight monomer Experimental selfcuring resin, crosslinked monomer Jectron Luxene Epoxolon
Standard deviation

0.088

0.010

11,000

0.087

0.009

89.6

11,200

,
9 0.100 0.017 83.0 9,700

0.099

0.018

81.8

9,800

6 10 8

0.076 0.090 0.077 .

0.008 0.015 0.007

89.5 83.3 90.9

1 / 1

12,800 10,800 12,600

on recovery values: 0.87 per cent.

load is applied at 34 C., the noncrosslinked self-curing resins recover 93 per cent, whereas the crosslinked self-curing resins give a recovery value of 96 per cent after yi hour. The corresponding values for 24 hour recovery after 4,000 Gm. load application at 34 C. are 95 and 97 per cent. When the total deflection values are below 3 mm., complete recovery r&ults for all materials. Deflection and Recovery Values at 58 C.-At 58 C., the order of stiffness of the resins noted above is changed by the fact that Epoxolon exhibits deflection values which are similar to or greater than the deflection values for the selfcuring resins. At this temperature, the deflection values for crosslinked heat-curing resins are slightly lower than those for the noncrosslinked resins, particularly with the higher loads. No significant difference in deflection is noted between crosslinked and noncrosslinked self-curing resins at 58 C. All self-curing resin and Epoxolon specimens except one collapsed under a total load of 2,300 to 2,500 Gm. or even under a load of 1,500 Gm. at 58 C. Some recovery values are above 100 per cent. The recorded deflection values for recovery are in these instances smaller than the initial deflection values. These data are explained as a result of continued polymerization of the resin.

1086

.S@RENSEN AND RYGE TABLE IV. ANALYSIS OF VARIANCE: DEGREESOF FREEDOM

I -

N 0. J;pD',o,s. . y;:";

DEFLECTIONVALUES MEAN SQUARE 21.3370 109.8286 87.5616 6.6717 16.3299

SOURCEOF VARIATION
-----

SUM OF SQUARES 128.0222 109.8286 175.1232 80.0608 97.9795 69.6813 69.2684 10.7955 740.7595

F 4;; 341 26 1: 22

Material ZETdperature Material and load Material and temDerature Temperature andioad Material X load X temperature Residual Total F 0.001 (1.40) = 12.61. F 0.001 (12.40) = 3.64.

16

::
12 6

TABLE V. ANALYSIS OF VARIANCE: DEGREESOF FREEDOM 6 : 2 ii

RECOVERYVAL.UES(?-$ HR.) SUM OF SQUARES 8.1286 5.8825 1.0071 2.1177 2.7489 0.9965 7.4094 1.6881 29.9788 MEAN SQUARE 1.3548 0.3529 0.4581 0.9965 1.2349 0.0603

SOURCEOFVARIATION ----Material Temperature Load Material and load Material and temperature Temperature and load Material X load X temperature Residual Total F 0.001 (1.28) = 13.50. F 0.001 (6.28) = 5.24.

F 22.47 97.55 16.70 5.85 7.60 16.52 20.48

EE

Jectron recovers completely (99 to 100 per cent) after 2,500 Gm. load application during a l/2 hour storage period ; 4,000 Gm. total load application results in 96 per cent recovery. After the 24 hour storage period, the recovery is 99 per cent. The heat-curing polymethyl methacrylate resins do not recover 100 per cent from any of the test loads during the l/i hour storage period. When loads of 1,500 and 2,500 Gm. are applied, the recovery value is 96 fo 98 per cent after the l/z hour period. The vz hour recovery after 4,000 Gm. load application is 92 to 94 per cent. A 24 hour storage period results in values of 100 per cent for loads of 1,500 and 2,500 Gm. and 96 to 98 per cent for the 4,000 Gm. loads. Epoxolon and self-curing resins show recovery values from 76 to 90 per cent for loads of 1,500 and 2,500 Gm. Complete recovery results, in all instances, when the total deflection values are below 3 mm. Analysis of Va&znce.-The analysis of variance given in Tables IV and V shows that all calculated F ratios are highly significant (p<O.OOl). The differ-

Volume 12 Number 6

FLOW

AND

RECOVERY

OF DENTURE

PLASTICS

lOXi

ences in deflection and recovery for materials, temperatures, and loads included in the analysis are, therefore, considered significant; also, the double interactions between material and load, material and temperature, temperature and load, and the triple interaction (material, load, and temperature j are all of statistical signifi-. cance. This analysis, therefore, strongly rejects the null hypothesis that the specimens all belong to the same sample population. Indentation Resistance Values.---Small differences exist between some types according to the data. The t test was performed on the mean recovery values for the indentation specimens. The values for the two heat-curing resins and Jcctron and Epoxolon are found to belong to the same population (differences not statistically significant). Similarly, the two self-curing resins and Luxene do Ilot exhibit statistically significant differences among each other in indentation resistance and recovery values. Statistically significant differences, however, are found between the two groups of materials outlined above. The t values obtained from any combination of materials between the two groups in all instances fall beyond the 99.5 confidence level (p<O.O05).
CONCLUSIONS

A comparative study of seven denture resins was carried out to evaluate the property of flow and recovery, and the following conclusions were made : 1. As temperature and load are increased, the deflection values increase. 2. At temperatures of 21 C. and 34 C., all materials except the self-curing resins were found to recover completely under the loads employed. 3. The self-curing resins did not recover completely even after 24 hours when subjected to 4,000 Gm. load at 34 C. 4. At 58 C., Jectron exhibited full recovery after $4 hour when subjected to loads of 2,500 Gm. Luxene and heat-curing resins recovered fully after 24 hours, and the other materials exhibited permanent deformation at all loads, even after 24 hours. Only Jectron withstood a 4,000 Gm. load at 58 C. without permanent deformation. 5. The use of crosslinked monomer decreased the deflection values slightly but did not result in significant improvement of the recovery values. 6. The deflection values required to produce permanent deformation were of the order of 3 mm. or over for all materials. 7. The deflection required to produce permanent deformation is larger than that which would normally be encountered when these materials are used as denture materials or repair materials. Therefore, permanent deformation is not considered a problem of practical significance for these materials at temperatures below mouth temperature. 8. The indentation resistance and recovery test divides the materials into tm-o distinct groups. The two heat-curing resins and Jectron and Epoxolon exhibited significantly larger resistance to indentation and also better recover\ than did the two self-curing resins and Luxene.

1088

S#RENSEN

AND

RYGE

J. Pros. Den. Nov..Dec., 1962

9. Additional work is indicated tq establish the exact relationship between temperatures and load in their roles as determining factors in permanent deformation of denture resins.
REFERENCES

9. 10. II. 12. 13.

Skinner, E. W., and Cooper, E. N. : Physical Properties of Denture Resins. I. Curing Shrinkage and Water Sorption, J.A.D.A. 30:1845-1852, 1943. Methods of Measuring Molding and Post-molding Changes in Acrylic Denture Materials, Vernonite Work Bench 2 :2, 1943. Woelfel, J. B., and Paffenbarger, G. C. : Dimensional Changes Occurring in Artificial Dentures, Internat. D. J. 9:451-460, 1959. Rupp, N. W., Dickson, G., Lawson, M. E., Jr., and Sweeney, W. T.: A Method for Measuring the Mucosal Surface Contours of Impressions, Casts and Dentures, J.A.D.A. 54:24-32, 1957. Ryge, G., and Fairhurst, C. W.: An Evaluation of Denture Adaptation on the Basis of Contour Meter Recordings, J. PROS. DEN. 9:755-760, 1959. Anthony, D. H., and Peyton, F. A. : Evaluating Dimensional Accuracy of Denture Bases With a Modified Comparator, J. PROS. DEN. g&3-692, 1959. Woelfel, J. B., Paffenbarger! G. C., and Sweeney, W. T.: Changes in Dentures During Storage in Water and m Service, J.A.D.A. 62:643-657, 1961. Peyton, F. A., Anthony, D. H., Asgar, K., Charbeneau, G. T., Craig, R. G., and Meyers, G. E.: Restorative Dental Materials, ed. 1, St. Louis, 1960, The C. V. Mosby Company, p. 399. Tylman, S. D., and Tylman, S. G.: Theory and Practice of Crown and Bridge Prosthodontics, ed. 1, St. Louis, 1960, The C. V. Mosby Company, p. 1032. Paffenbarger, G. C., Stanford, J. W., and Sweeney, W. T.: American Dental Association Specifications for Dental Materials 1960-1961, ed. 4, Chicago, 1960, American Dental Association. D. 553. Paffenbarger, G. C., Stanford, J. W., and Sweeney, W. T.: American Dental Association Specifications for Dental Materials 1960-1961, ed. 4, Chicago, 1960, American Dental Association. D. 62. A S T M Standards 1958. Part 9, Philadelphia, 1958, American Society for Testing Materials, p. 273. Sweeney, W. T., Sheehan, W. D., and Yost, E. L.: Mechanical Properties of Direct Filling Resins, J.A.D.A. 49:513-521, 1954. 604 NORTH SIXTEENTH ST. MILWAUKEE 3, WIS.