NUREG/CR-3629

SAND83-2651

RV

Printed April 1984

The Effect of Thermal and Irradiation

Aging Simulation Procedures on

Polymer Properties

L. D. Bustard, E. Minor, J. Chenion

F. Carlin, C. Alba, G. Gaussens, M. LeMeur

Prepared by

Sandia National Laboratories

Albuquerque, New Mexico 87185 and Livermore, California 94550

for the United States Department of Energy

under Contract DE-AC04-76DP00789

Prepared for

U. S. NUCLEAR REGULATORY COMMISSION
NOTICE

This report wasprepared as an account of work sponsored by an

agency of the United States Government. Neither the United

States Government nor any agency thereof, or any of their employees, makes any warranty, expressed or implied, or assumes

any legal liability or responsibility for any third party's use, or the

results of such use, of any information, apparatus product or

process disclosed in this report, or represents that its use by such

third party would not infringe privately owned rights.

Available from

GPO Sales Program

Division of Technical Information and Document Control

U.S. Nuclear Regulatory Commission

Washington, D.C. 20555

and

National Technical Information Service

Springfield, Virginia 22161
NUREG/CR-3629

SAND83-2651

RV

THE EFFECT OF THERMAL AND IRRADIATION

AGING SIMULATION PROCEDURES ON POLYMER PROPERTIES

L. D. Bustard and E. Minor

Sandia National Laboratories

Albuquerque. New Mexico 87185, USA

J. Chenion. F. Carlin, C. Alba. and G. Gaussens

CEA-ORIS LABRA at Saclay

91190 Gif-sur-Yvette. France

M. LeMeur

CEA-DAS-SAF

92260 Fontenay-aux-Roses. France

Printed April 1984

Sandia National Laboratories

Albuquerque. New Mexico 87185

Operated by

Sandia Corporation

for the

U.S. Department of Energy

Prepared for

Electrical Engineering Branch

Division of Engineering Technology

Office of Nuclear Regulatory Research

U.S. Nuclear Regulatory Commission

-Washington. DC 20555

Under Interagency Agreement 40-550-75

NRC FIN No. A-1051
PREVIOUS PUBLICATIONS IN THIS SERIES

1. K. T. Gillen. R. L. Clough. G. Ganouna-Cohen. J. Chenion.

and G. Delmas. Loss of Coolant Accident (LOCA)

Simulation Tests on Polymers: The Importance of

Including Oxygen. NUREG/CR-2763, SAND82-1071, July 1982.

2. K. T. Gillen, R. L. Clough. G. Ganouna-Cohen, J. Chenion,

and G. Delmas, "The Importance of Oxygen in LOCA Simulation Tests," Nuclear Engineering and Design. 74 (1982).

pgs. 271-285.

ii
ABSTRACT

Prior to initiating a qualification test on safetyrelated equipment, the testing sequence for thermal and

irradiation aging exposures must be chosen. Likewise. the

temperature during irradiation must be selected. Typically.

U.S. qualification efforts employ ambient temperature

irradiation, while French qualification efforts employ 700 C

irradiations. For several polymer materials, the influence

of the thermal and irradiation aging sequence, as well as the

irradiation temperature (ambient versus 70 0 C). has been

investigated in preparation for Loss-of-Coolant Accident

simulated tests.

Ultimate tensile properties at completion of aging are

presented for three XLPO and XLPE, five EPR and EPDM, two

CSPE (HYPALON), one CPE, one VAMAC, one polydiallylphtalate.

and one PPS material.

Bend test results at completion of aging are presented

for two TEFZEL materials.

Permanent set after compression results are presented for

three EPR. one VAMAC, one BUNA N. one Silicone, and one Viton

material.

iii/iv

TABLE OF CONTENTS

Executive Summary 1

1.0 Introduction 3

2.0 Samples 4

2.1 U.S. Samples 4

2.2 French Samples 5

3.0 Facilities i0

3.1 Radiation Aging Facility 10

3.2 Thermal Aging Facility 18

4.0 Experimental Techniques 20

4.1 U.S. Samples 20

4.2 French Samples 26

5.0 Results 41

5.1 U.S. Samples 41

5.1.1 CSPE and CPE Jacket Materials 41

5.1.2 EPR Insulation Materials 47

5.1.3 XLPO Insulation Materials 47

5.1.4 TEFZEL Materials 47

5.1.5 Compression Set Tests 60

5.2 French Samples 60

5.2.1 PRC (82 Ii) 63

5.2.2 EPDM (82 12 and 82 19) 63

5.2.2.1 EPDM (82 12) 63

5.2.2.2 Fire-proof EPDM (82 19) 63

5.2.3 EPR (82 H4 and 82 J4) 67

5.2.4 VAMAC (82 H3 and 82 J3) 67

5.2.5 HYPALON (82 G10) 68

5.2.6 PPS (82 H6) 68

5.2.7 Polydiallylphtalate (82 H5) 68

6.0 Conclusion 76

References 77

V
LIST OF FIGURES

2.1 Dimensions for 82 GlO. 82 H3, and 82 H4 French 7

Dumbbell Samples

2.2 Compression Set Fixtures Used for 82 J3 and 8

82 J4 French O-ring Seal Samples

2.3 Dimensions for 82 H5 and 82 H6 ISO Dumbbell Samples 9

3.1 Artist's Rendition of Low Intensity Cobalt 11

Array (LICA) Facility

3.2 Arrangement of Low Intensity Cobalt Array (LICA) 12

Facility for U.S.-French Aging Program

3.3 Locations of Thermoluminescent CaF 2 Wafers 13

Inside LICA Irradiation Can During Dose Rate

Gradient Mapping

3.4 A LICA Irradiation Test Cell 16

3.5 EPR 1 and EPR 2 Insulation Specimens Prepared 17

to be Inserted into the Sample Aging Region of

a LICA Irradiation Test Cell

3.6 Oven Aging Cell 19

4.1 U.S. Compression Set Fixture 24

4.2 Orientation of U.S. Compression Set Fixtures 25

in Radiation Field

4.3 82 H5 and 82 H6 Samples Prepared for Aging 32

4.4 82 H5 Samples Prior to Insertion into LICA 33

Irradiation Cell

4.5 Orientation of 82 H5 and 82 H6 Samples During 34

Irradiation

4.6 Preparation of 82 H3. 82 H4, and 82 G1O Samples 35

for Aging

4.7 82 H3. 82 H4. and 82 G1O Samples Shown as Prepared 36

to be Inserted into LICA Irradiation Cell

4.8 Orientation of 82 H3. 82 H4. and 82 G1O Samples 37

During Irradiation

vi
LIST OF FIGURES (Continued)

4.9 82 J3 Samples Prepared to be Irradiated 38

4.10 Irradiation Aging Configuration Used for 39

82 J4 Samples

5.1 Ultimate Tensile Elongation of CSPE in 42

Various Environments

5.2 Ultimate Tensile Strength of CSPE in Various 43

Environments

5.3 Ultimate Tensile Elongation of CPE in Various 44

Environments

5.4 Ultimate Tensile Strength of CPE in Various 45

Environments

5.5 Ultimate Tensile Strength of CPE in Various 46

Environments

5.6 Repeatability of Ultimate Tensile Elongation 48

Results for CPE During Two R2 7 Exposures

5.7 Repeatability of Ultimate Tensile Strength 49

Results for CPE During Two R2 7 Exposures

5.8 Ultimate Tensile Elongation of EPR 1 in 50

Various Environments

5.9 Ultimate Tensile Strength of EPR 1 in Various 51

Environments

5.10 Ultimate Tensile Elongation of EPR 2 in 52

Various Environments

5.11 Ultimate Tensile Strength of EPR 2 in Various 53

Environments

5.12 Ultimate Tensile Elongation of XLPO 1 in 54

Various Environments

5.13 Ultimate Tensile Strength of XLPO 1 in Various 55

Environments

5.14 Ultimate Tensile Elongation of XLPO 2 in 56

Various Environments

vii
LIST OF FIGURES (Continued)

5.15 Ultimate Tensile Strength of XLPO 2 in 57

Various Environments

5.16 Ultimate Tensile Properties for PRC (82 Ii) 64

5.17 Ultimate Tensile Properties for EPDM (82 12) 65

5.18 Ultimate Tensile Properties for Fire-Proof 66

EPDM (82 19)

5.19 Ultimate Tensile Properties for EPR (82 H4) 69

5.20 Permanent Set After Compression for EPR (82 J4) 70

5.21 Ultimate Tensile Properties for VAMAC (82 H3) 71

5.22 Permanent Set After Compression for 72

VAMAC (82 J3)

5.23 Ultimate Tensile Properties for HYPALON 73

(82 G1O)

5.24 Ultimate Tensile Properties for PPS (82 H6) 74

5.25 Ultimate Tensile Properties for 75

Polydiallylphtalate (82 H5)

viii
LIST OF TABLES

2.1 Nominal Insulation and Jacket Thicknesses for 5

U.S. Samples

3.1 Relative Dose Rate Gradients, R/RA. for Several 14

LICA Irradiation Positions

4.1 Radiation Dose and Thermal Exposure Time for 23

U.S. Insulation and Jacket Specimens

4.2 Radiation Doses and Thermal Aging Conditions 26

for Each U.S. Compression Set Fixture

4.3 Thermal Exposure Temperatures for French Samples 29

4.4 Total Radiation Dose and the Thermal Exposure 30

Time for Each Group of French Samples

4.5 Accuracy of French Measurements 40

5.1 Bend Test Results for TEFZEL 1 58

5.2 Bend Test Results for TEFZEL 2 59

5.3 U.S. Compression Set Test Results 61

5.4 Tensile and Compression Set Results for 62

French Samples

ix
ACKNOWLEDGMENTS

Our appreciation is extended to Mike Luker, who ably

assisted throughout the experimental aging program. John

Lewin. Tim Gilmore. Jerry Seitz, Jack Bartberger, Pat Drozda.

and Lowell Jones also provided valuable assistance during the

experimental effort.

X
EXECUTIVE SUMMARY

As part of a joint French/U.S. sponsored research

program, the influence of accident testing conditions on the

behavior of polymer materials is being investigated. Test

variables in the accident program include: irradiation temperature, oxygen presence during accident simulations, and

simultaneous versus sequential accident exposures. In preparation for the accident tests, polymer materials were exposed to irradiation and elevated temperatures to produce an

"accelerated age". Test variables in the aging program were

irradiation temperature, the order of the aging sequence, and

simultaneous versus sequential aging techniques. The influence of aging dose rate and accident oxygen concentration has

previously been documented1 and our current work is an

extension of this previous effort.

In this report, test results at completion of the aging

exposures are presented for several commercial insulation and

jacket materials, compression and gasket materials, and

thermosetting and thermoplastic materials. Our goals for the

aging portion of the research program were:

1. To investigate whether polymer materials are sensitive to the sequential order in which they are irradiated and thermally aged. Previously published

results2 for low-density polyethylene (LDPE) and

polyvinylchloride (PVC) indicated that irradiation

followed by a thermal aging exposure was the more

spvere sequence. We wished to establish the applicability of this conclusion for a broader class of

materials. Both irradiation followed by thermal exposure and thermal exposure followed by irradiation

aging sequences were part of the testing program.

2. To investigate the importance of irradiation temperature during sequential aging exposures. French

regulatory documents 3 require aging and accident

irradiations for qualification testing to be performed at 70 0 C. In contrast, typical U.S. qualification efforts perform ambient temperature irradiations. Irradiations at ambient (-270C) and 700 C

were performed as part of the testing program.

3. To provide a variety of aged samples for use during

LOCA simulation experiments.
Our experimental results at completion of the aging program indicate:

1. If sequential ordering of irradiation and thermal

exposures was important to the aging degradation of

tensile properties, usually the irradiation followed

by thermal exposure sequence was most severe.

2. In general, the choice of irradiation temperature was

secondary to the choice of aging sequence in its effect on polymer properties.

3. For several materials, tensile properties at completion of aging were only slightly affected by both the

irradiation temperature and the order of the sequential aging environmental exposures.

4. At most, only slight differences in permanent set

were noted as a result of the various aging techniques.

Ultimate tensile properties at completion of aging are

presented for three cross-linked polyolefin (XLPO) and cross

linked polyethylene (XLPE). five ethylene propylene rubber

(EPR) and ethylene propylene diene terpolymer (EPDM), two

chlorosulfonated polyethylene (CSPE, HYPALON). one chlorinated polyethylene (CPE), one acrylic polyethylene (VAMAC),

one polydiallylphtalate. and one phenylene polysulfide (PPS)

material.

Bend test results at completion of aging are presented

for two TEFZEL materials. o

Permanent set after compression results are presented for

three ethylene propylene rubber (EPR), one acrylic polyethylene (VAMAC), one BUNA N, one Silicone, and one Viton

material.

2
1.0 INTRODUCTION

When used as part of a safety-related system, equipment

must meet certain qualification criteria. Several documents

describe or suggest the tests and data necessary to establish

qualification. For example. IEEE standards. USNRC Rules

(1OCFR50.49) 5 and documents (NUREG-0588) 6 and French

Documents (HM/63-7195/6) 3 provide guidance concerning

qualification. These documents generally require qualification efforts to account for aging of components under normal

operating conditions by performing accelerated aging of

equipment or components prior to simulation of accident

conditions.

The aging environment inside a nuclear reactor containment is a multistress environment including thermal and

radiation stresses. Historically, aging in this multistress

environment is simulated by a sequential application of

single stress environmental exposures. For example, IEEE

323-19747 suggests a thermal aging followed by irradiation

aging exposure. This exposure is considered the most severe

sequence for most equipment and applications. "However, the

sequence used shall be justified as the most severe for the

item being tested.''7

As part of a joint French/U.S. sponsored research program, we are investigating the influence of testing conditions on the behavior of polymer materials. Variables in the

test program include: aging sequence, irradiation temperature, oxygen presence during accident simulations, and

simultaneous versus sequential accident and aging exposures.

The influence of dose rate and oxygen concentration has previously been documented1 and our current work is an extension of this previous effort.

In preparation for LOCA research experiments, we have

aged several commercial insulation and jacket materials.

compression and gasket materials, and thermosetting and

thermoplastic dumbbells. We have accumulated sufficient

aging data to demonstrate that some materials are sensitive

to the order and manner in which they are irradiated and

thermally aged. Properties of other polymer materials did

not depend on the order and technique of radiation and

elevated temperature exposures. In this report we summarize

our data and discuss its significance toward qualification

testing of nuclear grade safety-related equipment.

3
2.0 SAMPLES

2.1 U.S. Samples

The U.S. samples consisted of six insulation materials,

two jacket materials, and five compression materials. The

insulation and jacket materials were carefully obtained by

disassembling cable received from five U.S. manufacturers of

Class 1E cables. The materials are:

EPR 1 A radiation crosslinked fire-retardant EPDM insulation obtained from a shielded instrumentation

cable.

EPR 2 A chemically crosslinked fire-retardant EPDM insulation obtained from a 600V, 3-conductor control

cable.

XLPO 1 A crosslinked polyolefin insulation obtained from

a shielded instrumentation cable.

XLPO 2 A crosslinked polyolefin insulation obtained from

a 600V, 3-conductor control cable.

TEFZEL 1 A TEFZEL insulation removed from a thermocouple

extension cable.

TEFZEL 2 A TEFZEL insulation removed from a shielded instrumentation cable.

CSPE A chlorosulfonated polyethylene jacket removed from

a 600V. 3-conductor control cable.

CPE A chlorinated polyethylene jacket removed from a

600V, 3-conductor control cable.

Each of the jacket and insulation specimens were cut to

a length of 10.9 + .3 cm (except for EPR 1 which had an

initial length of 10.2 + .3 cm). The insulation specimens

were tubular in shape. The nominal insulation thickness is

summarized in Table 2.1. The jacket specimens were cut with

a die into rectangular pieces. The width of each specimen

was .56 cm. The nominal jacket thicknesses are also presented in Table 2.1.

The five compression materials were obtained from the

same U.S. manufacturer. Samples, received from the manufacturer as compression molded sheets with nominal thicknesses of .178 and .191 cm, were cut into small rectangles

with approximate dimensions: .6 cm x 1.6 cm. The five

materials were: EPR A. EPR B. BUNA N. SILICONE, and VITON.

4
Table 2.1

Nominal Insulation and Jacket Thicknesses

for U.S. Samples

Material

EPR 1

EPR 2

XLPO 1

XLPO 2

TEFZEL 1

TEFZEL 2

CSPE

CPE

Nominal Thickness (cm)

.064

.076

.076

.076

.038

.051

.114

.114

2.2 French Samples

The French samples consist of six elastomer materials

used in the manufacture of electrical cables (insulation and

jacket materials), two O-ring seal materials and two thermoplastic and thermosetting materials used in the manufacture

of connectors.

The electrical cable materials are in the form of either

110 mm-long pieces of insulating material stripped from the

copper conductor (identified by "I"). dumbbells cut from

jacket material and identified by "G". or standard dumbbells

cut from compression molded sheets (identified by "H").

Elastomer dumbbell dimensions are shown in Figure 2.1. The

six cable materials are:

82 Ii PRC

82 12 EPDM

82 19 EPDM

82 G1O HYPALON

Chemically crosslinked polyethylene in the

form of conductor insulation for 3-conductor

cables.

Ethylene propylene diene terpolymer conductor insulation. Samples taken from a

3-conductor cable.

Alumina-loaded. ethylene propylene diene

terpolymer conductor insulation. This

material was removed from a 3-conductor

cable.

Chlorosulfonated polyethylene used in the

manufacture of cable jackets.

5
82 H3 VAMAC

82 H4 EPR

Acrylic polyethylene in the form of sheets from

which dumbbells (Figure 2.1) were cut. Material is used in electrical cable jackets.

mechanical parts, and connectors.

Copolymer ethylene-propylene rubber in the form

of 3 mm sheets from which dumbbells (Figure

2.1) were cut. Material is used in the manufacture of insulation for electrical cables

sheathed with fire-proof EPDM.

The two O-ring seal samples (identified by "J") have an

inner diameter of 12 mm and an outer diameter of 17 mm. They

were enclosed and held under compression in aluminum grooves

as shown in Figure 2.2. The O-ring seal materials are:

82 J3 VAMAC

82 J4 EPR

Same material as 82 H3. used in the manufacture

of O-ring seals.

Same material as 82 H4. used in the manufacture

of O-ring seals.

The two thermoplastic and thermosetting materials used

in the manufacture of connectors were in the form of International Organization for Standardization (ISO) dumbbells.

The dimensions for these dumbbells is illustrated in Figure

2.3. The two materials are:

82 H5 Polydiallylphtalate

Thermosetting polyester used in connectors and mechanical parts.

Phenylene polysulfide used in the

manufacture of switches and connectors.

82 H6 PPS

The French sample identification code (82 Il. 82 H5,

etc.) will be used in the remainder of this report. The code

presents:

" The year of the starting investigation,

" The sample shape code letter.

" A number identifying the material type.

6
EE

EE

co o

Rh.

4mm

IL

Figure 2.1. Dimensions for 82 G1O, 82 H3. and 82 H4 French

Dumbbell Samples - H3 French Standard

(Commission of Normalization NO NF.T 51-034-June 1968)

7
A 06.2 mm

AA' SECTION

Figure 2.2. Compression Set Fixtures Used for 82 J3 and

82 J4 French O-ring Seal Samples

8
0

Figure 2.3. Dimensions for 82 H5 and 82 H6 ISO Dumbbell

Samples

9
3.0 FACILITIES

3.1 Radiation Aging Facility8

Figure 3.1 shows an artist's rendition of the Low

Intensity Cobalt Array (LICA) radiation facility. Approximately 16,000 curies of Co-60 is positioned at the bottom of

a water-filled tank. Radiation aging is carried out in

water-tight test cells by lowering the cells to the bottom

of the tank. Water, separating the Co-60 from experimenters

at the top of the tank, provides radiation shielding.

Approximately 10.000 curies of Co-60 is positioned in a

circular array to provide high dose-rate exposures. This

portion of the radiation facility was not used in this test.

The remaining 6,000 curies of Co-60 is positioned in two

parallel arrays as shown in Figure 3.2. Test cell holders.

each containing four cylindrical holes, are oriented parallel

to the linear cobalt holders. One holder is located between

the two linear arrays of cobalt; the remaining holders are

located on the two sides of the cobalt-60 sources at various

distances from them. Test cells placed in any of the holes

of a given holder receive comparable radiation dose rates.

The dose rate is governed by the distance of the cell

from the cobalt array. Center-of-can dose rates are given

in Figure 3.2. Gradients in dose rates occur in the individual test cells; for example, there is a dropoff in dose

rates between the parts of the cell closest to, and furthest

from, the cobalt. A Victoreen Model 550 Radicon III Integration/Rate Electrometer with a Model 550 air ionization

probe was used to measure the dose rate at the center of the

test cell. Accuracy was ± 5 percent. Harshaw TLD-400's

(calcium fluoride manganese activated thermoluminescent

detectors) were used to map the radiation gradients for

several of the LICA positions. Figure 3.3 illustrates the

positioning of the CaF 2 Mn wafers during gradient mapping:

Table 3.1 summarizes the measured gradients. Accuracy of the

CaF 2 wafers was + 10 percent. For LICA can positions III

A. III B. IV A. IV B. V A. and V B. center-of-can dose rates

only were measured. Gradients are similar (by symmetry) to

those measured for the respective C and D positions. Gradient effects were reduced by rotating the cans during the

exposure or by appropriate positioning of the samples within

the test cell.

10
Figure 3.1. Artist's Rendition of Low Intensity Cobalt

Array (LICA) Facility

11
DOSE RATE KRD/H

LEVEL 5/28/82

COBAL 71 PENCILS

0000 0000

0000

0000

0000 000

VI

V 85

19

IV 114

65

19

6

D C B A

Figure 3.2. Arrangement of the Low Intensity Cobalt Array

(LICA) facility for U.S./French aging program.

French samples were aged using positions

IV A-IV D. U.S. Samples were aged using

positions III A-III D and V A-V D.

12
2 CENTERLINE

Z AXIS OF F

Z IRRADIATION

0 CAN 14.0 cm

Z5 8c9cm

> 2

0 -4

ca <

W BOTTOM OF LICA IRRADIATION BRASS CAN

Figure 3.3. Locations of thermoluminescent CaF 2 wafers

inside LICA irradiation can during dose rate

gradient mapping. CaF 2 wafers were placed at

Positions A. B. C. D. E. F. and G.

13
Table 3.1

Relative Dose Rate Gradients. R/RA. for Several

LICA Irradiation Positions. Measurement

Locations A-G are Shown in Figure 3.3.

LICA Position

Measurement

Location IIIC HID IVC IVD VC VD

A 1.00 1.00 1.00 1.00 1.00 1.00

B 0.97 1.14 1.01 1.03 1.09 0.92

C 0.69 0.77 0.96 0.98 1.37 1.32

D 0.93 0.83 0.91 1.02 1.02 0.95

E 1.29 1.27 0.96 1.08 0.83 0.76

F 1.05 1.04 0.94 0.94 1.04 0.95

G 0.93 0.85 0.92 0.96 1.06 0.90

14
A detailed sketch of a test cell is shown in Figure 3.4.

The cylindrical sample aging region (10 cm diameter and 23 cm

long) is located inside a brass can, which in turn is suspended from the lid of a double-walled stainless-steel can.

(The double-walled design provides some thermal insulation.)

When the stainless-steel lid is lifted free of the stainlesssteel can, a brass lid at the bottom of the brass can is

easily removed, allowing access to the sample aging region.

Figure 3.5 illustrates insulation specimens prepared to be

inserted into the sample aging region.

The sample region is heated using an insulated nichrome

wire wrapped around the sides of the brass can and also

around a pancake heater which lies between the brass can and

the stainless-steel lid. The auxiliary pancake heater was

found to be useful for reducing rather substantial temperature gradients at the top of the sample aging region caused

by the heat-sink effect of the massive top of the stainlesssteel can. To accurately control and monitor the temperature

in the sample region, two resistance temperature devices

(RTDs) were incorporated in the design. A control RTD is

directly clamped to the inside wall of the brass can and a

monitor RTD is positioned close to the center of the sampleaging region. A 2.9 cm OD plastic tube runs from the top of

the stainless-steel can up through the water tank. Lead

wires for the heater and the two RTDs feed through this tube.

In addition, a small tube inside the outer plastic tube is

used to circulate air or other gaseous environments past the

sample region at controlled flow rates. The temperature

capabilities of the test cells are room temperature to 150 0 C.

15
0

STEST

SPECIMENS

AIR DIFFUSION

PLATE .JtFigure 3.4. A LICA Irradiation Test Cell

16
Figure 3.5. EPR 1 and EPR 2 insulation specimens prepared

to be inserted into the sample aging-region of

a LICA irradiation test cell.

17
3.2 Thermal Aging Facility8

The Thermal Aging Facility uses air circulating ovens.

each modified to accommodate a number of self-contained aging

cells. A detailed sketch of one of these aging cells is

shown in Figure 3.6. It consists of a bell jar glass chamber

which rests on an aluminum stand. A gas inlet line enters

the sample aging region from the bottom through a hole in the

aluminum base. A small hole at the top of the glass chamber

serves as a gas exit and as a means of introducing a permanently positioned thermocouple into the center of the

sample region. Metal collars surrounding the glass bell jars

improve the thermal stability and reduce temperature gradients in the sample aging region. Sample holders fit inside

the glass chamber. The aging cells used for this test were

constructed in three sizes with internal volumes of .9 liter.

2.5 liters, and 3.9 liters.

18
,THERMOCOUPLE

GLASS CHAMBER 7/SAMPLE BASKET

/;/.ALUMINUM COLLAR

r-AMPLES

IJ

GAS INLET

I iLUMINUM A BASE

... ... LEGS

---- .

Figure 3.6. Oven Aging Cell

19
4.0 EXPERIMENTAL TECHNIQUES

4.1 U.S. Samples

The U.S. insulation and jacket samples were exposed to

five different aging procedures. These procedures (and the

shorthand codes used in the rest of the report to describe

them) are:

A = R7 0 -+ 120*C.: A 16-day irradiation at

-65 krd/h and 700C followed by a 16-day

thermal exposure at 120 0 C.

B = R27 -+ 120°C: A 16-day irradiation at

-65 krd/h and ambient temperatures (-270C)

followed by a 16-day thermal exposure at 1200C.

C = 120 0C -4 R7 0 : A 16-day thermal exposure at

1200C followed by 16-day irradiation at

-65 krd/h and 700C.

D = 120 0 C -+ R2 7 : A 16-day thermal exposure at

1200C followed by a 16-day irradiation at

-65 krd/h and ambient temperatures ( 27 0 C).

E = R1 2 0 : A 16-day simultaneous exposure to 120 0 C

thermal and -65 krd/h irradiation environments.

The 120 0 C. 16-day deviated temperature exposure was

chosen based on Arrhenius calculations which assumed a

40-year service operation at 45 0 C and cable material activation energy of 1.0 eV.

The insulation specimens were placed in sample fixtures

as illustrated by Figure 3.5. EPR 1 and EPR 2 samples were

irradiated together. Likewise. XLPO 1 and XLPO 2 samples

were irradiated together. The jacket specimens (CSPE and

CPE) were irradiated separately. During irradiations, air

flow to the 1.8 liter irradiation cell was approximately

40 cc/min.

For thermal aging, 0.9 liter thermal aging cells were

employed for the insulation specimens. Sample holders similar to those shown in Figure 5 (but smaller in diameter) were

used to support each individual insulation specimen. EPR 1.

EPR 2. XLPO 1. and XLPO 2 samples were each aged separately.

The jacket specimens were aged using the 2.5 liter thermal

aging cells. CPE and CSPE were thermally aged separately.

Air flow to the thermal aging cells was -20 cc/min for

both the insulation and jacket specimens. This corresponds to

20
.5 to 2 "complete" air changes an hour. The air flow removes

from the vicinity of the samples any thermal decomposition

products that are outgassed by the samples.

For each material, approximately 80 sample specimens

started each aging sequence. Several times during both the

irradiation and thermal exposures, aging was momentarily

interrupted to allow for removal of several sample specimens.

These specimens were used to determine the degradation history during the aging exposures. Midway during the irradia--

tion exposure, the sample cell was rotated -1800 to average radiation gradient effects. All samples pulled from the

cell prior to completion of the irradiation were removed

from the center of the cell. This minimized the effect of

radiation gradients on intermediate exposure results.

Table 4.1 summarizes the total radiation dose and the

thermal exposure time for each group of U.S. insulation and

jacket specimens.

Tensile tests were performed at Sandia National

Laboratories on the EPR 1, EPR 2, XLPO 1, XLPO 2, CSPEo and

CPE samples. For each experimental condition, three or four

samples were tested to determine the ultimate tensile

elongation, e. and the ultimate tensile strength, T.

Tensile measurements were performed at ambient temperatures

(-23 0 C) using Instron 1125 (EPR 2 specimens; aging

environments A. B. D. and E) and Instron 1130 machines (all

other specimens). Samples were gripped using pneumatic

jaws: initial jaw separation was 5.1 cm and samples were

strained at 12.7 cm/min. The strain was monitored with an

Instron electrical tape extensometer clamped to the sample.

The systematic difference in normalized elongation and

tensile strength due to the use of two different tensile

macchines was approximately 12%. Data obtained on the 1130

was higher than that obtained by the 1125.

Bend tests were performed on the TEFZEL 1 and TEFZEL 2

samples rather than tensile tests since aged specimen tubes

shattered when gripped by the pneumatic jaws of the Instron

tensile testing machine. Bend radii between 75 and 6 times

the radii of the TEFZEL specimens were employed. Each

specimen was successively wrapped around tubes of smaller

diameter until insulation cracking was visually observed.

21
The U.S. Compression Set Samples were exposed to three

different aging procedures. These procedures (and the

shorthand used in the rest of the report to describe them)

are:

R27 -* 120*C = A 16-day irradiation at -60 krd/h

and ambient temperatures (-270C) followed by

a 16-day thermal exposure at 120 0 C.

120 0 C R27 = A 16-day thermal exposure at 1200C

followed by a 16-day irradiation at -60 krd/h

and ambient temperatures (-27 0 C).

R20= A 16-day simultaneous exposure to 120 0 C

thermal and -60 krd/h irradiation environments.

The compression set samples were exposed using a fixture

as shown in Figure 4.1. Each layer of the fixture contained

three .127 + .001 cm spacers and four compression set

samples. Each of the five layers of one fixture was used for

a different compression sample material; namely EPR A. EPR

B. BUNA N. VITON, or SILICONE. Two sample fixtures were irradiated in an aging cell. The fixtures were oriented so

that the compression fixture surfaces were perpendicular to

the Cobalt-60 array (see Figure 4.2). Air flow to the irradiation cell was approximately 40 cc/min. Thermal aging

was performed using a 2.5 liter aging cell containing four

fixtures. Air flow to the thermal aging cell was also

40 cc/min. Table 4.2 summarizes irradiation doses and thermal aging times for each fixture.

The compression set samples ranged in thickness between

.165 and .205 cm. Prior to compression, each individual

sample was measured for thickness and its position in the

fixture noted. After exposures to radiation and thermal

environments, the sample thickness was again measured. Prior

to the final measurements, the fixture was disassembled

(releasing the compressive strain) and a 30-minute recovery

time allowed.

Our compression set samples have much smaller thicknesses

than those recommended by ASTM Standard D395-78. 9 This

Standard recommends (for Method B) test specimens with

1.25 cm thicknesses. Our sample thicknesses more realistically simulate use conditions, but generate much larger

errors in the calculated values for compression set.

Absolute error for our compression set values is + 0.1.

22
Table 4.1

Radiation Dose and Thermal Exposure Time

for U.S. Insulation and Jacket Specimens

Sample Group

XLPO 1A

XLPO 1B

XLPO iC

XLPO 1D

XLPO IE

XLPO 2A

XLPO 2B

XLPO 2C

XLPO 2D

XLPO 2E

EPR 1A

EPR lB

EPR 1C

EPR ID

EPR 1E

EPR 2A

EPR 2B

EPR 2C

EPR 2D

EPR 2E

CSPE A

CSPE B

CSPE C

CSPE D

CSPE E

CPE A

CPE B

CPE C

CPE D

CPE E

Total Radiation

Dose[Mrd(air equiv.)]

24.2*

24.2

23.4

23.1

24.3

22.7*

24.2

23.4

23.0

24.3

Thermal Exposure

Time (HRS)

385 hours

385 hours

384 hours

385 hours

386 hours

25.7

25.5

25.0

25.3

25.7

25.7

25.5

25.0

25.3

25.7

25.0

25.4

24.2

24.2

24.6

23.9

23.4

23.1

23.1

23.4

22.3

22.9

22.3

22.3

22.4

22.3

22.9

22.3

22.3

22.4

386

385

384

385

386

385

385

384

384

384

385

385

384

384

384

389

380

389

389

384

389

389

385

385

384

386

377

383

384

381

386

377

383

384

381

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

TEFZEL

TEFZEL

TEFZEL

TEFZEL

TEFZEL

TEFZEL

TEFZEL

TEFZEL

TEFZEL

TEFZEL

1A

1B

IC

ID

1E

2A

2B

2C

2D

2E

* XLPO 1A and XLPO 2A were irradiated separately.

23
A A

Figure 4.1. U.S. Compression Set Fixture

24
CO-60

Figure 4.2. Orientation of U.S. Compression Set

Fixtures in Radiation Field
Table 4.2

Radiation Doses and Thermal Aging Conditions

for Each U.S. Compression Set Fixture

Compression

Set Fixture

Total Dose

(Mrd)

Thermal Aging

Aainc Seauence Time (hrs)

#38

#12

#37

#32

#13

#14

#20

#50

Unaged NA NA

23.8 NA

120 NA

R27 4 120

R27 - 120

120 4 R27

120 - R27

22.9

23.8

23.8

23.4

23.0

386

382

386

386

386

386

4.2 French Samples

The French samples were exposed to four different aging

procedures. These procedures (and the shorthand codes used

in the rest of the report to describe them) are:

A = T 4 R70:

B = R7 0 4 T:

C = T 4 R27:

D = R2 7 4 T:

A 10-day thermal exposure followed by a

9- or 10-day irradiation at -115 krd/h

and 70 0 C.

A 9- or 10-day irradiation at -115 krd/h

and 70 0 C followed by a 10-day thermal

exposure.

A 10-day thermal exposure followed by a

9- or 10-day irradiation at -115 krd/h

and ambient temperatures (-27 0 C).

A 9- or 10-day irradiation at -115 krd/h

and ambient temperatures (~27 0 C)

followed by a 10-day thermal exposure.

The 10-day thermal exposure temperature depended on the

specimen material. Table 4.3 lists each of the French

26
Samples and the appropriate thermal aging temperature.

Various sample groups were irradiated over a several month

period. Co-60 decay during this time period necessitated

varying the irradiation exposure time from 9 days to 10 days

so that each sample group was irradiated to a similar dose

(-25 Mrd).

Table 4.4 summarizes the total radiation dose and the

thermal exposure time for each group of French samples. The

insulation specimens (82 Ii. 82 12. 82 19) were irradiated

and thermally aged using fixtures similar to that shown in

Figure 3.5. 82 Il and 82 12 samples were irradiated together

in the same aging cell. 82 19 samples were irradiated alone.

Air flow to each of the 1.8 liter irradiation cells was

-60 cc/min. Thermal aging of each group of insulation

specimens was performed separately using a 0.9 liter aging

cell and an air flow of -30 cc min. The 82 H5 samples were

irradiated as shown in Figures 4.3 through 4.5. Metallic

washers were used to keep each dumbbell separate from all

others. A similar arrangement was used for the 82 H6 samples

(but without the basket). Air flow to the irradiation chambers was -60 cc/min. The 82 H5 samples were thermally aged

using 0.9 liter thermal cells and ~30 cc/min air flow. The

82 H6 samples were thermally aged using 3.9 liter aging cells

and a -100 cc/min air flow. 82 H3, 82 H4, and 82 G10

dumbbells were assembled as shown in Figures 4.6 and 4.7 and

oriented for irradiation as shown in Figure 4.8. Air flow

to the 1.8 liter irradiation cell was -60 cc/min; air flow

to the 0.9 liter thermal aging cell -30 cc/min. The 82 J3

compression set assemblies were randomly placed in a basket

and irradiated as shown in Figure 4.9. The 82 J4 compression set assemblies were stacked in a basket and irradiated as shown in Figure 4.10.

Air flow to the 1.8 liter irradiation cell was -60

cc/min for the 82 J3 and 82 J4 samples. These samples were

therm- ally aged using 0.9 liter aging cells with an air

flow of -30 cc/min.

The ultimate tensile elongation, e. and ultimate tensile

strength, T. were measured at CEA-ORIS-LABRA in Saclay for

French elastomer samples 82 If. 82 12, 82 19, 82 H3, 82 H4,

and 82 G10. the thermoplastic material 82 H6. and the thermosetting material 82 H5. A ZWICK Model 7025/3 test machine.

located in a room with controlled temperature of 210 C. was

used for the tensile tests. Dumbbells and conductor insulation samples were gripped in the jaws of the test machine.

Initial spacing between the jaws was 40 mm for the 82 GIO.

82 H3, and 82 H4 dumbbells, approximately 150 mm for the

82 H5 and 82 H6 dumbbells, and on the average 110 mm for the

27
82 I1, 82 12. and 82 19 insulation specimens. An extensometer was located at the center of each test piece. Its gap

was 10.0 mm. The strain rate was 50 mm per minute.

Compression set measurements were performed at

CEA-ORIS-LABRA in Saclay for French elastomer samples 82 J3

and 82 J4.

Table 4.5 summarizes the accuracy of the French measurements. Each measurement is made on five test pieces. If a

measurement showed excessive discrepancy from the average it

was rejected and a new average was computed.

28
Table 4.3

Thermal Exposure Temperatures For French Samples

Sample

Description

1. PRC Insulation

2. EPDM Insulation

3. EPDM Insulation

4. PPS Dumbbells

5. Polydiallylphtalate

Dumbbells

6. VAMAC Acrylic

Polyethylene

Dumbbells

7. EPR Dumbbells

8. HYPALON Dumbbells

9. VAMAC Acrylic Polyethylene O-ring

seal samples

10. EPR O-ring seal

samples

Sample

Code

82 II

82 12

82 19

82 H6

82 HS

82 H3

Exposure

Temperature (OC)

140

140

140

160

160

120

140

140

120

82

82

82

H4

GIO

J3

82 34 140

29
Table 4.4

Total Radiation Dose and the Thermal Exposure Time

for Each Group of French Samples

Radiation Exposures

Radiation

Dose

Thermal Exposure Time

82 IIA

B

C

D

82 12A

B

C

D

82 19A

B

C

D

82 H6A

B

C

D

82 H5A

B

C

D

82 H3A

B

C

D

82 H4A

B

C

D

82 G1OA

B

C

D

24.7

24.7

24.7

24.9

24.7

24.7

24.7

24.9

24.0

25.3

23.9

25.6

26.0

26.0

25.8

26.2

24.1

24.6

23.8

24.0

25.4

25.4

25.4

25.4

25.1

25.1

24.9

24.9

25.5

25.5

24.4

24.4

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

Mrd

240.5

240.2

240.5

240.2

240.5

240.2

240.5

240.2

258.5

238.8

258.5

241.1

238.6

238.7

238.6

238.7

240.2

238.6

240.2

241.0

240.0

240.2

240.0

240.2

258.5

268.8

258.5

268.8

239.0

243.9

239.0

243.9

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

hours

30
Table 4.4 (Continued)

Total Radiation Dose and the Thermal Exposure Time

for Each Group of French Samples

Radiation Exposures

Radiation

Dose

Thermal Exposure

Time

82 J3A

B

C

D

82 J4A

B

C

D

25.4 Mrd

25.4 Mrd

24.5 Mrd

24.5 Mrd

24.0 Mrd

24.6 Mrd

24.1 Mrd

24.3 Mrd

240.0 hours

241.3 hours

240.1 hours

240.2 hours

245.5 hours

243.9 hours

245.5 hours

239.0 hours

31
Figure 4.3. 82 H5 and 82 H6 Samples Prepared for Aging

32
Figure 4.4. 82 H5 Samples Prior to Insertion into LICA

Irradiation Cell

33
Co--60

Figure 4.5. Orientation of 82 H5 and 82 H6 Samples

During Irradiation

34
Figure 4.6. Preparation of 82 H3, 82 H4, and 82 G10

Samples for Aging

35
Figure 4.7. 82 H3, 82 H4. and 82 G10 Samples Shown as

Prepared to be Inserted into LICA

Irradiation Cell

36
Co-60

Figure 4.8. Orientation of 82 H3, 82 H4, and 82 GI0

Samples During Irradiation

37
Figure 4.9. 82 J3 Samples Prepared to be Irradiated

38
CO-60

Figure 4.10. Irradiation Aging Configuration Used for

82 J4 Samples

39
Table 4.5

Accuracy of French Measurements

Measured Parameter Accuracy

Dimensions

Dumbbell Size

Insulation Outer Diameter

Insulation Inner Diameter

Wire Thickness

Tensile Strength

Dumbbells

Conductor Insulation

Tensile Elonqation

+ 0.1 mm

+ 0.5 mm

+ 0.3 mm

+ 0.2 mm

+ 5%

+ 15%

Dumbbells

Conductor Insulation

Compression Set (Permanent Set)

+ 5%

+ 5%

+ 9%

40
5.0 RESULTS

5.1 U.S. Samples

Sequential exposures to irradiation and thermal environments were employed for aging sequences A. B, C, and D

(Section 4.1). Each environmental exposure lasted for -380

hours (Table 4.1). Thus the total sequential exposure time

for both the irradiation and thermal aging environments was

-760 hours. Several times during this 760-hour exposure

period, aging was momentarily interrupted to allow for removal

of several sample specimens. These specimens were used to

determine the degradation history during the aging exposures.

In this section we plot tensile property degradation versus

exposure time for the CSPE, CPE, EPR 1, EPR 2. XLPO 1, and

XLPO 2 materials. For each aging sequence, the first 380

hours of our plots represents one of the environmental stress

exposures (irradiation or thermal), while the second 380 hours

represents the second environmental stress exposure of the

sequence. Aging exposure E was a simultnaeous exposure to

irradiation and 1200C thermal environments. It lasted -380

hours (see Table 4.1). Tensile property degradation during

the E aging exposure is also shown in our figures.

5.1.1 CSPE and CPE Jacket Materials

The ultimate tensile properties of CSPE and CPE depended

on the order of the sequential exposures. Figures 5.1 and

5.2 illustrate tensile property degradation of CSPE as a

function of exposure time to radiation and thermal environments. The R7 0 -' 120 0 C exposure most severely degrades

both the ultimate tensile elongation and the ultimate tensile

strength. The R1 2 0 exposure yields comparable results.

The 120C -+ R2 7 sequence is the least degrading sequence.

For CSPE, jacket degradation during sequential sequences

depends on whether the irradiation is performed at ambient or

700C temperatures; 700C irradiations are more severe.

CPE elongation degradation does not depend on irradiation

temperatures (see Figure 5.3). The R -+ 120 sequences produces more elongation degradation than does the 120 -ý R

sequence or the R1 2 0 simultaneous exposure. Ultimate tensile strength results, Figures 5.4 and 5.5. indicate that

thermal exposures reduce tensile strength while ambient

irradiation exposures increase tensile strength. Irradiation

exposures at elevated temperatures do not strongly affect

CPE's tensile strength properties.

41
1.2

1.0

0.8

e/e0

0.6

0.4

0.2

0.0-

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.1. Ultimate Tensile Elongation of CSPE in Various

Environments. Sample tensile elongation divided

by initial (unaged) elongation is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

42
1.2

lO

0.8

T/To "

0.6

0.4 CSPE

*=A:

o=B:

0.2- O=C: t=D:

EI=E:

0.0 - I - 0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.2. Ultimate Tensile Strength of CSPE in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

43
1.2

1.0

0.8

0.6

0.4

0.2

0.0

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.3. Ultimate Tensile Elongation of CPE in Various

Environments. Sample tensile elongation divided

by initial (unaged) elongation is plotted-versus

aging time. Each portion of the sequential

exposures lasted ~380 h.

44
a

T

1.8 1 1 1 1 1

CPE

1.6 O=B: R2 7 -.- T I A,= D : T'RR2 I

EI= E :R120

1.4

/To 1.2-

1.0 -

0.8

0.6-

I I I I I II

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.4. Ultimate Tensile Strength of CPE in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted -versus

aging time. Each portion of the sequential

exposures lasted -380 h.

45
1.8

1.6

1.4

T/To 1.2

1.0 -

0 1

0.8- I

0.6 1

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.5. Ultimate Tensile Strength of CPE in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted -versus

aging time. Each portion of the sequential

exposures lasted -380 h.

46
For some CPE samples, irradiations were terminated when

our irradiation cells mistakenly filled with water. The

exposure sequence was restarted with new samples. Figures

5.6 and 5.7 demonstrate tensile property results for the two

sets of exposures: one sequence successfully completed, the

other identical sequence terminated prior to completion. The

data illustrates the extent of repeatability of results.

5.1.2 EPR Insulation Materials

Ultimate tensile property degradation for EPR 1, a radiation cross-linked FR-EPDM° is illustrated in Figures 5.8 and

5.9. Irradiation reduces both the ultimate tensile elongation and ultimate tensile strength. Degradation is worst for

the R2 7 exposure, with lesser degradation noted for the

R7 0 and R1 2 0 irradiations. The opposite effect is noted

for EPR 2, a chemically cross-linked FR-EPDM (Figures 5.10

and 5.11). For this material, the R1 2 0 and R70 irradiations more degrade the EPR tensile properties than does the

R27 exposure. When irradiation and thermal stresses are

applied sequentially, neither EPR 1 nor EPR 2's ultimate

tensile elongation properties depended on the sequential

ordering. EPR 1 and EPR 2 tensile strength properties are

also not affected by sequential ordering.

5.1.3 XLPO Insulation Materials

XLPO 1 and XLPO 2 tensile properties are illustrated in

Figures 5.12-5.15. Only the ultimate tensile strength of

XLPO 2 was sensitive (mildly) to sequential ordering of

radiation and thermal stresses. The R 4 T sequences

increased the tensile strength more than did the T - R

sequences.

5.1.4 TEFZEL Materials

Tables 5.1 and 5.2 present bend test results for TEFZEL

1 and 2 respectively. Four specimens (two white and two

colored) were tested for each aging condition. If all four

samples passed the bend test, a P is shown in the table.

Those table locations where samples failed the bend test are

marked with an F. TEFZEL degradation is clearly dependent

on irradiation temperature. We experienced no bend test

failures for TEFZEL specimens aged using ambient temperature irradiations. We did observe bend test failures when aging

procedures employed either 700C or 1200C irradiations. For

both TEFZEL materials, the 1200C -> R70 sequence was more

severe than the R7 0 -> 1200C exposure.

47
1.2

1.0

0.8

e/eo

II I I I I

CPE

0= R2 7 EXPOSURE #1

0= R27 EXPOSURE #2

I I I t I I

0.6

0.4

0.2

0.01) 100 200 300 400 500 600 700 800

TIME (hours)

Figure 5.6. Repeatability of Ultimate Tensile Elongation

Results for CPE During Two R2 7 Exposures

48
1.4

1.3

1.2

1.1

I

CPE

0 = R2 7

* = R2 7

I I I I I

EXPOSURE #1

EXPOSURE #2

*140

T/To I

0 f

1.0

0.9

0.80 I I Ia I I I I I

100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.7. Repeatability of Ultimate Tensile Strength

Results for CPE During Two R2 7 Exposures

49
1.2

e/eo

1.0

0.8

0.6

0.4

.0.2

0.0 0.1O 0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.8. Ultimate Tensile Elongation of EPR 1 in Various

Environments. Sample tensile elongation divided

by initial (unaged) elongation is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

50
T/To

1.4

1.2

1.0

0.8

0.6

0.4

0.2

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.9. Ultimate Tensile Strength of EPR 1 in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

51
1.2

1.0

0.8

e/e0

0.6

0.4

0.2-

0.00 1- 0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.10. Ultimate Tensile Elongation of EPR 2 in Various

Environments. Sample tensile elongation

divided by initial (unaged) elongation is

plotted versus aging time. Each portion of the

sequential exposures lasted -380 h.

52
1.4

1.2

1.0

T/To

0.8

0.6

0.4

0.2-

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.11. Ultimate Tensile Strength of EPR 2 in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

53
1.2

1.0

0.8

e/0o

0.6-

0.4

0.2

0.0 -

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.12. Ultimate Tensile Elongation of XLPO 1 in

Various Environments. Sample tensile elongation divided by initial (unaged) elongation is

plotted versus aging time. Each portion of the

sequential exposures lasted -380 h.

54
1.4

1.2

1.0

T/T 0

0.8-

0.6

0.4

0.200 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.13. Ultimate Tensile Strength of XLPO I in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

55
e/eo

1.4

1.2

1.0

0.8

0.6

0.4

0.2

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.14. Ultimate Tensile Elongation of XLPO. 2 in

Various Environments. Sample tensile elongation divided by initial (unaged) elongation is

plotted versus aging time. Each portion of the

sequential exposures lasted -380 h.

56
1.4

1.2

1.0

T/To0. 0.8-

0.6

0.4-

0.2

0 100 200 300 400 500 600 700 800 900

TIME (hours)

Figure 5.15. Ultimate Tensile Strength of XLPO 2 in Various

Environments. Sample tensile strength divided

by initial (unaged) strength is plotted versus

aging time. Each portion of the sequential

exposures lasted -380 h.

57
Table 5.1

Bend Test Results for TEFZEL 1

Bend Radius/Insulation Radius

75X 69X

F:

B:

D:

A:

C:

E:

Unaged P

R2 7-4120 P

120-+R2 7 P

R7 0-+120 P

120+R7 0 P

R120 P

P = Pass Bend Test

F = Fail Bend Test

P

P

P

P

P

P

56X 50X 44X 31X

P P P P

P P P P

P P P P

P P P P

P P P F

P P F F

22X l1X 6X

P

P

P

F

F

P

P

P

F

P

P

P

F

F

58
Table 5.2

Bend Test Results for TEFZEL 2

Bend Radius/Insulation Radius

75X 69X 56X 50X 44X 31X 22X 1iX 6X

F: Unaged P P P P P P P P P

B: R2 7 4120 P P P P P P P P P

D: 1204R2 7 P P P P P P P P P

A: R7 0 4120 P P P P P P F F

C: 1204R7 0 P P P F F

E: R1 2 0 P P P. P P P F F

P = Pass Bend Test

F = Fail Bend Test

59
5.1.5 Compression Set Tests

Our compression set tests employed compression samples

with thicknesses -. 18 cm. As mentioned in Section 4, this

thickness represents actual use conditions but produces large

uncertainties in the value of compression set, C:

t - ti o - to -tn

where to = original thickness

ti= final thickness

tn= compressed thickness.

We predict our absolute uncertainties for C to exceed

.10. For all five materials, our uncertainty exceeds the

compression set variation caused by aging differences. (See

Table 5.3.)

5.2 French Samples

Each French aging sequence included two environmental

stress exposures - an irradiation exposure and a thermal

aging exposure. Mechanical tensile tests and compression set

measurements were performed at the completion of each exposure. Results are presented in Table 5.4.

Measurement results are shown for each material in

Figures 5.16 through 5.24. Measurement values are normalized

with respect to those relating to unaged control specimens

of the same material (blank samples U). For each aging sequence, usually two data values are plotted. The first value

reflects test results at completion of the first exposure of

the aging sequence, while the second value indicates results

at the completion of the aging exposure. For a few test

conditions, only data at the completion of the sequence were

obtained. This single data value is plotted.

60
Table 5.3

U.S. Compression Set Test Results

EPR A EPR B BUNA A SILICONE VITON

Unaged (#38)

Partially Aged:

R2 7 (#12)

120 (#37)

Aged:

R1 20 (#32)

R27 -ý 120

#13

#14

120 -3 R2 7

#20

#50

.09 + .01

.54 + .04

.31 + .07

.74 + .03

.67 + .02

.67 + .03

.68 + .04

.79 + .06

.11 + .02

.78 + .03

.73 + .05

1.0

.96 + .03

.98 + .03

.91 + .02

.95 + .01

.07 + .01

.48 + .01

.39 + .02

.68 + .01

.63 + .01

.59 + .02

.68 + .02

.71 + .02

.07 + .03

.82 + .02

.17 + .01

1.0

.83 + .02

.86 + .01

.72 + .01

.81 + .01

.17 + .01

.80 + .05

.27 + .03

.97 + .02

.88 + .01

.89 + .01

.80 + .01

.83 + .02

*Errors Reflect + a for Four Samples. Absolute Error is + .10.

61
Table 5.4

Tensile and Compression Set Results for French Samples

MATERIAL

Elastomeric

9 TESTS" U * *

Materials:

PRC 140 T 1.3 1.1 1.2 1.1 0.9 1.1 1.1 1.0 1.0

82 I1 e 370 332 267 264 30 332 269 245 43

EPDM 140 T 0.6 0.6 0.3 0.4 0.4 0.6 0.5 0.4 0.2

82 12 e 240 241 82 124 1.5 241 118 135 0.5

Fire-proof

EPDM 140 T 0.6 0.6 0.7 0.7 0.4 0.6 0.8 0.7 0.4

82 19 e 245 222 83 113 32 222 84 107 34

EPR 140 T 1.7 1.5 1.3 1.5 0.8 1.5 1.4 1.6 0.8

82 H4 e 174 186 99 124 81 186 93 116 73

EPR 140 Compres- 8.2 67 -- 71 -- 58 -- 57

sion

82 J4 Set

VAMAC 120 1.8 1.7 1.8 1.8 1.8 1.7 1.8 1.8 1.8

82 H3 312 308 245 248 238 308 207 217 215

VAMAC 120 Compres- 9.6 -- 56 -- 71 -- 68 64 76

Sion

82 J3 Set

HYPALON

52 tC10

140 T 0.9 0.7 0.7 0.6 0.7 0.7 0.8 0.7 T .~ . - _ _

B A22 249 205 332 204 28A 214

Thermoplastic material:

PPS 160 IT 1 8.7 _8.0 8.4 8.1 8.0 8.4 7.8

82H e 0.7 1 0.6 1 0.7 10.7 1 0.6 1 0.7 1 0.

Thermoset material:

Polydiallylphtalate 160 T 4.6 4.5 4.8 4.4 5.0 4.5 4.8 4.6 4.7

82 H5 I ] 10.3 10.4 0.3 0.3 10.310.40.3 0.4 0.3

*Code - U = Blank sample

A = Thermal aging at 9*C, followed by irradiation at 70*C

B = Irradiation at 700C, followed by thermal aging at 8"C

C = Thermal aging at G*C, followed by irradiation at 27*C

D = Irradiation at 270C, followed by thermal aging at 8°C

0 = Thermal aging temperature

* T = ultimate tensile strength (Units = 10 MPa)

e = ultimate tensile elongation (units = %)

*** First column = Results at completion of first exposure of the sequence

Second column = Results at completion of second exposure of the sequence

62
5.2.1 PRC (82 If)

Figure 5.16 illustrates the normalized tensile properties

for chemically cross-linked polyethylene (PRC). The order

of aging exposures does not seem to affect the tensile

strength. The deviation of the measured data from the

average value is + 10 percent. which is not significant.

However, tensile elongation is influenced by sequential

exposure order to a much greater extent than the tensile

strength. The PRC material is strongly degraded by the irradiation then thermal exposure sequences (sequences B and

D), whereas degradation is slight for the thermal exposure

then irradiation sequences (sequences A and C). In all

cases, irradiation at 700C or 270C causes identical changes

in tensile strength or tensile elongation, with or without a

prior thermal exposure at 1400C.

5.2.2 EPDM (82 12 and 82 19)

Samples 82 19 are fire-proof EPDM material, whereas the

82 12 samples are not. Figure 5.17 illustrates measurement

results for 82 12, while Figure 5.18 presents results for

82 19.

5.2.2.1 EPDM (82 12)

When irradiation is performed at 700C, the order of aging

exposures does not affect the tensile strength (within

measurement accuracy of + 15 percent - see Table 4.5). At

270C however, the irradiation followed by thermal exposure

sequence (exposure sequence D) degrades the tensile strength

more than does the thermal followed by irradiation sequence

(exposure sequence C). Hence for tensile strength behavior

of the 82 12 material, irradiation temperature is important.

Ultimate tensile elongation is more degraded by the irradiation followed by thermal exposure sequences (sequences

B and D).

5.2.2.2 Fire-proof EPDM (82 19)

Both thermal followed by irradiation sequences (A and C)

increased the tensile strength, whereas both irradiation

followed by thermal sequences (B and D) decreased the tensile

strength. Interestingly, for both of these latter sequences

(B and D), the irradiation exposures at 70.C and 272C increased the tensile strength, contrary to the behavior of the

82 12 EPDM samples when irradiated. For all sequences.

elongation was decreased. The material appears to become

reticulated during aging exposures.

63
ULTIMATE

TENSILE STRENGTH

1.0

T/To

U A B C D

ULTIMATE

TENSILE ELONGATION

1.0 i- 0 9

9 0 9 0/00

QI

9

U A B C D

U = UNAGED

A= 140-,R 7 0

C = 140--,R2 7

D = R2 7 -140

B = R7 0 -- 140

Figure 5.16. Ultimate Tensile Properties for PRC (82 I1)

64
ULTIMATE

TENSILE STRENGTH

1.0

T/To

1.0

6/80

U A B C D

ULTIMATE

TENSILE ELONGATION

U A B C D

U =UNAGED

A = 140---R7 o

B =R17 0 -0-140

C = 140-0-112 -

D = R2 7 -- 140

Figure 5.17. Ultimate Tensile Properties for EPDM (82 12)

65
ULTIMATE

TENSILE STRENGTH

1.0

T/To

U A B C D

ULTIMATE

TENSILE ELONGATION

1.0 c

0 0

6/00

I I I IT

U A B C D

U = UNAGED

A= 140--R 7 0

B= R7 0 -,-140

C = 140--'R2 7

D = R2 7 -- 140

Figure 5.18. Ultimate Tensile

EPDM (82 19)

Properties for Fire-proof

66
5.2.3 EPR (82 H4 and 82 J4)

The same EPR material was used to make 3 mm-thick sheets

of EPR and also O-ring seals. Dumbbells (82 H4) as shown in

Figure 2.1 were cut from the sheets and used for ultimate

tensile strength and ultimate tensile elongation measurements. O-ring seals (82 J4) with an inner diameter of 12 mm

and an outer diameter of 17 mm were supplied by the same

manufacturer as the sheet EPR material. These were used for

compression (permanent) set measurements. Ultimate tensile

measurement results for the 82 H4 samples are shown in

Figure 5.19. Permanent set after compression measurements

for the 82 J4 samples are illustrated in Figure 5.20.

For the 82 H4 tensile specimens, irradiation at 270C and

at 700C have the same effect on ultimate tensile

properties. Identical changes in tensile strength and

tensile elongation were observed for the two thermal

followed by irradiation sequences (A and C). A similar

observation is relevant for the two irradiation followed by

thermal exposure sequences (B and D).

The effect of irradiation is more substantial for ultimate tensile elongation than for ultimate tensile strength.

Both the 27°and 700C irradiations reduced the tensile

elongation by -30 percent whereas the tensile strength was

only reduced by 10-20 percent.

There are only slight differences in permanent set caused

by the different aging sequences (Figure 5.20).

5.2.4 VAMAC (82 H3 and 82 J3)

The same VAMAC material was used to make 3 mm-thick

sheets of VAMAC and also O-ring seals. Dumbbells (82 H3) as

shown in Figure 2.1 were cut from the sheets and used for

ultimate tensile strength and ultimate tensile elongation

measurements. O-ring seals (82 J3) were used for compression

(permanent) set measurements. Ultimate tensile measurement

results for the 82 H3 samples are shown in Figure 5.21.

Permanent set after compression measurements for the 82 J3

samples are illustrated in Figure 5.22.

For the 82 H3 tensile specimens, irradiations at 270C and

at 70 0C have the same effect on ultimate tensile properties.

The material tensile properties are also unaffected by the

order of the aging sequence. Both the tensile strength and

the tensile elongation are unaffected by the thermal aging

67
exposure. Only the irradiation exposure changed the tensile

properties of VAMAC.

There are only slight differences in permanent set caused

by the different aging sequences (Figure 5.22).

5.2.5 HYPALON (82 G1O)

An electric cable was stripped of its HYPALON jacket.

(HYPALON is the trade name of Dupont for CSPE.) Dumbbells

as shown in Figure 2.1 were cut from the material and used

for ultimate tensile strength and ultimate tensile elongation

measurements.

For this material (Figure 5.23). irradiations at 27 0 C and

at 700C have the same effect on ultimate tensile

properties. Changes in ultimate tensile strength and

elongation are also independent of the order of the aging

exposures (irradiation and thermal).

5.2.6 PPS (82 H6)

Phenylene polysulfide (PPS) dumbbells as shown in Figure

2.3 were injection molded by the material manufacturer. The

effects of aging sequences on this material's ultimate

tensile properties are shown in Figure 5.24. This material

is highly resistant to aging. Its mechanical properties are

so little affected by the aging sequences that it is

difficult to detect any meaningful differences between the

various aging sequences.

5.2.7 Polydiallylphtalate (82 H5)

Polydiallylphtalate dumbbells as shown in Figure 2.3 were

molded by the material manufacturer. The effects of aging

sequences on this material's ultimate tensile properties are

shown in Figure 5.25. The first aging exposure (1600C thermal exposure or 27 0 C irradiation) results in an increase in

tensile elongation, possibly caused by lengthening of the

macro-molecular chains. Irradiation at 700C does not increase the elongation. The second aging exposure of the

aging sequence (either irradiation or thermal exposures)

causes an increase in ultimate tensile strength and a reduction in ultimate tensile elongation. This possibly reflects

additional cross linking of the material. For polydiallylphtalate. the order of the aging sequence does not affect the

ultimate tensile properties.

68
ULTIMATE

TENSILE STRENGTH

1.0

I

0 0 0 0 0 ?

- . - . - a ~* I

- a - a ~. I

U A B C D

ULTIMATE

TENSILE ELONGATION

0 C) 1.0O %.

- a ,a'

0

0/00 ?

~a. I - I

- ____________

I I

U A B C D

U = UNAGED

A = 140-,- R7 0

C = 140-.-R2 7

D = R2 7-- 140

1B = RRto -w-140

Figure 5.19. Ultimate Tensile Properties for EPR (82 H4)

69
PERMANENT SET

AFTER COMPRESSION

1.0

~2~~~ TI

U A B C D

U =UNAGED

A= 140-R 70

B = R7 0 --- 140

C= 140-a-R 2 7

D =R 2 7 -e140

Figure 5.20. Permanent Set After Compression for EPR (82 J4)

70
ULTIMATE

TENSILE STRENGTH

1.0

T/T 0

aa*a~u *ma5

U A B C D

1.0

0/eo -I

ULTIMATE

TENSILE ELONGATION

0

9 0

0 0 0)

- a - a - a - a. a U U a a

U A B C D

U = UNAGED

A = 120-,-RTO

C =120-s-112 1

D = 1 2 -.10420

B =R 7O--120

Figure 5.21. Ultimate Tensile Properties for VAMAC (82 H3)

71
PERMANENT SET

AFTER COMPRESSION

1.0

m

U A B C D

U = UNAGED

A = 120-- R7 0

B =R 7 0 -- 120

C = 120--R 2 7

D =R27-a120

Figure 5.22. Permanent Set

(82 J3)

After Compression for VAMAC

72
ULTIMATE

TENSILE STRENGTH

1.0

T/To

U A B C D

ULTIMATE

TENSILE ELONGATION

1.0

0 I

9

I I I

U A B C D

U UNAGED

A = 140--R7 0

B =R 7 0 -- 140

C = 140-,--R2 7

D =R 2 7 -- 140

Figure 5.23. Ultimate

(82 G1O)

Tensile Properties for HYPALON

73
ULTIMATE

TENSILE STRENGTH

1.0

T/To

1.0

0/00

U A B C D

ULTIMATE

TENSILE ELONGATION

o 'ii Q

U A B C D

U = UNAGED

A= 160- R7 0

B =R70--160

C = 160--R2 7

D =R 2 7 --160

Figure 5.24. Ultimate Tensile Properties for PPS (82 H6)

74
ULTIMATE

TENSILE STRENGTH

1.0

T/To

U A B C D

ULTIMATE

TENSILE ELONGATION

0 0 0

1.0

0/00

--I?- -0--

U A B C D

U = UNAGED

A = 160-,- R 0

B = R 70 -'-160

C =160-aRi 7

D = Rg7 -o'-160

Figure 5.25. Ultimate Tensile

phtalate (82 HS)

Properties for Polydiallyl75
6.0 CONCLUSIONS

As part of a joint French/U.S. sponsored research program, we are investigating the influence of testing conditions on the behavior of polymer materials. In this report

we have summarized the response of several commercial insulation and jacket materials, compression and gasket materials,

and thermosetting and thermoplastic materials to various

aging environments.

Ultimate tensile properties measured during our aging

exposures exhibited several general trends:

1. If sequential ordering of irradiation and thermal

exposures was important to the aging degradation of

tensile properties, usually the irradiation followed

by thermal exposure sequence was most severe.

Examples are elongation and tensile strength for

CSPE. CPE, EPDM (82 12 and 82 19). and elongation for

PRC (82 Il). A counter example is TEFZEL 2 which was

more degraded by the thermal followed by the 700 C

irradiation exposure rather than the reverse

sequence. The observation that irradiation followed

by thermal exposures is the more severe sequence is

consistent with previously published results for low

density polyethylene (LDPE) and polyvinylchloride

(PVC).2 Neither LDPE nor PVC materials were

included in this study.

2. During the sequential irradiation and thermal exposures, we performed irradiations at both ambient

(-270C) and 70 0 C temperatures. In general, the

choice of irradiation temperature was secondary to

the choice of aging sequence in its effect on polymer properties. Irradiation temperature did influence the degradation behavior of some materials.

Examples are bend test results for TEFZEL 1 and

TEFZEL 2. elongation and tensile strength data for

CSPE, tensile strength data for EPR 2, and tensile

strength data for EPDM (82 12).

3. For several materials, tensile properties at completion of aging were only slightly affected by both

the irradiation temperature and the order of the

sequential aging environmental exposures. Examples

are XLPO 1, VAMAC (82 H3), PPS (82 H6), and

polydiallylphtalate (82 H5).

76
In addition to tensile measurements, we performed permanent set after compression measurements for several gasket

and O-ring seal materials. At most, only slight differences

in permanent set were noted as a result of the various aging

techniques.

REFERENCES

1. Gillen. K. T.. Clough, R. L., Ganouna-Cohen. G..

Chenion. J.. and Delmas. G.. "The Importance of Oxygen

in LOCA Simulation Tests." Nuclear Engineering and

Design. 74 (1982). pgs. 271-285.

2. Clough, R. L. and Gillen, K. T.. "Radiation-Thermal

Degradation of PE and PVC: Mechanism of Synergism and

Dose Rate Effects." NUREG/CR-2156. SAND80-2149, June

1981.

3. Fremont. Ph., "Specification Generale pour la Qualification des Materiels Class 1E des Centrales Nucleaires a

eau sous pression," Electricite de France document.

HM/63-7195/6, July 1983.

4. Nuclear IEEE Standards, Published by the Institute of

Electrical and Electronics Engineers, Inc.

5. 1OCFR50.49 "Environmental Qualification of Electric

Equipment Important to Safety for Nuclear Power Plants."

Nuclear Regulatory Commission, Federal Register. Vol. 48.

No. 15, 2729. January 21. 1983.

6. Szukiewicz, A. J.. "Interim Staff Position on Environmental Qualification of Safety-Related Electrical Equipment -- Including Staff Responses to Public Comments."

NUREG-0588, Rev. 1, U.S. Nuclear Regulatory Commission,

Washington, DC, July 1981.

7. IEEE Standard 323-1974, "IEEE Standard for Qualifying

Class 1E Equipment for Nuclear Power Generating

Stations." 1974.

8. The description of the thermal and radiation aging

facilities is a modified, updated version of the description that was provided by: Gillen, K. T., Clough.

R. L.. and Jones, L. H.. "Investigation of Cable Deterioration in the Containment Building of the Savannah

River Nuclear Reactor." NUREG/CR-2877. SAND81-2613,

August 1982.

9. ASTM D 395-78. An American National Standard.

77

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1234

1800

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2155

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6300

6400

6410

6420

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6440

6442

6444

6445

6445

6445

6446

6446

6446

6446

6446

6446

6447

6449

6450

6450A

6452

8214

3141

3151

C. Yonas

J. Chang/G. J. Lockwood

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D. A. Dahlgren

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S. L. Thompson

B. E. Bader

L. D. Bustard (24)

C. M. Craft

L. L. Bonzon (20)

W. H. Buckalew

J. W. Grossman

D. B. Hente

F. V. Thome

F. J. Wyant

D. L. Berry

K. D. Bergeron

J. A. Reuscher

J. Bryson

M. Aker/J. S. Philbin

N. A. Pound

C. M. Ostrander (5)

W. L. Garner

DIST-4
UU 3U NUCLEAR REGULATORY COMMISSION I PEPORT NUMBER fAX#ftW , yrIC. OW Vo" IO 4 any,,)

BIBLIOGRAPHIC DATA SHEET NUREG/CR-3629- SAND83-2651

1;LIN-0 D*01-

3 TITLE AND SU"TITLE 4 RECIPIENT S ACCESSION NUMBER

The Effect of Thermal and Irradiation Aging 5 DATE REPORT COMPLETEC

Simulation Procedures on Polymer Properties MONTH YEAR

6 AUT.4OISI 7 DATE REPORT ISSUED

L. D. Pustard F. Carlin M. LeMeur IONTM VIAA

E. Minor C. Alba February 1984

J. Chenion G. Gaussens , PROJECT TASKIWORK UNIT NUMBER

S PERFORMING ORGANIZATION NAME AND MAILING ADDRESS I.,cludt iZe CeO&

Sandia National Laboratories

Albuquerque, New Mexico 87185 tO FIN NUMBER

A1051

11 SPONSOiRING ORGANIZATION NAME AND MAILING ADDRESS (Ifte..Ae ZP Ce0*) 12@ TYPE OF REPORT

Electrical Engineering Branch

Division of Engineering Technology

Office of Nuclear Regulatory Research 12 PERIOD COVERED iclus,,•,

U. S. Nuclear Regulatory Commission

Washington, D.C. 20555 March 1982-March 1984

13 SUPPLEMENTARY NOTES

14 ABSTRACT 0O0 m ;cW 9, AIt.)

Prior to initiating a qualification test on

safety-related equipment, the testing sequence for thermal

and irradiation aging exposures must be chosen. Likewise.

the temperature during irradiation must be selected.

Typically. U.S. qualification efforts employ ambient

temperature irradiation while French qualification efforts

employ 706C irradiations. For several polymer materials.

the influence of the thermal and irradiation aging sequence

as well as the irradiation temperature (ambient versus 70C)

has been investigated in preparation for Loss-of-Coolant

Accident simulated tests.

Ultimate tensile properties at completion of aging are

presented for three XLPO and XLPE. five EPR and EPDM. two

CSPE (HYPALON). one CPE. one VAMAC. one polydiallylphtalate.

and one PPS material.

Bend test results at completion of aging are presented

for two TEFZEL materials.

Permanent set after compression results are presented for

three EPR. one VAMAC. one BUNA N. one Silicone. and one Viton

material.

le KEY WORDS AND OOCUMEN7 ANALYSIS it5b DESCRIPTORS

IS AVAIL. AILIIY STATEMENT I7 I EC~JR 17Y CLASS F ICATION i1s NUMBER OF PAGES

GPO Sales I¶ M71 assifiedI 81

Unlimited NTIS 19 SECURITY CLASSIFICATION 12 PRICE

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[• Sandia National Laboratories