filii^iiiiliiliiilii ill ill AlllDS lSbl73 PUBLICATIONS

United States Department of Commerce

Technology Administration

National Institute of Standards and Technology

NIST BUILDING SCIENCE SERIES 176

Performance of Tape-Bonded Seams of EPDM

Membranes: Effect of Material and Application

Factors on Peel Creep-Rupture Response

Walter J. Rossiter, Jr., Mark G. Vangel, Kevin M. Kraft, and James J. Filliben

NIST BUILDING SCIENCE SERIES 176

Performance of Tape-Bonded Seams of EPDM

Membranes: Effect of Material and Application

Factors on Peel Creep-Rupture Response

Walter J. Rossiter, Jr.

Building and Fire Research Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

Mark G. Vangel

Statistical Engineering Division National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

Kevin M. Kraft

Building and Fire Research Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

James J. Filliben

Statistical Engineering Division National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

May 1997

U.S. Department of Commerce

William M. Daley, Secretary

Technology Administration

Mary L. Good, Under Secretary for Technology

National Institute of Standards and Technology

Robert E. Hebner, Acting Director
National institute of Standards and Technoiogy Buiiding Science Series 176

Nati. inst. Stand. Technoi. BIdg. Sci. Ser. 176, 57 pages (May 1997)

CODEN: NBSSES

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 1997

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402-9325
ABSTRACT

An investigation, conducted under the auspices of an industry-government consortium, studied

the effects of material and application factors on the peel creep-rupture response and peel strength

of EPDM (ethylene-propylene-diene terpolymer) tape-bonded seam specimens Two material

factors (tape system and thickness) and five application factors (EPDM surface condition, primer,

application temperature, application pressure, and time-at-application-temperature) were

examined in a two-level statistically designed experiment. Some tapes had thicknesses typical of

those commercially available at the time of the study, and were designated as having 'standard'

thickness. The thicknesses of standard' and thin tapes were approximately 0.9 mm (0.035 in)

and 0.6 mm (0.025 in), respectively. Specimens were prepared either primed or unprimed using

EPDM that was either cleaned or contaminated. Application temperatures were low, 5 °C

(41 °F), or high, 60 °C (140 °F), and application pressures were low, 0.2 MPa (30 Ibf/in^), or

high, 2 MPa (300 Ibfin^). The time at which the specimens remained at the application

temperature was short, about 24 hours, or long, 672-960 hours. To interpret the data, plots of

mean time-to-failure and mean peel strength versus the combinations of application factors for

each of the four pairs of tape system and tape thickness were analyzed. Comparisons of times-tofailure between the tape-bonded sample sets were made with those of liquid-adhesive-bonded

sample sets tested in an earlier phase of the study. The main conclusions regarding tape-bonded seams from the present investigation are that:

• Primed, clean EPDM provided the longest times-to-failure and highest peel strengths.

• Primed, clean EPDM and 'standard' thickness tape afforded times-to-failure that were

statistically significantly higher than minimum mean times-to-failure of well prepared liquidadhesive-bonded sample sets determined in an earlier investigation.

• The application temperatures and application pressures used in the investigation did not affect

the times-to-failure of sample sets prepared with primed, clean EPDM, that had, as stated,

relatively long times-to-failure.

• 'Standard' thickness tape provided significantly. longer times-to-failure than thinner tape.

• The two tape systems generally responded similarly to factors that promoted either shorter or longer times-to-failure.

Key Words: adhesive tapes; adhesive testing; application factors; building technology, creeprupture; EPDM membranes; peel strength; roofing; seams; time-to-failure

iii

TABLE OF CONTENTS

Page

ABSTRACT iii

1. INTRODUCTION 1 1.1 Background 1 1.2 Phase I Findings 1 1.3 Objective and Scope of Phase II 2

2. EXPERIMENTAL DESIGN 5 2.1 Factors 5 2.2 Sample Size and Levels for Factors 5 2.3 Pilot Study to Determine Creep Load 5 2.4 Fractional Factorial Design 6

3. SPECIMEN PREPARATION AND TESTING 11

3.1 Materials 11

3.2 Creep-Rupture Tests 11

3.3 Peel-Strength Tests 11

3.4 Measurement of Tape Modulus 12

4. RESULTS AND DISCUSSION 13

4.1 Statistical Analysis 13

4.2 Discussion of Creep-Rupture Data 13

4.2.1 Material Factors 18

4.2.2 Application Factors 18

4.3 Discussion of Peel-Strength Data 19

4.4 Failure Mode During Creep-Rupture and Peel-Strength Measurements 22

5. SUMMARY AND CONCLUSIONS 25

6. ACKNOWLEDGMENTS 27

7. REFERENCES 29

APPENDIX A. SPECIMEN PREPARATION Al

APPENDIX B. CREEP-RUPTURE DATA DEVELOPED IN MAIN EXPERIMENT ... Bl

APPENDIX C. EXPERIMENT TO INVESTIGATE TSl VARIABILITY CI
LIST OF TABLES

Page

Table L Material and application factors varied during preparation of Phase II specimens ... 4

Table 2. Combinations of material factors selected in the experimental design 6

Table 3. Combinations of application factors selected in the experimental design 7

Table 4A. Description of the Tape System 1 sample sets 8

Table 4B. Description of the Tape System 2 sample sets 9

Table 5 A. Summary of the T-peel creep-rupture data for Tape System 1 16

Table 5B. Summary of the T-peel creep-rupture data for Tape System 2 17

Table 6A. Summary of the T-peel strength data for Tape System 1 20

Table 6B. Summary of the T-peel strength data for Tape System 2 21

Table 7. Comparison between Phase I and Phase II times-to-failure and peel strengths 23

Table B 1 . Creep-rupture data developed for Tape System 1 in the Main Experiment B2

Table B2. Creep-rupture data developed for Tape System 2 in the Main Experiment B9

Table CI. Description of TSl tapes and primers used in the investigation of TSl variability . CI

vi
LIST OF FIGURES

Page

Figure 1 . Mean Time-to-Failure Versus Load for the Tape-Bonded and Liquid-AdhesiveBonded Specimens Investigated in Phase I [3] 3

Figure 2. Mean Time-to-Failure in Hours Versus Combinations of Application Factors 14

Figure 3. Mean Peel Strength Versus the Combinations of Application Factors 15

Figure Al. Plan view of a piece of EPDM used in specimen preparation A2

Figure CI. Mean times-to-failure of the sample sets prepared to examine TSl tape

variability C2

Figure C2. Mean peel strength of the sample sets prepared to examine TSl tape variability. . C2

Figure C3. Tape modulus (longitudinal direction) at 300 % elongation C4

vii

1. INTRODUCTION

1.1 Background

An industry-government consortium study has been undertaken to: (1) compare the creep-rupture

performance of tape-bonded and liquid-adhesive-bonded seams of EPDM membranes, and (2)

recommend a test protocol and criteria for evaluating creep-rupture performance of such seams.

In recent years, the use of preformed tapes for fabricating seams of EPDM membranes has

increased substantially, and is expected to continue to grow [1]. The consortium study was

initiated at the National Institute of Standards and Technology (NIST) in late 1994 in response to industry requests that independent evaluations be conducted and that nonproprietary data be

developed on the performance of tape-bonded seams [2].

Three EPDM membrane manufacturers (Carlisle Syntec, Firestone, and GenFlex), and two tapesystem manufacturers (Adco and Ashland) along with two trade associations (NRCA and RCI)*

joined with NIST through a Cooperative Research and Development Agreement (CRADA) to design and conduct the study. The experimental program consists of three 1-year phases. Phases

I and II have been completed and Phase III is ongoing. A summary of the objective of each phase

is as follows:

• In Phase I, the creep-rupture response (time-to-failure) of tape-bonded seam specimens

subjected to various peel loads under ambient conditions was compared to that of liquidadhesive-bonded specimens.

• In Phase II, which is the subject of the present report, the peel creep-rupture response and peel

strength of tape-bonded seam specimens were investigated under ambient conditions for a number of material and application variables (Section 1.3).

• In Phase III, the creep-rupture response of tape-bonded seam specimens will be investigated as a function of test temperature and type of loading (i.e., peel versus shear).

In the creep-rupture experiments, seam specimens of a fixed length are stressed under a constant

load and the time over which they sustain the load until total separation (i.e., the time-to-failure)

is recorded. Results from previous NIST studies on liquid-adhesive-bonded specimens have

shown that creep-rupture tests provide a sensitive procedure for evaluating the effects of a

multiplicity of application and environmental factors including EPDM surface condition, adhesive

thickness, temperature, and ozone on the capability of seams to sustain loads over time [3-9].

These results contributed to recommendations on proper field application of seams. The findings

from these past studies also gave impetus to the present industry-government consortium study,

because the sensitivity of the creep-resistance of tape-bonded seam specimens to factors such as

load, EPDM surface condition, use of primer, and tape thickness was not known.

1.2 Phase I Findings

The results of Phase I were published in NIST Building Science Series (BSS) 175, "Performance

of Tape-Bonded Seams of EPDM Membranes: Comparison of the Peel Creep-Rupture Response

*The National Roofing Contractors Association (NRCA) and the Roof Consultants Institute (RCI).

1
of Tape-Bonded and Liquid-Adhesive-Bonded Seams" [3]. In the Phase I study, seam specimens were prepared at room temperature, 23 °C±2 °C(73 °F + 4 °F)*, using two commercial tape

systems (i.e., tape and primer) and one commercial liquid adhesive. In all cases, the EPDM

rubber was well cleaned and, in the case of the tape-bonded specimens, a primer was applied.

Seam specimens were tested for peel strength and for peel creep-rupture resistance (i.e., times-tofailure) under loads ranging from 3. 1 N to 24.9 N (0.7 Ibf to 5.6 Ibf) in increments of

3.1 N(0.71bf).

Figure 1 shows a plot of mean time-to-failure versus load for the Phase I experiments [3]. No

data points are shown for the 3.1 N (0.7 Ibf) load, because no specimen failures have been

observed.** As is evident in Figure 1, the tape-bonded sample sets had times-to-failure that were,

in most cases, comparable to or greater than those of the liquid-adhesive-bonded sample sets. And, the tape-bonded specimens provided mean time-to-failure results that were reproducible

between replicate sets. The liquid-adhesive-bonded sample sets showed considerable variability.

For example, at 9.3 N (2.1 Ibf), the times-to-failure of the five liquid-adhesive-bonded sample sets ranged from about 7 hours to 500 hours (fig. 1). In. contrast, their mean peel strengths ranged

from only 1.87 kN/m to 1.94 kN/m (10.3 Mn to 1 1.1 Ibf/in) [3]. That is, although there was

wi^e variability in the times-to-failure, the variability in the peel strengths was small. This finding

supports the thesis that creep-rupture tests are more sensitive than peel-strength tests for

evaluating factors affecting the capability of seam specimens to support loads over time [3-9].

1.3 Objective and Scope of Phase II

This report presents the results of the Phase II research to investigate the effects of material and

application factors on the peel creep-rupture response and peel strength of tape-bonded seam

specimens. The specimens were prepared under a variety of conditions according to a predetermined statistical design. A description of the seven factors—tape system, tape thickness,

EPDM surface condition, primer, application temperature, application pressure, and time-attemperature—varied during specimen preparation is given in Table 1 with a comment as to why

each factor was included. The peel strengths of the specimens were measured, and times-tofailure were determined under a peel load of 9.3 N (2. 1 Ibf). The data were statistically analyzed

to determine the effects of each factor (Table 1), or interactions between them, on time-to-failure

and peel strength. ..

' ..

The Phase II research is an extension of that conducted in Phase I. In Phase I [3], the specimens were 'well prepared' in the laboratory in that the EPDM was always cleaned and primed (in the case of tapes), and the application temperature and application pressure were selected to be in the

range that may be experienced in the field (Table 1). The Phase II research addressed the

assumption that these material and application factors are variable in practice, and changes in the

level of these factors may affect seam time-to-failure and peel strength. For example, in practice,

more than one tape system is available, and the tapes can be manufactured with different

*Temperature vanations are absolute bounds.

Tests at the 3 . 1 N (0.7 Ibf) load are ongoing and, as of this writing, after over 16,800 hours (about 23

months), no specimen failures have been observed.
LOAD, Ibf

I

Replicate 1 • Replicate 2

A Replicate 3

Replicate 4

Replicate 5

Tape System 1 Tape System 2

Liquid Adhesive

10 15

LOAD, N

20 25

Figure I. Mean Time-to-Failure Versus Load for the Tape-Bonded and Liquid-Adhesive-Bonded

Specimens Investigated in Phase I [3].

thicknesses. Moreover, it is reasonable to assume that cleaning and priming the EPDM might not

be carried out in the field as recommended by manufacturers. Also, typical field temperatures at which seams are fabricated may vary fi-om 0 °C (32 °F) or colder to 60 °C (140 °F) or hotter,

and pressures applied by roofing mechanics are variable due to the human element associated with

manual labor, e.g., strength. Phase II was designed to quantify the effects of these factors.

Additionally, consistent with the overall objective of the research program, the creep-rupture

behavior of tape-bonded sample sets prepared under a variety of conditions are compared with

that of well prepared liquid-adhesive-bonded sample sets. In recent years, field experience with

liquid-adhesive-bonded seams has been, in most cases, satisfactory. Consequently, the laboratorymeasured times-to-failure of well prepared liquid-adhesive-bonded specimens were taken as the

benchmark for acceptable creep lifetimes.

3
Table 1. Material and application factors varied during preparation of Phase II specimens

Factor Description Comment

Tape System • Tape System 1 (TSl)

• Tape System 2 (TS2)

In practice, tapes are available fi-om a number of

suppliers.

Tape

Thickness

• Thin: about 0.5 mm to 0.6 mm

(0.020 in to 0.025 in)

• 'Standard': about 0.9 mm to 1 .0 mm

(0.035 in to 0.040 in)

Note: The thicker tapes had

thicknesses typical of those commercially available at the time of

tHp iiiw <itnnv' oLuuy t}iii<? tnpv \A7Prp Hf^Qicmiitf*H

, tiitio, uity wtit uc^oi^iidi^Li as having 'standard' thickness.

In practice, as manufactured products, tapes may be

produced in a variety of thicknesses. Today's tapes

generally have thickness of about 0.9 mm (0.035 in). It was of interest to quantify the effect of tape thickness on

time-to-failure and compare the results to those

previously obtained on liquid-adhesive-bonded

specimens. In the latter case, thin layers of adhesive had

significantly reduced times-to-failure in comparison to

UllV^K loiyClo KJL cH-lllColVC vJj .

EPDM Surface

Condition

• Clean

• Contaminated

In practice, proper application of seams requires that the surface of the EPDM sheet be well cleaned. The degree

of cleaning can be variable in the field. Lack of cleaning

may result in unacceptable seams.

Primer

- }

• Primed EPDM

• Unprimed EPDM

In practice, proper application of tape-bonded seams

requires that the surface of the EPDM sheet be primed.

Nevertheless, it may be assumed that, due to the human

element mvolved, primer may be omitted for some

reason; e.g., roofmg crew arrives at the job site without

primer. Lack of priming may result in unacceptable

Application

Temperature

• Low: 5 ''C (41 '^F)

• High: 60 °C (140 °F)

In practice, seams may be fabricated with membrane

materials at temperatures ranging from 0 °C (32 °F) or colder to 60 °C (1 40 °F) or higher. The selected range

simulates hot and cold temperatiires that are routinely

experienced in the field.''

Application Pressure

• Low: 0.2 MPa (30 Ibf/in')

• High: 2 MPa (300 Ibfi'm')

In practice, seams may be fabricated over a range of

pressures depending on the roofmg mechanic. Strong

[10] has reported that normal application pressures

exerted by roofmg mechanics are about 0.7 MPa

( 1 00 Ibf^in^). The range selected for study brackets that pressure by a factor of about three.

Time-atTemperature'

• Short: 20 h to 24 h at the application temperature; then stored at room

temperature until tested

• Long: stored at application

temperature until tested, about 672 h to 960 h

In practice, seams may remain for relatively long periods

of time at the temperature at which they were fabricated. On the other hand, under some circumstances, the temperature may change shortly after seam preparation.

"Field experience with tapes available when the experiment was designed provided no reason for including tape

thicknesses greater than 'standard.' •"Temperatures below 0 °C (32 °F) and above 60 °C (140 °F) are encountered in practice. However, practical constraints associated with preparing laboratory specimens below 0 °C (32 °F) and above 60 °C (140 °F) precluded

investigating the effects of such temperature extremes.

' "Time-at-temperature" refers to holding the completed specimen at the preparation temperature for a specified

duration.

4
2. EXPERIMENTAL DESIGN

2.1 Factors

The seven factors detailed in Table 1 were selected for study* by the consortium steering

committee members. These factors can be classified into two material factors (tape system and

tape thickness) and five application factors (EPDM surface condition, primer, application

temperature, application pressure, and time-at-temperature). Whenever possible, the user would

like to select a combination of levels of these application factors which would consistently

produce good-quality seams whatever the values of the material factors. Of the material factors,

the user may, or may not, have the possibility of selecting the tape system and tape thickness.

A naive approach to experimentation would vary each of the seven factors individually, leaving all but one factor set at 'typical' values for each experiment. This form of experimentation is highly

inefficient, since it provides no information on potential factors which might prove important in combination with one another: for example, high pressure might be desirable at low temperatures,

but low pressure might be better at high temperatures. When the effect of a factor on a response

depends on the level of other factors, these factors are said to interact. 'One factor at a time'

experimentation provides no information about potential interactions, since the factors are never

varied simultaneously.

2.2 Sample Size and Levels for Factors

Available experimental resources such as time for testing, test chambers, and raw materials

suggested that it would not be possible to test more than about 500 specimens. For example, once a creep chamber was committed to testing, it ought not to be disturbed until all specimens

had failed. Such constraints made it necessary to design a single large experiment (including a

pilot study) rather than a series of smaller experiments.

From Phase I experience with the creep-rupture tests [3], it appeared that eight specimens for

each combination of factor levels would be adequate. For simplicity, it was decided to consider

only two levels of each of the seven factors, and to choose these levels far enough apart so that

the range of practical importance was generally covered (Table 1).

2.3 Pilot Study to Determine Creep Load

Phase I produced extensive data on times-to-failure and peel strength at various loads (fig. 1), so

it was decided to perform the present investigation at a single load. Implicit in this decision is the

assumption that the experimentalist would be willing to ignore any interaction of load with the

other factors under consideration.

A pilot study was performed to select a single load. Eight sample sets, each having eight

specimens, were subjected to creep-rupture testing at each of four loads: 9.3 N, 12.5 N, 15.6 N,

and 18.7 N (2.11bf, 2.8 Ibf, 3.5 Ibf, and 4.2 Ibf). Four of these sample sets were 'poorly

prepared' (unprimed, contaminated EPDM surface, and 0.2 MPay30 IbCin^ application pressure).

*Refen"ed to herein as the Phase II Main Experiment.

5
whereas the remaining four were 'well prepared' (primed, clean EPDM surface, and

2 MPa/300 Ibfi'in^ application pressure). On the basis of this pilot study, it was considered that a load of 9.3 N (2. 1 Ibf) would likely result in a creep experiment which could be completed within a reasonable time; that is, specimens would fail soon enough to obtain results within a few weeks

or less, but not so quickly as to obscure relevant distinctions among the sample sets.

2.4 Fractional Factorial Design

The primary objective of the Phase II Main Experiment was to detemiine which factors and

interactions are most important, as measured by the effect that varying these factors had on creep

life and peel strength. As discussed in Section 2. 1, it is necessary to vary factors together in order

to estimate interactions. A statistical design which required testing at all combinations of levels

for all factors is called a (full) factorial design. Usually two levels are chosen for each factor,

since such a design is relatively easy to analyze, and since more levels can require considerably

more testing. It is also desirable that, where appropriate, levels of factors be set at the extremes

of what is likely to be observed in practice.

When the amount of testing required for a full factorial experiment (even with only two levels per

factor) is prohibitive, a carefijlly chosen fraction of all possible combinations is usually selected at the cost of not being able to assess separately all of the interactions and possibly, also, certain

main effects. Such a design, called a fractional factorial, was used in this study.

There are 2' = 128 possible combinations of the seven factors (each at one of two levels) given in

Table 1. Eight specimens for each of these 128 combinations would require 1024 specimens for

the flill experiment. This was too many by about a factor of two, so a half-fraction of the full factorial design was chosen. This design included the four combinations of material factors

(Table 2), and 16 of the 32 possible combinations of the application factors (Table 3). The same

16 combinations of the application factors were assigned to each of four combinations of the

material factors. Since the user of a tape system may have little or no ability to control the

material factors, it was concluded that this design would lead to the selection of combinations of

levels of application factors which produced 'good' seams, as quantified by time-to-failure and

peel strength, for all combinations of material factors.

Table 2. Combinations of material factors selected in the

experimental design

Tape System Tape

No. Thickness

TSl Thin

TSl 'Standard'

TS2 Thin

|_ TS2 'Standard'

6
Table 3. Combinations of application factors selected in the experimental design

nrUM bunace

Condition Primer

Application

Temperature

Application

Pressure

Time-atTemperature

Contaminated Primed High High Short

Contaminated Unprimed Low High Short

Contaminated Unprimed High Low Short

Contaminated Primed Low Low Short

Clean Unprimed High High Short

Clean Primed Low High Short

Clean Primed High Low Short

Clean Unprimed Low Low Short

Contaminated Primed High High Long

Contaminated Unprimed Low High Long

Contaminated Unprimed High Low Long

Contaminated Primed Low Low Long

Clean Unprimed High High Long

Clean Primed Low High Long

Clean Primed High Low Long

Clean Unprimed Low Low Long

'See Table 1 for description of the factors.

The resultant design provided 64 sample sets (four for each combination of material factors times

16 for each combination of application factors) divided equally between the two tape systems.

Tables 4A and 4B describe the 32 sample sets for Tape System 1 and the 32 sample sets for Tape

System 2, respectively.

7
Table 4A. Description of the Tape System 1 sample sets

Material Factors Application Factors Sample Tape Tape EPDM Surface Application Application Time-atSet No. Thickness System Condition Primer Temperature Pressure Temperature

1 Thin 1 Contaminated Primed High Low Short 2 Thin 1 Contaminated Unprimed Low High Short

3 Thin 1 Contaminated Unprimed High Low Short

4 Thin 1 Contaminated Primed Low High Short

5 Thin 1 Clean Unprimed High Low Short 6 Thin 1 Clean Primed Low High Short 7 Thin 1 Clean Primed High Low Short 8 Thin 1 Clean Unprimed Low High Short 9 Standard 1 Contaminated Primed High Low Short 10 Standard 1 Contaminated Unprimed Low High Short

11 Standard 1 Contaminated Unprimed High Low Short 12 Standard 1 Contaminated Primed Low High Short

13 Standai'd 1 Clean Unprimed High Low Short 14 Standard 1 Clean Primed Low High Short 15 Standard 1 Clean Primed High Low Short 16 Standard 1 Clean Unprimed Low High Short 33 Thin 1 Contaminated Primed High Low Long

34 Thin 1 Contaminated Unprimed Low High Long

35 Thin 1 Contaminated Unprimed High Low Long

36 Thin 1 Contaminated Primed Low High Long

37 Thin 1 ... Clean Unprimed High Low Long

38 Thin 1 Clean Primed Low High Long

39 Thin 1 Clean Primed High Low Long

40 Thin 1 Clean Unprimed Low High Long

41 Standard 1 Contaminated Primed High Low Long

42 Standard 1 Contaminated Unprimed Low High Long

43 Standard 1 Contaminated Unprimed High Low Long

44 Standard 1 Contaminated Primed Low High Long

45 Standard 1 Clean Unprimed High Low Long

46 Standard 1 Clean Primed Low High Long

47 Standard 1 Clean Primed High Low Long

48 Standard 1 Clean Unprimed Low High Long

8
Table 4B. Description of the Tape System 2 sample sets

Material Factors Application Factors Sample

Set No. Tape

Thickness

Tape

System

EPDM Surface Condition Primer

Application

Temperature

Application

Pressure

Time-atTempciaturc

17 Thin 2 Contaminated Primed High Low Short 18 Ihin 2 Contaminated Unprimed Low High Short 19 Thin 2 Contaminated Unprimed High Low Short 20 Thin 2 Contaminated Primed Low High Short 21 Thin 2 Clean Unprimed High Low Short 22 Thin 2 Clean Primed Low High Short 23 Thin 2 Clean Primed High Low Short 24 Thin 2 Clean Unprimed Low High Short 25 Standard 2 Contaminated Primed High Low Short 26 Standard 2 Contaminated Unprimed Low High Short 27 Standard 2 Contaminated Unprimed High Low Short 28 standard 2 Contaminated Primed Low High Short 29 Standard 2 Clean Unprimed High Low Short 30 Standard 2 Clean Primed Low High Short

31 Standard 2 Clean Primed High Low Short 32 Standard 2 Clean Unprimed Low High Short 49 Thin 2 Contaminated Primed High Low Long

50 Thin 2 Contaminated Unprimed Low High Long

51 Thin 2 Contaminated Unprimed High Low Long

DZ Ihin 2 Contaminated Pnmed Low T T* 1_ High Long

CI Ihin 2 Clean T T J unpnmed T T' 1. High Low Long

54 Thin 2 Clean Primed Low High Long

inm 2 Clean Primed High Low T _ _ Long

DO Ihin 2 Clean Unprimed Low High T ^ ~ Long

57 Standard 2 Contaminated Pnmed High Low Long

58 Standard 2 Contaminated Unprimed Low High Long

59 Standard 2 Contaminated Unprimed High Low Long

60 Standard 2 Contaminated Primed Low High Long

61 Standard 2 Clean Unprimed High Low Long

62 Standard 2 Clean Primed Low High Long

63 Standard 2 Clean Primed High Low Long

64 Standard 2 Clean Unprimed Low High Long

9
r
3. SPECIMEN PREPARATION AND TESTING

3.1 Materials

Two tape systems, comprised of a preformed tape and primer and designated Tape System 1 (TSl) and Tape System 2 (TS2), were used to prepare the specimens. Both the TSl and TS2

tapes, and also the TS2 primer, were obtained at the beginning of the Phase II studies.* The TSl

primer was that previously used during the Phase I studies. The EPDM sheet was a commercial

product having a thickness of about 1.5 mm (0.060 in). Appendix A presents the experimental

details on specimen preparation under the various conditions listed in Table 1 . The experimental

design included TSl and TS2 tapes that were commercial products at the time of the study.

These commercial tapes were designated as having 'standard' thickness, which is the term used in this present report for the thicker tapes. The 'thin' tapes were noncommercial products made

specifically for the Phase II investigations.

3.2 Creep-Rupture Tests

Eight peel specimens, randomly selected from each sample set, were subjected to creep-rupture

testing under the 9.3 N (2. 1 Ibf) load. The tests were conducted at room temperature,

23 °C ± 2 °C (73 °F + 4 °F), in laboratory-constructed chambers according to the general

procedure described in Martin, Embree, Stutzman, and Lechner [5]. The chambers were designed

to load the specimens simultaneously. The relative humidity in the chambers was maintained

between 40 % and 45 % using a saturated potassium carbonate solution [11]. Built-in fans

circulated the air in the chambers. The relative humidity in each chamber was checked using a Labcraft Digital Hygrometer, Model Number 244-354.** Specimens were conditioned for a minimum of 16 hours in the chambers before applying the creep load. The times-to-failure (i.e., time under load until the two EPDM strips comprising the specimens completely separated) were

recorded (± 1 s) electronically for each specimen using a computerized monitoring and datalogging system.

3.3 Peel-Strength Tests

Four T-peel specimens were randomly selected from each sample set, and the T-peel strengths were determined at room temperature, 23 °C ± 2 °C (73 °F ± 4 °F), at a crosshead rate of 50

mm/min (2 in/min). The universal testing machine was equipped with hardware and software for

recording and calculating peel-strength data. After testing, each specimen was visually examined

and the mode of failure, adhesive or cohesive, was noted.

*The TSl tapes arrived in two shipments; whereas the TS2 tapes came in one shipment.

**Certain company products are mentioned by name in the text to specify adequately the experimental procedure and

equipment used, hi no case does such identification imply recommendation or endorsement by the National histitute of

Standards and Technology, nor does it imply that the equipment is necessarily the best available for the purpose.

11
3.4 Measurement of Tape Modulus

Tensile modulus of the tapes was determined at room temperature using the universal testing

machine at a crosshead rate of 500 mm/min (20 in/min). Dumbbell-shaped specimens, having a

total length of 75 mm (3 in) with a reduced section length of 25 mm (1 in) and width of 3.2 mm

(Vs in) were cut from the tape-roll material using a die and press. Before cutting, the tape was

covered with talc to prevent sticking to the die.

12
4. RESULTS AND DISCUSSION

4.1 Statistical Analysis

To analyze the Phase II Main Experiment results, the plots in Figures 2 and 3 were prepared as summaries of the time-to-failure and peel-strength data, respectively. Note that the time-tofailure axis is logarithmic, while the peel strength axis is linear. The plots are means (either timeto-failure or peel strength) for each of the 16 combinations of application factors. The plot

characters (along with the figure legends) identify the combinations of the tape system and tape

thickness (i.e., the material factors). The horizontal axis specifies the levels of the five application

factors. The application factor combinations are ordered in increasing mean response. The mean

for the four sample sets (i.e., TSl-thin, TS1-' standard', TS2-thin, and TS2-'standard') prepared

at each combination of application factors is indicated by the dotted line.

Formal statistical analyses including analysis of variance and multiple comparisons provided

quantitative support for the discussions that follow (Sections 4.2 and 4.3). However, because the

discussions of Figures 2 and 3 adequately describe the results of the study, a complex presentation

of the formal analyses is omitted.

In addition to the creep-rupture data developed in Phase II, Figure 2 also contains a horizontal

dashed line. It represents the average time-to failure for the three sets of well prepared liquidadhesive-bonded specimens (i.e., those fabricated with industry-recommended adhesive thickness

and clean EPDM) that had the lowest average times-to-failure at 9.3 N (2.1 Ibf) in Phase I (fig. 1). The dashed line is included to provide a point of comparison between the Phase II data for tapebonded sample sets and liquid-adhesive-bonded sample sets (Section 4.2.2). The lowest mean

times-to-failure for the liquid-adhesive-bonded sample sets were selected for comparison, because

sets with these mean times-to-failure are considered representative of the minimum of the range of

liquid-adhesive-bonded seams typically used in current practice. That is, the question addressed is whether tape-bonded sample sets prepared under a variety of conditions perform equal to, or

better than, the lowest mean performance of well prepared liquid-adhesive-bonded sample sets.

4.2 Discussion of Creep-Rupture Data

The results of the creep-rupture tests as a fianction of material and application factors are summarized in Tables 5 A and 5B for the 32 TSl and 32 TS2 sample sets, respectively. Appendix

B gives the time-to-failure and failure mode for each specimen along with the thickness of the

tape. As shown in the Tables 5A and 5B, the majority (about 80 %) of the coefficients of

variation (CoV) for the mean times-to-failure were greater than 20 %. This was in contrast to the

results of the Phase I study [3] wherein about 75 % of the coefficients of variation were less than

20 percent. It seems likely that the increased data scatter in the present study could be attributed to increased nonuniformity between specimens in a set because of preparation under application

conditions that are more difficult to control than those in Phase I (e.g., high and low temperatures

versus room temperatures).

13
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DC

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Liquid Adhesive a... A

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2 Material Factors:

4

13

TS 1 Thin = 1 TS 1 Standard = 2

3

3 TS2Thin = TS 2 Standard

3= 4

Surf. Primer 1 1 1 1 1 1 2 1 2 2 2 2 1 2 2 2

Surf. Cond. 2 2 1 1 2 2 2 1 2 2 1 2 1 1 1 1 Temperature 2 2 1 1 1 1 1 2 1 2 1 2 2 1 2 2

Pressure 1 1 1 1 2 2 1 2 1 2 2 2 2 2 1 1 Time at Temp. 2 1 2 1 2 1 2 1 1 1 2 2 2 1 1 2

Application Factor Combinations

Figure 2. Mean Time-to-Failure in Hours Versus Combinations of Application Factors. (Primer:

Unprimed = 1, Primed = 2; EPDM Surface Condition: Clean = 1, Contaminated = 2; Application Temperature: Low = 1, High = 2; Application Pressure: Low - 1, High - -

2; Time-at-Temperature: Short = 1, Long = 2.) The horizontal dashed line represents

the mean time-to-failure of the three sets of well prepared, liquid-adhesive-bonded

specimens (i.e., those fabricated with industry-recommended adhesive thickness and

clean EPDM) that had the lowest mean times-to-failure at the 9.3 N (2. 1 Ibf) load in Phase I (see fig. 1). The dotted line represents the mean for the four sample sets of

tape-bonded specimens prepared at each combination of application factors.
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1 1

iJlaterial Factors:

TS 1 Thin = 1 TS 1 Standard = 2

TS2Thin =3

TS 2 Standard =4

Surf. Primer 1 1 1 1 2 2 2 1 1 1 2 1 2 2 2 2

Surf. Cond. 2 2 2 2 2 2 2 1 1 1 2 1 1 1 1 1 Temperature 2 1 1 2 2 1 1 1 1 2 2 2 1 1 2 2

Pressure 1 2 2 1 2 1 1 1 1 2 2 2 2 2 1 1 Time at Temp. 2 2 1 1 2 1 2 1 2 1 1 2 2 1 1 2

Application Factor Combinations

Figure 3. Mean Peel Strength Versus the Combinations of Application Factors. (Primer:

Unprimed = 1, Primed = 2; EPDM Surface Condition: Clean = 1, Contaminated = 2; Application Temperature: Low = 1, High = 2; Application Pressure: Low = 1, High =

2; Time-at-Temperature: Short = 1, Long = 2.) The dotted line represents the mean for

the four sample sets of tape-bonded specimens prepared at each combination of

application factors.)

15
Table 5A. Summary of the T-peel creep-rupture data for Tape System 1 Sample Time-to-Failure. hours CoV'' Failure

Set No. min max mean sd" % Mode'

1 1.74 4.95 3.46 1.26 36.5 3(8)

2 • - • 6.37 6.39 6.38 0.01 0.1 2(8) 3 0.05 0.07 0.06 0.01 13.5 2(8)

4 7.35 11.96 8.84 1.49 16.8 2(8) 5 0.39 0.99 0.57 0.20 34.2 2(8)

6 . , 2.76 11.24 8.02 3.36 41.9 1(2), 2(1), 3(5)

7 ^ 4.00 9.94 6.38 2.12 33.2 2(6), 3(2)

8 0.29 0.63 0.42 0.12 28.2 2(8)

9 10.99 46.28 30.26 11.81 39.0 1(6), 3(2)

10 6.42 6.52 6.47 0.03 0.5 2(8)

11 0.08 0.24 0.17 0.06 32.9 2(8)

12 4.02 9.47 6,37 ^.02 31.7 2(8) 13 1.74 5.97 3.17 1.26 39.9 2(8)

14 7.79 158.39 53.09 62.36 117.5 1(7), 3(1) 15 84.21 152.21 127.63 23.89 18.7 1(8)

16 0.67 2.46 1.27 0.68 53.9 2(8)

33 1.41 21.49 8.58 7.37 86.0 3(8)

34 6.34 6.35 6.35 0.00 0.0 2(8)

35

' 0.03 0.05 0.04 0.01 18.6 2(8)

36 0.73 3.38 1.82 0.97 53.0 2(8)

37 1.68 3.98 2.61 0.97 37.3 2(8)

38 0.68 2.42 1.75 0.55 31.4 1(2), 3(6)

39 20.10 35.27 27.35 '

. 5.97 21.8 3(8)

40 0.17 0.34 0.27 0.05 20.2 2(8)

41 37.06 150.45 80.35 "

34.90 43.4 1(1), 3(7)

42 6.37 7.20 6.49 0.29 4.4 2(8)

43 0.20 0.72 0.40 0.17 . 41.8 2(8)

44 4.25 7.51 5.60 1.11 19.8 2(8)

45 22.42 56.19 32.80 10.53 32.1 2(8)

46 2.09 5.26 3.94 1.09 27.7 2(6), 3(2)

47 154.23 211.21 184.31 17.46 9.5 3(8)

48 0.37 0.79 0.50 0.14 28.6 2(8)

^sd indicates standard deviation. ''CoV indicates coefficient of variation. "Failure mode: 1 = cohesive; 2 - adhesive; 3 - mixed; numbers in parentheses indicate the number of specimens

in the sample set that experienced the given mode.

16
Table 5B. Summary of the T-peel creep-rupture data for Tape System 2

Sample

Set No.

Time-to-Failure, hours CoV' I' tii 1 urc min max mean % Mode''

1 / 1 .4/ 19.22 9.75 7.07 72.5 2(5), 3(3)

1 o18 0.01 0.03 0.01 0.01 45,7 2(8)

19 0.03 0.08 0.05 0.02 31.5 2(8)

20 1.54 4.86 3.59 1.15 32.0 2(8) 21 2.3

4.78 3.29 0.74 22,5 2(8)

22 CO! 37.34 23.24 9.09 39,1 1(3), 2(1), 3(4)

23 n c\A 7.94 33.80 20.82 9.41 45.2 1(6), 2(2)

24 U.4j 0.79 0.60 A 1 0.13 22.2 2(8)

1 A/1 3.1)4 22.22 7.66 6.96 AA O 90.8 2(8)

26 6.4 / 6.65 6.54 A AT 0.07 1.0 2(8)

27 0.22 0.37 0.30 A A^ 0.05 16,4 2(8)

28 1 A 1 C

10. 15 33.17 22.10 7.33 33,2 2(7). 3(1)

29 2.20 49.77 17.89 1 A OA 19.89 1 1 1 ,2 1(2), 2(4), 3(2)

30 36.39 77.77 54.13 15,51 28,7 1(2), 2(1), 3(5) 31 22.35 34.09 28.19 4.76 16,9 1(8)

32 2.46 6.84 4.06 1.92 47,2 2(8)

49 0.21 0.85 0.37 0.21 57,8 2(8)

50 0.01 0.01 0.01 0.00 35,7 2(8)

C 1 A A 1 U.Ul 0,03 0,02 A AA U.UL) O /I A 24,

2(8) CODZ A on 5.58 2.34 1 AO 1.48 /CI 1 63.

2(8) CI J. Oft 92.90 35.99 3z. j6 on c yV.D 2(8)

D4 c c c

J. J J 39.70 26.34 lU. / J

/lA Q

4U.ft O/IA

1(2), 2(1), 3(5) CC CO/C OA 1057.66 695.68 OAA 1 1 zUU. 33 zo.o 1(8) JO U.3o 0.72 0.53 A 1 O

U. 1/ z 1 .o 2(8)

-) / I). 46 11.89 5.18 A A/Z 4.46 OC A 86.

2(8)

58 6.39 6.44 6.41 A A'^ 0.02 A

0.3 2(8)

59 0.06 0.11 0.08 0.02 26,1 2(8)

60 4.61 21.85 14,24 7.13 50,1 2(6), 3(2)

61 20.97 44.75 36.52 7.86 21,5 1(4), 3(4)

62 20.57 58.81 37.51 13.40 35,7 1(2), 2(2), 3(4)

63 2.65 66.71 33.68 30.64 91.0 1(4), 2(4)

64 0.83 2.33 1.30 0.49 37.7 2(8)

°sd indicates standard deviation. ''CoV indicates coefficient of variation. 'Failure mode: 1 = cohesive; 2 = adhesive; 3 = mixed; numbers in parentheses indicate the number of specimens

in the sample set that experienced the given mode.

17
As is evident in Figure 2, the mean times-to-failure of the tape-bonded sample sets were quite

variable, ranging from a few minutes (i.e., 0.01 hour) to about 700 hours. Figure 2 provides a

basis for comparing the effects of varying both the material and application factors on time-tofailure. As is to be discussed, the main effects observed are associated with tape thickness,

primer, and EPDM surface condition. A secondary effect associated with the interaction of high

temperature, high pressure, and clean EPDM was also observed.

4.2. 1 Material Factors. From an examination of the plot characters in Figure 2, the 'standard'

thickness sample sets had, in most cases, greater times-to-failure than the thin sample sets. Simultaneous confidence intervals (details not shown) demonstrated that the 'standard '-thickness

sample sets had significantly (95 % level) longer mean times-to-failure than the corresponding thin

sample sets for 1 1 of the 16 application factor combinations. And, the thin sample sets did not

have significantly longer times-to-failure in the remaining five cases. That is, the time-to-failure

results provided no evidence that thinner tapes should be used. The observation of thick tape

being longer lived than thin tape was consistent with past NIST results whereby relatively thick

layers of butyl-based liquid adhesive provided longer times-to-failure than did relatively thin

liquid-adhesive layers [4].

It may also be seen in examining Figure 2 that, for the combinations of application factors, no

trend of time-to-failure behavior as a fianction of tape system is evident. For 10 of the 16

combinations of application factors, simultaneous confidence intervals showed no significant

difference in the times-to-failure of the TS 1 and TvS2 data sets. Where a significant difference

existed, the TS 1 sample sets had greater mean time-to-failure in four cases, while the TS2 sample

sets had shorter mean time-to-failure in two cases.

Two general conclusions can be drawn from Figure 2 regarding the effect of material factors on

the creep-rupture behavior of the two tape systems. First, 'standard' thickness tape provided

significantly longer times-to-failure than thinner tape. Second, the two tape systems (i.e., TSl

and TS2) responded in the same manner to the different combinations of application factors. That

is, factors that promoted either shorter or longer times-to-failure generally did so for both tape

systems.

4.2.2 Application Factors. In considering the application factors, it is of interest to compare in Figure 2 the time-to-failure data for the 16 Phase II sample set combinations with the average

time-to-failure for the three sets of liquid-adhesive-bonded specimens from Phase I. Eight of the

application factor combinations have lower mean times-to-failure than the average for liquidadhesive-bonded sample sets. Ofthese eight application factor combinations, seven sets were

unprimed. Moreover, of those seven unprimed sets, five included the contaminated EPDM

surface condition. Among the six application factor combinations having the mean times-tofailure greater than the liquid-adhesive-bonded sample sets, five were primed, and five had clean

EPDM surfaces. And, also included among the six combinations having the highest mean timesto-failure are the four cases where the EPDM is both primed and cleaned. A corollary to this

latter observation is that, within the limits set in the experiment, temperature, pressure, and timeat-temperature did not affect the creep-rupture response of the primed and clean sample sets to

the extent that the mean times-to-failure were less than that of the liquid-adhesive-bonded

sample sets.

18
The findings in Figure 2 quantify the importance of both priming and cleaning the EPDM rubber,

which is in accord with manufacturers' recommendations for fabrication of tape-bonded seams

[2]. In general terms, the data in Figure 2 suggest that, if tape-bonded seams are primed, it is reasonable to expect that they will have creep lifetimes comparable to liquid-adhesive-bonded seams. On the other hand, primed tape-bonded seams having clean EPDM can have longer creep

lives than liquid-adhesive-bonded seams. And, it is important to point out, the relatively long

creep lifetimes of seams made with primed, clean EPDM are not expected to be adversely affected

by application temperature and pressure (within the limits selected for the study), which are

factors that are uncontrollable in practice.

It is of interest to note that there was one combination of application factors which produced

relatively long times-to-failure even though the specimens were unprimed—this is the fourth

combination fi'om the right in Figure 2. Notice that this combination had clean EPDM surfaces,

high temperature, high pressure, and long time-at-temperature. Apparently this combination of

appHcation factors compensated for the unprimed EPDM, as it was the only combination that

included no primer and, yet, had times-to-failure greater than the liquid-adhesive-bonded sample

sets. This finding has little practical importance, as achieving this combination of application

factors in the field may be impossible. It would seem far simpler to ensure that the EPDM is primed and cleaned during seam fabrication.

The most important results on creep life have been summarized in the above paragraphs.

However, additional details can still be learned fi-om Figure 2. Note, for example, that the results

for the rightmost two combinations are very similar for sample sets having 'standard' thickness

tape. Since the only factor which differs between these combinations is time-at-temperature, this

provides evidence that, at least by itself, time-at-temperature does not have much of an effect for

'well-made' specimens (i.e., primed and clean EPDM).

4.3 Discussion of Peel-Strength Data

The mean peel-strength data given in Figure 3 represent four measurements for each of the 64

factor combinations. Tables 6A and 6B provide a summary of these data for the 32 TSl and 32

TS2 sample sets, respectively. As can be seen in Figure 3, the mean peel strengths ranged from

about 0. 18 icN/m to 2.3 kN/m (1 Ibfi'in to 13 Ibf/in). Values at the upper end of the range were

typical of those previously measured for tape-bonded seams made with primed, clean EPDM

[2,3].

Regarding material factors, as evident in Figure 3, the sample sets made with 'standard' thickness

tape tended to be stronger than those made with thin tape. And, overall, there was little difference in peel strength between the two tape systems except with primed, clean EPDM.

Regarding application factors, priming and cleaning of EPDM surfaces was necessary for high

peel strength, while unprimed, contaminated EPDM resulted in low peel strength. Notice in

Figure 3 that the four combinations of application factors that had the greatest peel strength were

prepared with primed and clean EPDM. In contrast, the four combinations of application factors

that had the lowest peel strength were prepared with unprimed, contaminated EPDM. Also, it is interesting to note that the sample sets prepared with unprimed, clean EPDM at high temperature.

19
Table 6A. Summary of the T-peel strength data for Tape System 1 Sample Peel strength, kN/m Peel Strength. Ibf/in CoV^ Failure Set No. min max mean min max mean % Mode'

1 1.17 1.31 1.22 0.06 6.7 7.5 7.0 0.36 5.1 3 2 0.34 0.42 0.37 0.04 2.0 2.4 2.1 0.21 9.7 2

3 0.28 0.33 0.30 0.02 1.6 1.9 1.7 0.13 7.8 2

4 0.77 0.84 0.79 0.03 4.4 4.8 4.5 0.18 4.1 2

5 0.82 0.86 0.84 0.02 4.7 4.9 4.8 0.10 2.2 2 6 1.42 1.54 1.48 0.06 8.1 8.8 8.5 0.31 3.7 1 7 1.36 1.38 1.37 0.01 7.8 7.9 7.8 0.07 0.9 3 8 0.58 0.67 0.64 0.04 3.3 3.8 3.6 0.24 6.4 2

9 1.55 1.74 1.63 0.10 8.8 9.9 9.3 0.55 5.9 3 10 0.46 0.53 0.50 0.03 2.6 3.0 2.9 0.17 5.8 2

11 0.35 0.47 0.40 0.05 2.0 2.7 2.3 0.30 13.0 2

12 1.17 1.34 1.22 0.08 6.7 7.7 7.0 0.46 6.5 2

13 1.23 1.46 1.40 0.11 7.0 8.3 8.0 0.64 8.1 2

14 0.95 1.56 1.27 0.30 5.4 8.9 7.3 1.72 23.7 1 15 1.73 1.78 1.75 0.03 9.9 10.2 10.0 0.16 1.6 1 16 1.03 1.65 1.28 0.27 5.9 9.4 7.3 1.53 21.0 2 33 0.70 1.37 1.08 0.29 4.0 7.8 6,2 1.67 26.9 3 34 0.30 0.38 0.35 0.04 1.7 2.2 2.0 0.20 10.1 2 35 0.13 0.30 0.19 0.08 0.7 1.7 1.1 0.43 39.8 2 36 0.72 0.88 0.78 0.07 4.1 5.0 4.4 0.41 9.2 2 37 0.91 1.22 1.09 0.15 5.2 7.0 6.2 0.85 13.6 2 38 0.96 1.50 1.18 0.25 5.5 8.6 6.7 1.44 21.4 1 39 1.14 1.52 1.35 0.18 6.5 8.7 7.7 1.05 13.6 3 40 1.01 1.16 1.09 0.07 5.8 6.6 6.2 0.40 6.4 2

41 0.95 1.71 1.43 0.33 5.4 9.8 8.1 1.91 23.4 3 42 0.47 0.53 0.49 0.03 2.7 3.0 2.8 0.16 5.8 2 43 0.41 0.52 0.47 0.04 2.4 3.0 2.7 0.25 9.2 2 44 1.21 1.66 1.41 0.18 6.9 9.5 8.0 1.05 13.1 2 45 1.48 1.76 1.60 0.14 8.4 10.1 9.2 0.80 8.8 3 46 1.19 1.58 1.45 0.18 6.8 9.0 8.3 1.01 12.2 1 47 1.70 1.87 1.80 0.07 9.7 10.7 10.3 0.40 3.9 3 48 1.03 1.32 1.15 0.12 5.9 7.5 6.6 0.70 10.6 2

"sd indicates standard deviation. ''CoV indicates coefficient of variation. 'Failure mode: 1 = cohesive; 2 = adhesive; 3 = mixed.

20
Table 6B. Summary of the T-peel strength data for Tape System 2

Sample Peel strength. kN/m Peel Strength. Ibf/in CoV^ Failure

Set No. min max mean min max mean % Mode'

17 0.89 0.99 0.94 0.05 5,1 5.6 5.4 0.28 5.1 2

18 0.17 0.20 0.19 0,02 0,9 1.1 1.1 0.09 8.5 2

19 0.20 0.36 0.30 0.07 1.2 2.0 1.7 0.40 23.0 2 20 0.70 0.77 0.74 0.03 4.0 4.4 4.2 0.18 4.3 2

21 0.94 1.42 1.23 0.21 5.4 8,1 7.0 1,21 17.2 2 22 1.69 1.80 1.75 0.05 9,7 10,3 10.0 0,28 2.8 3 23 1.61 1.73 1.69 0.05 9,2 9.9 9.6 0,31 3.2 1 24 1.05 1.27 1.17 0.10 6,0 7.3 6.7 0.59 8.9 2 25 1.12 1.35 1.20 0.11 6,4 7.7 6.8 0.61 8.9 2 26 0.49 0.53 0.50 0.02 2,8 3.0 2.9 0,10 3.4 2 27 0.75 0.81 0.77 0.03 4,3 4.6 4.4 0,16 3.6 2

28 1.00 1.41 1.17 0.17 5,7 8,0 6.7 0.97 14.5 2 29 1.09 1.28 1.19 0.08 6,2 7.3 6.8 0.45 6.6 2 30 2.20 2.45 2.32 0.12 12,5 14,0 13.3 0.71 5.4 3 31 2.05 2.20 2.13 0.06 11,7 12.6 12.1 0.34 2.8 3 32 1.24 1.63 1.40 0.17 7,1 9.3 8.0 0.96 12.0 2 49 0.39 0.66 0.54 0.11 2.2 3.8 3.1 0.64 20.9 2 50 0.16 0.19 0.18 0.01 0.9 1.1 1.0 0.06 6.3 2

51 0.02 0.09 0.07 0,03 0.1 0.5 0.4 0.18 46.7 2 52 0.69 0.77 0.73 0.04 3.9 4.4 4.2 0.23 5.6 2 53 1.60 1.92 1.76 0.13 9.1 10.9 10.1 0.75 7.4 2 54 1.45 1.79 1.59 0.16 8.3 10.2 9.1 0.89 9.8 2 55 2.27 2.38 2.31 0.05 12.9 13.6 13.2 0.29 2.2 1 56 0.95 1.17 1.07 0.10 5.4 6.7 6.1 0.56 9.2 2 57 0.55 0.71 0.63 0,09 3.2 4,1 3.6 0.49 13.7 2 58 0.50 0.58 0.53 0.04 2.9 3,3 3.1 0.20 6.6 2 59 0.23 0.29 0.25 0.02 1.3 1,6 1.5 0.14 9.6 2 60 1.03 1.34 1.12 0.15 5.9 7.7 6.4 0.83 12.9 2

61 1.55 1.91 1.69 0.16 8.8 10.9 9.7 0.89 9.2 3 62 1.97 2.19 2.08 0.09 11.2 12.5 11.9 0.53 4.4 3 63 2.26 2.36 2.30 0.04 12.9 13.5 13.1 0.25 1.9 3 64 1.14 1.42 1.27 0.12 6.5 8.1 7.2 0.67 9.3 2

*sd indicates standard deviation. ''CoV indicates coefficient of variation. 'Failure mode: 1 = cohesive; 2 = adhesive; 3 = mixed.

21
high pressure, and long time-at-temperature had relatively high strength (fifth combination from

the right in Figure 3).

4.4 Failure Mode During Creep-Rupture and Peel-Strength Measurements

Examination of the failure modes in Tables 5 A and 5B for the creep-rupture sample sets and

Tables 6A and 6B for the peel-strength sample sets shows that the vast majority failed adhesively or in a mixed mode (i.e., some areas of the specimen bond failing cohesively and others

adhesively). Specimens prepared without primer or with contaminated EPDM might be expected

to fail adhesively. In the Phase II Main Experiment, 75 % of the sample sets were prepared with

EPDM that was either unprimed or contaminated, or both. And, it was found that all specimens

in sets having both unprimed and contaminated EPDM failed adhesively in the creep-rupture and

peel-strength tests.

However, in contrast, only 8 % of the 32 tested sample sets (16 in creep and 16 in peel strength)

having primed, clean EPDM failed in a totally cohesive mode. For the creep-rupture

measurements, these were Sample Sets Nos. 15, 31, and 55; for the peel-strength measurements,

they were Sample Sets Nos. 6, 14, 15, 23, 38, 46, and 55. Note that only two of the seven samples sets (Nos. 15 and 55) that failed cohesively in peel strength also failed cohesively in creep; Sample Set No. 3 1 failed cohesively in creep, and in a mixed mode in peel. On the other

hand, no sample set prepared with primed, clean EPDM failed totally in an adhesive mode. Most

of them contained some specimens that failed cohesively and others that failed in a mixed mode

(with, in some cases, a few specimens that failed adhesively). In two instances (Sample Sets Nos.

39 and 47), all specimens having cleaned, primed EPDM failed in a mixed mode. The observation

that few primed, clean sample sets failed cohesively was in distinct contrast to the findings in Phase I, wherein almost all sample sets failed cohesively* [2,3].

Selected primed specimens, prepared using either clean or contaminated EPDM and which failed

adhesively, were examined with light microscopy at xlOO magnification to determine the locus of

adhesive failure. In the case of the TSl primed, clean specimens, the failure was between the tape

and the primer. The bonds between the clean EPDM and primer (and within the tape) were

apparently stronger than those between the tape and primer. In the case of the TSl primed,

contaminated specimens, two loci of failure were evidenced; between the EPDM and the primer,

and between the tape and the primer. No trend for one to predominate over the other in relation to the application conditions was observed. In contrast, the loci of failure for almost all TS2

primed specimens, whether clean or contaminated, were between the EPDM and the TS2 primer.

Statistical analysis of the creep-rupture data revealed that sample sets failing cohesively tended to have longer times-to-failure than those failing adhesively. Also, sample sets failing in a mixed

mode exhibited longer times-to-failure similar to those failing cohesively. The findings of this

analysis are implicit in the rank ordering of the times-to-failure given in the plot in Figure 2. The

data points for unprimed, contaminated sample sets, which failed adhesively, are found on the left side of the plot; whereas the data points for the primed, clean sample sets, which failed mainly

cohesively or in a mixed mode, are situated on the right side of the plot.

One TS2 sample set failed adhesively in Phase I, but that failure was attributed to preparing specimens with

primer that had reached the end of its shelf life [3].

22
One question was why the primed, clean sample sets in the Phase 11 Main Experiment underwent

relatively few cohesive failures, while in Phase I such sample sets almost always failed cohesively.

A possible reason was that the failure mode was influenced by the high and low application

temperatures and pressures (Table 1) used in preparing the Phase II specimens. In Phase I, the

specimens were prepared at room temperature, about 23 °C (73 °F), using cleaned, primed

EPDM; the application pressure was 0.7 MPa (100 Ibf/in^). That is, none of the specimens in the

Phase II Main Experiment were prepared using the same application conditions of Phase I. Thus,

additional sets of TSl and TS2 specimens were prepared using the Phase II materials and the

Phase I application conditions. The availability of these sample sets allowed for a comparison of

times-to-failure and peel strengths of Phase I and Phase II specimens prepared under identical

application conditions.

The comparison between the times-to-failure and peel strengths of the Phase I and Phase II sample sets, made under identical application conditions, is summarized in Table 7. The creeprupture tests were performed at a load of 9.3 N (2. 1 Ibf), i.e., the single load used in Phase II. It is evident in Table 7 that the TS2 sample sets performed comparably in Phases I and II. With

regard to creep, the range and mean of the times-to-failure were slightly lower in Phase II than in Phase I. Although the mean values were statistically significantly different, no importance was

attached to the slight difference. With regard to peel strength, no significant difference was found

between the mean values, and the ranges were about the same. In both peel and creep, the failure

modes were cohesive. Because the TS2 data for specimens made under identical conditions were

similar in Phases I and II, no further comparative testing of TS2 specimens was conducted. These

results for TS2 suggested that the application factors such as temperature and pressure may have

influenced the failure mode of the TS2 primed, clean sample sets tested in the Phase II Main

Experiment (Sections 4.2 and 4.3). Further experimentation would be needed to provide a

definitive conclusion.

Table 7. Comparison between Phase I and Phase II times-to-failure and peel strengths

Time-to-Failure, hours Peel Strength. kN/m (\hmn)

Adh.

Syst. Phase min max mean^ CoV min max mean"* CoV

TSl I 39.28 59.06 44.42 14.6 1 1.79

(10.2)

1.82 (10.4)

1.81 (10.4)

0.9 1

TSl II 4.73 147.0 52.22 132 1,2,3 1.28

(7.30)

1.73 (9.90)

1.55 (8.87)

11.4 1,2,3

TS2 I 66.14 105.1 89.33 17.1 1 2.05

(11.7)

2.42

(13.8)

2.25

(12.8)

6.6 1

TS2 II 51.40 74.15 61.41 12.4 1 2.17

(12.4)

2.32

(13.2)

2.23

(12.7)

3.2 1

'Average of seven or eight specimens.

'CoV indicates coefficient of variation. 'FM indicates failure mode; 1 = cohesive, 2 = adhesive, and 3 = mixed.

Average of four or five specimens.

23
In contrast to the TS2 results, it is evident in Table 7 that the TSl sample sets did not perform

comparably in Phases I and II. Although the mean times-to-failure of the Phase I and Phase II sample sets (i.e., 44 versus 52 hours) were not significantly different, the time-to-failure ranges were very different. Most notably, for the Phase II set, the range was from 4.7 hours to 147

hours, which resuhed in a coefficient of variation (CoV) of 132 %. The Phase I sample set showed a range of 39 hours to 59 hours with a CoV of 14.6 %. Also, for the Phase II sample set, the failure mode was variable—^three specimens failed cohesively, three adhesively, and one

mixed. All Phase I specimens failed cohesively. Moreover, the Phase II specimens that failed

adhesively had a mean time-to-failure of about 5 hours; whereas those that failed cohesively and

mixed had a mean time-to-failure of about 1 00 hours. These observations regarding differences

between the TS 1 results in Phases I and II suggest that, when comparisons of creep rupture data

are made between replicate sample sets, it may be necessary to compare more parameters than

mean time-to-failure to judge whether the data are similar.

The mean peel strength of the TSl Phase II sample set was about 15 percent less (the difference

was statistically significant) than that of the Phase I sample set. Although this small difference

was not, in itself, considered to be notable, the failure modes for the Phase II peel specimens were

cohesive, adhesive, or mixed—as was found for the creep-rupture specimens. Again, this was in

contrast with the Phase I specimens that failed cohesively during peel-strength measurements.

From the data and failure modes in Table 7, some difference in behavior between the Phase I and

Phase II TSl sample sets (prepared using the same conditions) was occurring. One hypothesis as

to the cause(s) was that the TSl primer from Phase I used preparing Phase II specimens (Section

3.1) was beyond its shelf life. Thus, a new batch of TSl primer was obtained, and an additional

set of TSl specimens was prepared using the Phase I application conditions. However, the creeprupture and peel-strength results fi"om this sample set and those of the TSl Phase II sample set (Table 7) were about the same. This observation suggested that the primer was not the cause.

Another hypothesis as to the cause of the variability between the TS 1 Phase I and Phase II data

was that the laboratory application technique had been unknowingly altered so that some TSl

Phase II specimens had failed adhesively. An experiment was needed to investigate the variability

of the TSl results.

The experiment and results are described in Appendix C. In summary, it was found that tape was

primarily responsible for the TSl variability, and little effect due to primer was observed. It was

also seen that the TSl sample sets in the experiment were statistically longer lived than the

minimum mean times-to-failure of three sets of well prepared liquid-adhesive-bonded specimens

from Phase I.

24
5. SUMMARY AND CONCLUSIONS

Tape adhesive systems are being used increasingly for preparing seams of EPDM roofing

membranes. An industry-government consortium study is underway to develop nonproprietary

data on tape-bonded seam performance. In Phase I, the creep-rupture response (time-to-failure)

of tape-bonded seam specimens subjected to various peel loads under ambient conditions was

compared to that of liquid-adhesive-bonded specimens. This report has described the results of

the Phase II research to study the effects of material and application factors on the peel-creeprupture response and peel strength of tape-bonded seam specimens. Two material factors—tape

system and tape thickness—and five application factors—EPDM surface condition, primer,

application temperature, application pressure, and time-at-application temperature—were

investigated in a statistically designed experiment. Two commercial tape systems were included

and the tapes had thicknesses of approximately 0.9 mm (0.035 in) or approximately 0.6 mm

(0.025 in). Because the thicker tapes had thicknesses typical of those commercially available at the time of the study, they were designated as having 'standard' thickness. The two levels at which each application factor was examined were chosen to represent, for the most part, the

range of commercial practice. Thus, specimens were prepared either primed or unprimed using

EPDM that was either clean or contaminated. Application temperatures were low, 5 °C (41 °F), or high, 60 °C (140 °F), and application pressures were low, 0.2 MPa (30 Ibfi'in^), or high, 2 MPa

(300 Ibfi'in^). And, the time at which the specimens remained at the application temperature were

either short, about 24 hours, or long, 672-960 hours.

The T-peel strengths and times-to-failure were determined at room temperature. The creep load

was 9.3 N (2.1 Ibf). To interpret the data, plots of mean time-to-failure and mean peel strength versus the combinations of application factors for each of the four pairs of tape system and tape

thickness were analyzed. Comparisons of times-to-failure between the tape-bonded sample sets were made with those of well prepared liquid-adhesive-bonded sample sets from Phase I. In recent years, field experience with liquid-adhesive-bonded seams has been, in most cases,

satisfactory. Consequently, the laboratory-measured times-to-failure of well prepared liquidadhesive-bonded specimens were taken as the benchmark for acceptable creep lifetimes. The

main conclusions regarding tape-bonded seams from the Phase II experimentation were that:

• Primed, clean EPDMprovided the longest times-to-failure and highest peel strengths. These

findings were consistent with manufacturers' recommendations for 'good application practice'

that require seams be primed and cleaned during fabrication. The findings are important

because they quantify such recommendations and emphasize the importance that they be

followed.

• Primed, clean EPDMand 'standard thickness tape ' afforded times-to-failure that were

statistically significantly higher than minimum mean times-to-failure ofwell prepared Uquidadhesive-bonded specimens investigated in Phase I. This result fi"om Phase II reinforces the

main conclusion from Phase I; that is, well prepared tape-bonded seam specimens of the type

in this study have satisfactory creep lifetimes in that, in most cases, they are comparable to, or

greater than, those of well prepared liquid-adhesive-bonded specimens.

• Application temperatures and application pressures used in the investigation did not affect

the times-to-failure ofspecimens prepared with primed, clean EPDM, that had, as stated,

relatively long times-tofailure. This is important as it indicates that tape-bonded seams can be

expected to have satisfactory creep lifetimes when prepared over a routinely encountered

25
range of application temperatures, i.e., 5 °C to 60 °C (41 °F to 140 °F), and

pressures—factors that can be uncontrollable in practice.

• 'Standard' thickness tape provided significantly longer times-to-failiire than thinner tape.

The thickness of the 'standard thickness' tapes were typical of those used in practice at the

time of the study, and no evidence was obtained that, for the two tape systems, thinner tapes

should be used.

• The two tape systems generally responded similarly tofactors that promoted either shorter or

longer times-tofailure.

In addition to these main conclusions, it was found that different batches of tape and primer of one tape system provided seam sample sets having variable times-to-failure. Investigation of the cause indicated that the tape was primarily responsible; no substantial effect due to primer was

observed. Investigations on the variability of the tape were beyond the scope of the project.

Although variable, sample sets prepared with this tape system had mean times-to-failure that were

statistically longer than the minimum mean times-to-failure of three sets of well prepared liquidadhesive-bonded specimens from Phase I.

26
6. ACKNOWLEDGMENTS

The research described in this paper was jointly sponsored by NIST and the CRADA members.

The authors acknowledge with thanks the support of the CRADA organizations and their

representatives: Dennis Fisher (Adco), David Hatgas (Ashland), Daniel Cotsakis (Carlisle

SynTec), Chester Chmiel (Firestone), Michael Hubbard (GenFlex), William Cullen and Thomas

Smith (NRCA), and Joe Hale (RCI). The authors also thank their NIST colleagues who

contributed to the study. Jack Lee assisted with the creep-rupture and peel-strength

measurements. Joannie Chin, Geoffrey Frohnsdorff, Jonathan Martin, Carl Schultheisz, and

Shyam Sunder provided many noteworthy comments in reviewing this report.

27

7. REFERENCES

[1] Russo, Michael, "More Business, Higher Profits, Heavier Fines," RSI Magazine, Vol. 73,

No. 2 (February 1995), pp. 34, 36, 38, & 40.

[2] Rossiter, Walter J., Jr., Lechner James A., Seiler, James F., Jr., and Embree, Edward,

"Performance of Tape-Bonded Seams of EPDM Membranes: Initial Characterization,"

Proceedings, 11th Conference on Roofing Technology, U.S. National Roofing Contractors

Association, Rosemont, IL (September 1995), pp. 78-89.

[3] Rossiter, Walter J., Jr., Vangel, Mark G., Embree, Edward, Kraft, Kevin M., and Seiler,

James F., Jr., "Performance of Tape-Bonded Seams of EPDM Membranes: Comparison of

the Peel Creep-Rupture Response of Tape-Bonded and Liquid-Adhesive-Bonded Seams,"

Building Science Series 175, National Institute of Standards and Technology (May 1996),

73 pages.

[4] Rossiter, Walter J., Jr., Martin, Jonathan W., Lechner, James A., Embree, Edward, and

Seiler, James F., Jr., "Effect of Adhesive Thickness and Surface Cleanness on CreepRupture Performance of EPDM Peel and Lap-Shear Joints," Roofing Research and

Standards Development: 3rd Volume, ASTM STP 1224, American Society for Testing and

Materials, West Conshohocken, PA (June 1994), pp. 123-138.

[5] Martin, Jonathan W., Embree, Edward, Stutzman, Paul E., and Lechner, James A.,

"Strength and Creep-Rupture Properties of Adhesive-Bonded EPDM Joints Stressed in Peel," Building Science Series 169, National Institute of Standards and Technology,

Gaithersburg, MD (May 1990), 59 pages.

[6] Martin, Jonathan W., Rossiter, Walter J., Jr., and Embree, Edward, "Factors Affecting the

Strength and Creep-Rupture Properties of EPDM Joints," Proceedings, Third International

Symposium on Roofing Technology, U.S. National Roofing Contractors Association,

Rosemont, IL (April 1991), pp. 63-71.

[7] Rossiter, Walter J., Jr., Martin, Jonathan W., Embree, Edward, Seiler, James F., Jr., Byrd,

W. Eric, and Ream, Ed, "The Effect of Ozone on the Creep-Rupture of Butyl-Adhered

EPDM Seam Specimens," Proceedings, 10th Conference on Roofing Technology, U.S.

National Roofing Contractors Association, Rosemont, EL (April 1993), pp. 85-92.

[8] Martin, Jonathan W., Embree, Edward, and Bentz, Dale P., "Effect of Time and Stress on

the Time-to-Failure of EPDM T-Peel Joints," Proceedings, 8th Conference on Roofing

Technology, U.S. National Roofing Contractors Association, Rosemont, IL (April 1987),

pp. 69-74.

29
[9] Rossiter, Walter J., Jr., Nguyen, Tinh, Byrd, W. Eric, Seiler, James F., Jr., Lechner, James

A., and Bailey, David M., "Cleaning Aged EPDM Rubber Roofing Membrane Material for

Patching: Laboratory Investigations and Recommendations," USACERL Technical Report

FM-92/05, U.S. Army Construction Engineering Research Laboratory, Champaign, EL

(August 1992), 58 pages.

[10] Strong, Alan, "Factors Influencing the Joining of Vulcanized Rubber Membranes," Paper

No. 60, Proceedings, ACS Rubber Division Meeting, American Chemical Society,

Washington, DC (1982).

[1 1] ASTM E 104 - 85 (Reapproved 1991), "Standard practice for Maintaining Constant

Relative Humidity by Means of Aqueous Solutions," Annual Book of Standards, Vol.

08.03, American Society for Testing and Materials, West Conshohocken, PA (1995).

30
APPENDIX A. SPECIMEN PREPARATION

This appendix describes specimen preparation. As indicated in the main text, two material factors

(tape system and thicicness) and five application factors (EPDM surface condition, primer,

application temperature and pressure, and time-at-temperature) were investigated in the Phase II Main Experiment (Table 1). The general specimen preparation conditions and procedures have

been previously described [2,4], and were followed in preparing the Phase II specimens.

Al. SPECIMEN MATERIALS AND DIMENSIONS

Two tape systems (TSl and TS2) were used to prepare T-peel seam specimens having dimensions

of 25 mm by 125 mm (1 in by 5 in) with a 75 mm (3 in) length bonded with tape. The tapes were

75 mm (3 in) in width. The EPDM rubber sheet having a nominal thickness of 1.5 mm (0.060 in)

was a commercial nonreinforced product amply covered on its surfaces with a talc-like release

agent. For each tape system, the tapes were supplied at two thicknesses, designated standard and

thin. The thicknesses of the 'standard thickness' tapes were generally 0.9 mm to 1.0 mm

(0.035 in to 0.040 in). These tapes were commercial products. The thicknesses of the 'thin' tapes were generally 0.5 mm to 0.6 mm (0.020 in to 0.025 in). These 'thin' tapes were

noncommercial products manufactured specifically for the Phase II investigations. In all cases, before a specimen was subjected to either a peel-strength or creep-rupture test, the thickness of

the tape was measured using the procedure described in Rossiter et al. [4]. Thickness

measurements of the creep-rupture specimens are included Appendix B.

A2. RUBBER SURFACE CONDITION

The surfaces of the EPDM rubber sheets used to prepare the T-peel specimens were designated

either clean or contaminated. In the case of the 'clean' surface, the as-received EPDM was first washed with Sparkleen-brand laboratory detergent in tap water, rinsed, and dried overnight or

longer. Just before fabrication of the seam specimens, the EPDM surface was further cleaned by

wiping with a cloth soaked in heptane. The procedure has been described in Rossiter et al. [4].

In the case of the 'contaminated' surface, the coverage of the release agent on the as-received

EPDM appeared to be sufficiently uniform that it could be used directly for specimen preparation.

However, because of the ample amount of release agent on the EPDM surfaces, neither the TSl

nor the TS2 tapes would adhere to the as-received EPDM. Thus, some release agent was

removed using the following procedure. A strip of 75 mm (3 in) wide masking tape was placed on the bonding area (fig. Al) of a 150 mm by 200 mm (6 in by 8 in) piece of as-received EPDM.*

Then, a 4.7 kg brass cylinder with a diameter of 75 mm (3 in) and a length of 1 19 mm (4.75 in)

was slowly (< 5 s) rolled back and forth once across the masking tape. When the masking tape

was peeled from the as-received EPDM, some release agent was removed fi"om the EPDM

surface. As a result, both tapes could now be bonded to the EPDM surface, which was

designated as contaminated.

The 25 mm by 1 25 mm (1 in by 5 in) T-peel specimens were subsequently cut from the sections of specimens

prepared using the 1 50 mm by 200 mm (6 in by 8 in) piece of EPDM.

Al
200 mm (8 in)

Bonding Section

75 mm (3 in) by

200 mm (8 in)

150 mm (6 in)

Figure Al. Plan view of a piece of EPDM used in specimen preparation.

The EPDM surface condition, i.e., clean or contaminated, was quantified by the technique

described in Martin et al. [5,6]. This technique uses computer-image processing to measure the

reflectance of tungsten light from the surfaces of the EPDM rubber strips. Light reflection from

the black EPDM surface increases with increasing contamination by the white release-agent

particles. Reflectance is quantified according to a grayscale output from the image processor.

The grayscale value is zero for black and 255 for a white surface. Forty grayscale measurements were made over the 75 mm by 200 mm (3 in by 8 in) bonding area of the EPDM (fig. Al). Only

about 5 percent of the cleaned pieces of EPDM were quantified, as past NIST experience has

indicated that the cleaning procedure produces uniform surfaces from specimen to specimen [4].

The average grayscale values of these clean surfaces were in the range of 38-42, with a coefficient

of variation of less than 10 percent. This range was similar to those values (i.e., 30-33, and 38) in previous NIST studies [2,4,5]. For contaminated specimens, the average grayscale values of the

EPDM were in the range of 130 to 150, with a coefficient of variation of 12 percent or less. Tables Bl and B2 contain the grayscale values for the TSl and TS2 specimens, respectively, used

in the creep-rupture tests. Note in the tables that a nominal value of 40 was assigned for the clean

specimens, because it was the mid-range value for those that were measured.

A3. PRIMER

Specimens were designated 'primed' and 'unprimed.' When 'unprimed,' the tape was applied

directly to either the clean or contaminated EPDM surface. When 'primed,' the thicknesses of the

primer were in accordance with each tape manufacturer's instructions: about 0.07 mm and

0.04 mm (0.0028 in and 0.0014 in) for Tape System 1 and Tape System 2, respectively. To

A2
control the thickness, a drawdown blade technique* with the EPDM held firmly on a vacuum table

was used [Al].

A4. TEMPERATURE

A4.1 High Temperature

For the hot temperature application, the EPDM (fig. Al) and tape pieces, 225 mm (9 in) in length, were placed in an oven at 60 °C ± 2 °C (140 °F ± 4 °F) for a minimum of 24 hours. The primer

was left at room temperature for safety purposes. A heated vacuum table, set close to the oven,

provided a working area to apply the primer and tape to the rubber. Two hot plates were covered

with a 250 mm by 300 mm by 6 mm (10 in by 12 in by 0.25 in) aluminum plate on which the

vacuum table was placed. The hot plates were heated such that a Type K (chromel-alumel)

thermocouple placed between the vacuum table and piece of rubber registered 60 °C ± 3 °C

(140 °F ± 5 °F). Additionally, a second aluminum plate with dimensions of 200 mm by 250 mm

by 6 mm (8 in by 10 in by 0.25 in) was set on a single hot plate, which was heated such that a Type K thermocouple placed between the plate and a piece of rubber on it read 60 °C ± 3 °C

(140 °F ± 5 °F). This plate was used to maintain the temperature of one of the mating pieces of

EPDM while the second was being primed.

In preparing a specimen, a preheated piece of EPDM was removed from the oven and set on the

vacuum table where it remained for about 3 minutes before application of the tape and primer (if

used). When primer was used, the solvent was allowed to evaporate for about 3 minutes before

the tape was applied to the primed EPDM. Then the tape/EPDM piece was transferred to the

heated aluminum plate where it was kept hot until the mating piece of EPDM was primed. After

solvent in the primer was judged to have evaporated from the second piece of primed EPDM

(about 3 minutes), the two were mated and immediately transferred to a pneumatic press for

pressure application (Section A5).

In cases where the specimen was not primed, the first piece of EPDM was set on the heated

vacuum table after removal from the oven. After 3 minutes, preheated tape was applied, and then

another piece of EPDM was removed fi"om the oven and mated directly with that covered with

the tape. The mated pieces were immediately transferred to the press for pressure application.

A4.2 Low Temperature

For the low temperature application, a top-opening refrigerator with interior dimensions of

1270 mm by 457 mm by 610 mm depth (50 in by 18 in by 24 in depth) provided the cold working

area. All materials, i.e., EPDM, tapes, and primers, were set on the bottom of the chamber along

with the vacuum table. The temperature of the chamber was set at 5 °C ± 2 °C (41 °F ± 3 °F),

and was measured with a Type K thermocouple placed between the vacuum table and a piece of

EPDM set on it. The materials were placed in the refrigerator over night before the specimens were prepared. When preparing the specimens, the lid of the refrigerator was open, and work

was conducted by leaning into the chamber. Condensation was not visible on the lower walls of

*This technique uses an adjustable knife blade (i.e., the drawdown blade), bar, or rod to spread the adhesive or primer on a substrate [Al]. The thickness is controlled by the distance between the blade edge and the substrate surface.

A3
the chamber, or on any materials, during specimen preparation. It was visible at times on the

walls of the chamber near the top opening. The tapes and primers (if used) were applied to pieces

of EPDM placed on the vacuum table. Evaporation of primer solvent required about 25 minutes

(as judged by pressing on the primed rubber with a finger) before the tape was put in place. After

the two pieces of EPDM were mated together, the specimen was immediately transferred to the

pneumatic press for pressure application.

A5. PRESSURE

The specimens were pressed together using a pneumatic press as described in Rossiter et al. [2].

Two pressures, designated high and low, were used in the study: 2 MPa (300 Ibf/in^) and

0.2 MPa (30 Ibf'in^), respectively. The time of pressure application was about 10 s. Immediately

after pressure application, the specimens were returned to either an oven or refrigerator where

they remained for the pre-selected time (Section A6) before conducting the creep-rupture and

peel-strength tests.

A6. TIME-AT-TEMPERATURE

'Time-at-temperature' means holding the completed specimen at the preparation temperature for a specified duration. Two times-at-temperature were specified and designated short and long.

The 'short' time-at-temperature was between 20 hours and 24 hours; i.e., about over night. After

the short time-at-temperature elapsed, the specimens were kept at room temperature until tested.

The 'long' time-at-temperature was essentially the period between specimen preparation and

testing, and ranged from 672 hours to 960 hours (28 days to 40 days). However, in this latter case, both creep-rupture and peel-strength specimens were kept at room temperature over night

before the tests were conducted.

A7. APPENDIX REFERENCE '

[Al] Landrock, Arthur H., Adhesives Technology Handbook, Noyers Publications, Park Ridge,

NJ(1985), p. 208.

A4
APPENDIX B. CREEP-RUPTURE DATA DEVELOPED IN MAIN EXPERIMENT

This Appendix contains the time-to-failure (TTF) data developed in the Phase II Main Experiment. All

specimens were tested at a load of 9.3 N (2. 1 Ibf). The following codes and abbreviations are used in the tables.

Column Number Information Given in the Column

1 Sample Set Number (Set No.); it corresponds to the set number given in Table 1 of the main text.

2 Replicate Number of the Sample Set (Set Rep); it was included in the table in

the event that more than one sample set was tested.

3 Specimen Number (No.); each specimen was assigned a unique number.

4 TS Number (No.); 1 = Tape System 1; 2 = Tape System 2.

5/6 Tape Thickness in millimeters (mm); Tape Thickness in inches (in).

7 Surface Condition (Cond); specimens were either clean or contaminated (cont.).

8 Gray Scale (GS) of the rubber; clean specimens were assigned a value of 40;

gray scales of the contaminated specimens were measured.

9 Application Pressure (Press); high = 2 MPa (300 Ibfin^); low = 0.2 MPa

(30 IbC^in').

10 Application Temperature (Temp); high = 60 °C (140 °F); low = 5 °C (41 °F).

1 1 Time-at-Application-Temperature (Time-at-Temp); short = 20 hours to 24

hours; long = 672 hours to 960 hours.

12 Primer: indicates whether the specimen was primed (Yes) or not primed (No).

13 Time-to-Failure (TTF).

14 Failure Mode (FM), indicates whether the predominant mode of failure was

cohesive (1), adhesive (2), or a combination of the two (3).

Bl
able B 1 . Creep-rupture data developed for Tape System 1 in the Main Experiment

Set No.

Set RepSpecimen

No. TSNo. Tape Thickness Surface ADDlication Time-atTemp Primer

TTF

mm in Cond OS Press Temp hours FM

1B63-27 0.724 0.029 Cont. 145 High High Short Yes 1 743

1R63-2S 0.673 0.027 Cont. 145 High High Yes 1 Q7R

1 1 1B63-26 1 0.676 0.027 Cont. 145 High High Short Yes 2.365 3

J ]

1B63-24

[

0.660 0.026 Cont. 145 High High Short Yes 3.639 3 1B62-15 0.619 0.024 Cont. 149 High High Short Yes 4.266 3 1R62-20 0.667 0.026 Cont. 149 High High Short Yes 4 361 3 1R63-23 0.648 0.026 Cont. 145 High High Short Yes 4.451 3 1B62-19 0.600 0.024 Cont. 149 High High Short Yes 4.946 3

2 2R3R-36 0.613 0.024 Cont. 146 High Low Short No 6 371 9

9 0.584 0.023 Cont. 137 High Low olUJX I O. J /9 2 1 2B37-35 1 0.613 0.024 Cont. 146 High Low Short No 6.381 2

2 2B38-40 0.597 0.024 Cont. 146 High Low Short No 6.383 2

9 O J o 0.616 0.024 Cont. 146 High Low OlltJl L Mn 9 0.610 0.024 Cont. 146 High Low ftL). JOH "^Rd 9 2 2B36-27 0.625 0.025 Cont. 137 High Low Short No 6.384 2

2 2R36-22 0.622 0.025 Cont. 137 High Low Short No 6.394 2

3 3B54-5 0.702 0.028 Cont. 136 Low High Short No 0.049 2

3 3B54-6 0.676 0.027 Cont. 136 Low High Short No 0.050 2

3 1 3B55-11 1 0.657 0.026 Cont. 139 Low High Short No 0.056 2

3 3B55-12 0.641 0.025 Cont. 139 Low High Short No 0.058 2

3 [ [ 0.651 0.026 Cont. 139 Low High Short No 0.064 2

3 0.699 0.028 Cont. 139 Low High Short No 0.065 2

3 3RS4-7 0.711 0.028 Cont. 136 Low High Short No 0.068 2

3 3355-9 0.679 0.027 Cont. 139 Low High Short No 0,070 2

4 4B44-40 0.737 0.029 Cont. 147 Low Low Short Yes 7.348 2 4 4B39-2 0.740 0.029 Cont. 140 Low Low Short Yes 7.689 2 4 1 4B42-24 I 0.714 0.028 Cont. 140 Low Low Short Yes 7.850 2 4

J

4B44-42 0.645 0.025 Cont. 147 Low Low Short Yes 8.351 2 4 4B39-7 J 0.721 0.028 Cont. 140 Low Low Short Yes 8.526 2 4 4B44-37 0.71

0.028 Cont. 147 Low Low Short Yes 9.330 2 4 4R42-26 0.71

0.028 Cont. 140 Low Low Short Yes 9.668 2 4 4R49.97 0.714 0.028 Cont. 140 Low Low Short Yes 1 1.959 2

0.603 0.024 Clean 40 High High Short No 0.385 2 0.606 0.024 Clean 40 High High Short No 0.408 2

5 5B4-9 0.625 0.025 Clean 40 High High Short No 0.443 2

0.613 0.024 Clean 40 High High onon INO 9

5 5B5-20 0.594 0.023 Clean 40 High High Short No 0.610 2

5 5B5-19 0.594 0.023 Clean 40 High High Short No 0.616 2

5 5B4-8 0.619 0.024 Clean 40 High High Short No 0.651 2

5 5B5-17 0.610 0.024 Clean 40 High High Short No 0.989 2

B2 — Tape System 1
Set No.

Set Rep

Specimen

No. TS

No. Tape Thickness Surface Application Time-atTemp Primer

TTF

mm m Cond GS Press hours FM

6 6B26-3» 0.413 0,016 Clean 40 High Low Short Yes 2,756 1 6 6B26-4

0.676 0,027 Clean 40 High Low Short Yes 3,437 1 6 0024-2/

J

0 718 40 mgn Low Short Yes 6,994 2 6 \ 6B24-23 0.333 0.013 Clean 40 High Low Short Yes 8,754 3 6 6B25-30 0.714 0,028 Clean 40 High Low Short Yes 9,085 3 o Am 1 1 0.654 0.026 Clean 40 High Low bnort Yes 1 A TOO ID, /zy 3 O 0.673 0.027 Clean 40 High Low oiiort Yes 11 \ A A

1 1 , 144 J o Ot>Z4-Z4 0.664 0,026 Clean 40 High Low onori Yes 11 T3'7

1 1 ,ZJ / 1

1 /B 1 1 - 1 y 0.752 0.030 Clean 40 Low High J^tiort Yes 3,yyy z

1 /Bl 1-2U 0.733 0.029 Clean 40 Low High Snort Yes A COOz

1 /Bl 1-1 J 0 7?7 0 07Q 40 T r*\Ji/ i_**JW mgn Snort Ye.s j,zz6 z 1 7B11-21 0.730 0.029 Clean 40 Low High Short Yes 5,346 2 7 7B10-13 0.692 0.027 Clean 40 Low High Short Yes 5,663 2

7 /By-l 0,702 0.028 Clean 40 Low High Snort Yes 7. /36 2

/ /By- / 0.737 0.029 Clean 40 Low High Snort Yes O CO A J

/ /By-o 0.749 0.030 Clean 40 Low High Snort Yes y.yjo

oo sBl /-2 1 0.538 0.021 Clean 40 Low Low Snort No A O O A 0.2o6 z

oO oB 1 / - 1 1) 0.553 0.022 Clean 40 Low Low onort JNo A "ICiA z

oO CD 1 ^ 1 O oBlD-12 0 563 0 09? Clean 40 T ow T cwv bnort No U.3 JO z 8 j 8B16-14 0.573 0.023 Clean 40 Low Low Short No 0.365 2 8 SB 16-8 0.585 0.023 Clean 40 Low Low Short No 0.463 2 6 oBl j-3 0.535 0.021 Clean 40 Low Low bnoiT XT/-. INO n A Qi Z Q

O OD 1 C 0 oJdI J-/ 0.533 0.021 Clean 40 Low Low onon INO u.4y / Z

QO

fiR TAG 0.560 0.022 Clean 40 Low Low onon iNO U.Oj J Z

Q yv_-o 1 -z J 0.879 0.035 Cont. 148 High High onoR I es 1 u.yyj

Qy yco 1 -Zj 0.832 0.033 Cont. 148 High High onon 1 es Zj.UZJ

Q ycoj-jy 0.994 0.039 Cont. 143 Hieh Hish onon I es Zj. / jU

9 1 9C63-40 ] 0.953 0,038 Cont. 143 High High Short Yes 27.587 1 9 9C63-37 0.956 0.038 Cont. 143 High High Short Yes 28.513

Qy yL. jy- 1 z 1.019 0.040 Cont. 147 High High onon I es 18 "JO/I JO. JZ4 "JJ o open Q ycjy-y 1.073 0.042 Cont. 147 High High onon I es 4j.Oj J

TJ y y(-^Dj-jo 0.972 0.038 Cont. 143 High High onon I es A(^ "77^ 40. Z /O 11

1 u lApn iQ 1.016 0.040 Cont. 140 High Low onon INO D.4ZU z

1 n inr^-jT Q HJL.32-y 0.943 0.037 Cont. 141 High Low onon INO 0.4j0 z

1 (\ lU

1

1 C\C^1 1

'3 1UC3 1 -3 1.019 0.040 Cont. 132 High Low onon XTr^ INO A /I /in 0.44U z

10 10C33-16 0.991 0.039 Cont. 140 High Low Short No 6.465 2

10 10C33-17 0.962 0.038 Cont. 140 High Low Short No 6.473 2

10 10C31-5 1.051 0.041 Cont. 132 High Low Short No 6.484 2

10 10C32-10 1.026 0.040 Cont. 141 High Low Short No 6.489 2

10 10C31-1 0,972 0.038 Cont. 132 High Low Short No 6.516 2

B3 — Tape System 1
Set No.

Set RepSpecimen

No. TSNo. Tape Thickness Surface Aoolication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

11 J 11B54-15 1 .Uo4 U.U4Z Loot. 1/17 14 / Low High Short No 0.080 2

11 11B54-16 1 .(JjZ A A/1 1 U.U4

Lont. ^ An 14 / Low High Short No 0.133 2

11 11B55-24 1.016 0.040 Cont. 140 Low High Short No 0.133 2

11 1 11B55-26 1 1.057 0.042 Cent. 140 Low High Short No 0.170 2

11

J

11B55-25

[

1 1 AO U.044 Cont. 140 Low High Short No 0.170 2

1

11B55-27 l.UlO A AylA Cont. ^ Af\ 14U Low High Short No 0.201 2

11 11B54-20 1 .UUJ A A/IA U.U4U Lont. 1 A 114 / Low High Short No 0.241 2

11 11B52-5 J

1 A1 A r\Ar\ Lont. 1 /I "3 14j Low High Short No 0.244 2

12 12C37-1 1111 1.111 U.U44 r"/-vnt 1 ^lA

1 jU Low Low Short Yes 6.638 2 12 12C39-16 11

1 70 . 1 /z U.U40 Print 1 TO 1 jy Low Low Short Yes 5.972 2

12 12C37-2 1 1.111 0.044 Cont. 150 Low Low Short Yes 4.870 2 12 1 12C39-19 1 1.051 0.041 Cont. 139 Low Low Short Yes 7.199 2 12 12C37-4 1 . 1 Z / U.U44 Prvnt 1 ^A 1 jU Low Low Short Yes 4.022 2

12 [ 12C37-7 1 1 nfi1 . 1 Uo U.U44 L-ont. 1 "^A Low Low Short Yes 4.119 2

12 12C39-21 l.U/j A A/I 0 U.U4Z com. 1 TO 1 jy Low Low Short Yes 9.470 2 12 12C40-23 1 .usy A A/l '2 U.U4j Lont. 1 JO Low Low Short Yes 8.659 2

13 J 13C8-13 1 A 1 O 1 .u 1 y A r\Af\ Clean /I A4U /*V. High High Short No 1.743 2

13 J 13C8-8 J

1 A 1 A I .UlU A AylA Llean /I A4U High High Short No 2.398 2

13 1 13C9-17 0.968 0.038 Clean 40 High High Short No 2.655 2

13 1 13C8-12 1 1.003 0.040 Clean 40 High High Short No 2.785 2

13 13C7-4 1 .U ID A A/IA U.U4U Clean Af\ 4U Hign High Short No 2.945 2

13 ] 13C9-16 n Q77 u.y /z nU.Ujo ms Liean /I A4U Hign High Short No 3.181 2 13 13C9-21 U.UJo Pitman L-iean AC\ Hign High Short No 3.672 2

13 13C7-5 v^iean /I4UA Hign High Short No 5.970 2

14 14C28-25 nU. 710 / J\) u.UZ? PIClean /1A Hign Low Short Yes 7.794 1 14 1 14C29-30 n m 1 Liean /I A4U Hign Low Short Yes 11.125 1 14 14C29-32 0.816 0.032 Clean 40 High Low Short Yes 12.202 1 14 1 14C29-29 1 0.768 0.030 Clean 40 High Low Short Yes 16.531 1 14 14C29-33 U. /(Jo A AOO (J.UZo Clean /i A41) High Low Short Yes 20.331 1 14 j 14C28-22 [ (J. /4o A A7Q u.uzy Clean /I A4U High Low Short Yes 54.527 1 14 14C26-10 (J. /4j A AOQ u.uzy Clean /I A4U High Low Short Yes 143.854 3 14 14C26-12 A OOO A Al '2 Clean AC\ 4U High Low Short Yes 158.391 1

15 15C15-16 1 . 14U A A/l Clean /I A4U Low High Short Yes 84.214 1 15 15C13-7 1 n^7 1 .Uo / A A/1 7 U.U4Z Clean /I A4U Low High Short Yes 106.377 1 15 15C13-5 1.118 0.044 Clean 40 Low High Short Yes 114.425 1 15 15C15-17 1.124 0.044 Clean 40 TLow High Short Yes 130.008 1 15 15C13-1 1.099 0.043 Clean 40 Low High Short Yes 142.477 1 15 15C14-14 1.051 0.041 Clean 40 Low High Short Yes 144.875 1 15 15C14-11 1.124 0.044 Clean 40 Low High Short Yes 146.489 1 15 15C15-21 1.105 0.044 Clean 40 Low High Short Yes 152.213 1

B4 — Tape System 1
Set No.

Set Kcp

Specimen

No. TS

jNO.

Tape Thickness Surface Annlication Timc-atlemp j-'nmcr

TTi' mm in Cond GS Press Temp hours

16 1 16C24-39 1 0.998 0.039 Clean 40 Low Low Short No 0.668 2 16 1 16C24-38 1 0.993 0.039 Clean 40 Low Low Short No 0.704 2

16 1 16C24-41 1 0.978 0.038 Clean 40 Low Low Short No 0.791 2 16 16C24-37 1 0.988 0.039 Clean 40 Low Low Short No 0.884 2

16 16C23-32

\

0.990 0.039 Clean 40 Low Low Short No 1 . 1 40 2 16 I 16C23-30 0.970 0.038 Clean 40 Low Low Short No 1.351 2

16 1 16C23-33 1 0.995 0.039 Clean 40 Low Low Short No 2.150 2 16 1 16C21-17 1 0.968 0.038 Clean 40 Low Low Short No 2.462 2

33 1 33B61-10 1 0.606 0.024 Cont. 144 High Hiph Long Yes 1.406 3 33 1 33B61-13 1 0.597 0.024 Cont. 144 Hi eh High Long Yes 1.988 3 33 1 33B61-14 1 0.651 0.026 Cont. 144 High High Long Yes 3.218 3 33 33B61-9 0.638 0.025 Cont. 144 High High Long Yes 4.904 3 3j

!

J irJoU- /

J

0.619 0.024 Cont. 145 High High Long Yes 6.505 3 33 33B60-4 0.660 0.026 Cont. 145 High High Long Yes 13.817 3 33 1 33B60-5 1 0.657 0.026 Cont. 145 High High Long Yes 15.297 3 33 1 33B60-3 1 0.673 0.027 Cont. 145 High Hieh Long Yes 21.487 3

34 1 34B33-2 1 0.635 0.025 Cont. 150 Hieh Low Long No 6.342 2 34 1 34B35-19 1 0.654 0.026 Cont. 148 Hieh Low Long No 6.344 2 34 1 34B35-16 1 0.667 0.026 Cont. 148 High Low Long No 6.345 2 34 34B34-10 1 0.629 0.025 Cont. 150 High Low Long No 6.345 2 34

!

34B35-15

I

0.641 0.025 Cont. 148 High Low Long No 6.346 2 34 34B35-17 0.648 0.026 Cont. 148 High Low Long No 6.346 2 34 1 34B33-6 1 0.657 0.026 Cont. 150 High A AA^l Low Long No 6.347 2 34 1 34B34-13 1 0.632 0.025 Cont. 150 High Low Long No 6.348 2

35 1 35B56-21 1 0.581 0.023 Cont. 144 Low High A AA^A Long No 0.032 2 35 1 35B59-39 1 0.689 0.027 Cont. 139 Low High A AJ^l Long No 0.033 2 35 1 35B56-19 1 0.660 0.026 Cont. 144 Low High Long No 0.036 2 35 35B58-31 1 0.664 0.026 Cont. 144 Low High Long No 0.041 2 35

[

35B56-17

I

0.638 0.025 Cont. 144 Low Hieh Long No 0.044 2 35 35B58-29 0.619 0.024 Cont. 144 Low Hieh Long No 0.049 2 35 35B59-36 1 0.664 0.026 Cont. 139 Low Hieh Long No 0.050 2 35 1 35B59-40 1 0,686 0.027 Cont. 139 Low Hi eh Long No 0.051 2

36 1 36B41-20 1 0.737 0.029 Cont. 142 Low Low Long Yes 0.909 2 36 1 36B43-29 1 0.622 0.025 Cont. 146 Low Low Long Yes 3.378 2 36 1 36B43-32 ] 0.762 0.030 Cont. 146 Low Low Long Yes 2.152 2 36 36B41-21 0.749 0.030 Cont. 142 Low Low Long Yes 0.957 2 36 36B43-33 ; 0.676 0.027 Cont. 146 Low Low Long Yes 2.453 2 36 36B40-9 0.641 0.025 Cont. 141 Low Low Long Yes 1.386 2 36 36B43-34 0.765 0.030 Cont. 146 Low Low Long Yes 2.626 2 36 36B40-14 0.664 0.026 Cont. 141 Low Low Long Yes 0.728 2

B5 — Tape System 1
Set No.

Set Rep

Specimen

No. TSNo. Taoe Thickness Surface Aoolication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

37 1 37B46-8 1 0.552 0.022 Clean 40 Hi eh Long No 3.014 2 37 1 37B46-9 1 0.505 0.020 Clean 40 Hieh Hieh Long No 2.754 2 37 1 37B45-1 1 0.514 0.020 Clean 40 High High Long No 3.980 2 37 1 37B47-17 1 0.511 0.020 Clean 40 High High Long No 1.682 2 37

] 37B45-7

[

0 530 0 091 rienn 40 Hirugnah Hirugnah Long No 1.815 2 37 37B47-15 0 514 0 070 40 rugn Hirugnoh Long No 3.972 2 37 1 37B45-2 1 0vy.HOVj dRfi 0yj.yjmI Qy V_.lCall 40 rugn Hirugnoh Long No 1.861 2 37 1 37B47-20 1 0 01 Q 40 rugn Hirugnoh Long No 1.803 2

38 1 38B23-16 1 0 090 40 rugn J_/U W Long Yes 0.679 1 38 1 38B23-18 1 0 748 0 099 40 Hirugnah T r\\jii7 i_»U W Long Yes 1.277 1 38 1 38B21-4 1 0.588 0.023 Clean 40 High Low Long Yes 1.721 3 38 1 38B21-1 1 0.392 0.015 Clean 40 High Low Long Yes 1.728 3 38

J

38B21-3

J

0 47"? 0 01 Q I Call 40 Hirugnoh Low Long Yes 1.966 3 38 38B22-11 V_/.U 1 J 0 074 Clean 40 Hirugnoh Low Long Yes 2.045 3 38 1 38B23-20 1 0 094 40 Hirugnah Low Long Yes 2.150 3 38 1 38B23-21 1 0 710 0 098 40 Hirugnoh Low Long Yes 2.419 3

39 1 39B49-12 1 0 543 0 091 V-/ Ittill 40 T r\\7j Hiru^iah Long Yes 20.097 3 39 1 39B49-8 1 0.603 0.024 Clean 40 T nw Long Yes 21.026 3 39 1 39B50-16 1 0.641 0.025 Clean 40 Low High Long Yes 21.508 3 39 1 39B50-20 1 0.606 0.024 Clean 40 Low High Long Yes 26.359 3 39

]

39B48-1 0 f^OO 0 094 40 Low Hirugnoh Long Yes 29.438 3 39 39B49-13 J 0 f,7Q 0 09S Clean 40 Low Hirugnoh Long Yes 31.940 3 39 39B50-19 1 0VJ.VJHO fvAH 0 096 40 7JL/U W Hirugnah Long Yes 33.130 3 39 1 39B49-9 1 0 096 40 Low Hirugnoh Long Yes 35.272 3

40 1 40B 19-31 1 0.565 0.022 Clean 40 Low Low Long No 0.171 2 40 1 40B 19-30 1 0.595 0.023 Clean 40 Low Low Long No 0.225 2 40 1 40B20-39 1 0.580 0.023 Clean 40 Low Low Long No 0.226 2 40 40B20-36 1 0.603 0.024 Clean 40 Low Low Long No 0.277 2 40

j 40B 18-24[

0.585 0.023 Clean 40 Low Low Long No 0.292 2 40 40B20-37 0 580 0 023 Clean 40 Low Low Long No 0.294 2 40 1 40B20-41 1 0 09? 40 T cw\i i_/VJ w T rs\\T Long No 0.302 2 40 1 40B19-35 0 094 40 T r\\\7 vv T r\\Tu Long No 0.336 2

41 1 41C60-18 1 0 0'^^^ Cnnt 145 Hi ah Long Yes 37.062 3 41 1 41C60-19 1 yj.KJJyj Pnnt nigii Hirugnah Long Yes 54.797 3 41 1 41C60-17 1 0.822 0.032 Cont. 145 High High Long Yes 60.790 3 41

[

41C62-30

j

A Q7S A ATQ v-oni. 1

I AAn't Hirugnoh rugn Hi oh Long Yes 71.906 3 41 41C60-21 0.873 0.034 Cont. 145 High High Long Yes 74.698 3 41 41C62-31 1.003 0.040 Cont. 144 High High Long Yes 90.433 3 41 41C62-32 0.949 0.037 Cont. 144 High High Long Yes 102.70 3 41 41C58-7 0.959 0.038 Cont. 142 High High Long Yes 150.45 3

B6 — Tape System 1
Set No.

Set RepSpecimen

No. TSNo. Tape Thickness Surface Application Time-atTemp Primer

TTl' mm in Cond GS Press Temp hours FM

42 42C36-39 1 1.019 0.040 Cont. 144 High Low Nn 6 379 9 42 42C36-38 1 1.019 0.040 Cont. 144 High Low T An o No 6.381 2 42 42C34-23 1 0.987 0.039 Cont. 144 High Low T An o No 6.383 2 42 1 42C34-24 1 0.981 0.039 Cont. 144 High Low Long No 6.389 2 42

j

42C36-36 1 1.019 0.040 Cont. 144 High Low Long No 6.390 2 42 42C35-33 1 1 .022 A A /I A U.U4U Cont. ^ A 143 T T' L High Low Lont? No 6.399 2 42 1 1 .041 0.041 Cont. 144 T T 1 High Low Lone No 6.428 2 42 42C35-32 1 1 .029 A A y1 1 0.041 Cont. 143 T T' 1 High Low Lon2 No 7.197 2

43 43B53-8 1 0.948 0.037 Cont. 135 Low High I on 2 No 0.201 2 43 43B53-9 1 Q.921 0.037 Cont. 135 Low High No 0.237 2 43 43B56-29 1 0.930 0.037 Cont. 134 Low High T An o No 0 314 2 43 1 43B56-30 1 1.026 0.040 Cont. 134 Low High Long No 0.357 2 43

j

43B57-42 1 0.924 0.036 Cont. 146 Low High Long No 0.378 2 43 43B53-13 1 0.876 0.035 Cont. 135 Low High No 0.482 2 43 43B57-39 1 0.918 0.036 Cont. 146 Low High T one No 0.482 2 43 43B56-35 1 0.953 A A O O 0.038 Cont. 134 Low T T" L Lhgh No 0.722 2

44 44C42-42 1

1 AC yi 1.054 0.042 Cont.

^ A c 145 Low Low Lone Yes 4.81

2 44 44C41-32 1 1.146 0.045 Cont. 140 Low Low Lone Yes 5.526 2 44 44C38-12 1 1.187 0.047 Cont. 146 Low Low Lone Yes 7.508 2 44 1 44C38-8 1 1.130 0.045 Cont. 146 Low Low Long Yes 5.448 2 44

J

44C42-38 1 1.095 0.043 Cont. 145 Low Low Long Yes 6.411 2 44 44C41-33 1 1.127 0.044 Cont. 140 Low Low I one Yes 4.466 2 44 44C41-35 1 1.159 0.046 Cont. 140 Low Low T one Yes 6.359 2 44 44C42-37 1 l.1 1

0.044 Cont. 145 Low Low Long Yes 4.248 2

45 45C45-17 1 C\ QA<; u.yu-> U.Ujd dean 4U Tj; „Vi 1-hgh High Long No 26.528 2 45 1 45C45-20 1 O.Ojj Clean A A40 High High Long No 27.665 2 45 J 45C43-2 1 1.003 0.040 Clean 40 High High Lone No 22.424 2 45 1 45C44-12 1 0.937 0.037 Clean 40 High High Long No 36.261 2 45

[

45C45-21 1 Llean A A High High Long No 32.331 2 45 45C43-3 1 A OAA 0.899 A A*? C 0.035 Clean A A40 High High Lone No 34.510 2 45 45C44-9 1 A AO 0.933 A A") T 0.037 Clean A A40 T T' "U High T T' U High Lone No 56.189 2 45 45C45-16 1 0.908 0.036 Clean 40 High T T' 1 High Lone No 26.455 2

46 46C25-7 1 0.832 0.033 Clean 40 High Low Lone Yes 2.087 2 46 46C25-4 1 0.819 0.032 Clean 40 High Low Lone Yes 2.834 2 46 46C30-39 1 0.791 0.031 Clean 40 High Low Lone Yes 3.679 2 46 46C27-19 1 0.794 0.031 Clean 40 High Low Long Yes 3.991 2 46 46030-49 1 0.819 0.032 Clean 40 High Low T AnCT Yes 4*T, 178 I/O 9 46 46C30-36 1 0.797 0.031 Clean 40 High Low Long Yes 4.236 3 46 46C30-38 1 0.879 0.035 Clean 40 High Low Long Yes 5.258 3 46 46C25-5 1 0.778 0.031 Clean 40 High Low Long Yes 5.262 2

B7 — Tape System 1
Set No.

Set RepSpecimen

No. TSNo.

Taoe Thickness Surface AoDlication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

47 47C49-7 1 n c\A 1 U.U4

Clean 4U Low High Lone Yes 154.23 3 47 47C50-10 1

11 .Um1 nu U.U4U L-iean /I A Low TJirrV. Hign Long Yes 168.70 3 47 47C50-12 1 1.022 0.040 Clean 40 Low High Long Yes 182.45 3 47 1 47C51-19 1 1.057 0.042 Clean 40 Low High Long Yes 182.55 3 47

[

47C51-20 1 n QQ7 n\j.\)jy mo v^iean /I A Low High Long Yes 184.67 3 47 47C50-8 1 U.UJO v^iean 4A Low Hign Long Yes 192.78 3 47 1 47C50-13 1 U. 700 KJ.KJjy <^iean /1A Low Hign Long Yes 197.85 3 47 1 47C51-21 1 1 .U J J U.U4 1 Clean /I A Low Hign Long Yes 211.21 3

48 48C22-22 1 u.y 1 o U.UjD v^iean /I A Low Low Long No 0.371 2 48 48C22-25 1 A ATT L-iean /I A Low Low Long No 0.401 2 48 48C22-23 1 0.955 0.038 Clean 40 Low Low Long No 0.417 2 48

;

48C19-1 1 0.900 0.035 Llean 40 Low Low Long No 0.424 2 48 48C22-27 1 0.940 0.037 Clean 40 Low Low Long No 0.456 2 48 48C22-26 1 0.910 0.036 Clean 40 Low Low Long No 0.488 2 48 48C22-24 1 0.933 0.037 Clean 40 Low Low Long No 0.638 2 48 48C20-13 1 0.918 0.036 Clean 40 Low Low Long No 0.786 2

B8 — Tape System 1
Table B2. Creep-rupture data developed for Tape System 2 in the Main Experiment

Set Set Specimen TS Tape Thickness Surface Application Time-at- T'1'1'' XTNo. Rep No. No. mm in Cond GS Press Temp Temp Primer hours

17 1 17E1-27 2 0.559 0.022 Cont, 137 High High Short Yes 1.421 2 17 1 17E3-39 2 0.556 0.022 Cont. 145 High High Short Yes 3.222 2

17 1 17E53-17 2 0.549 0.022 Cont. 132 High High Short Yes 4.450 2

17 1 17E53-15 2 0.530 0.021 Cont. 132 High High Short Yes 7.008 2

17 1 17E53-16 2 0.572 0.023 Cont. 132 High High Short Yes 8.339 2

17 1 17E53-18 2 0.530 0.021 Cont. 132 High High Short Yes 16.786 3 17 1 17E53-19 2 0.549 0.022 Cont. 132 High High Short Yes 17.574 3 17 1 17E53-20 2 0.549 0,022 Cont. 132 High High Short Yes 19.219 3

18 1 18E35-18 2 0.514 0.020 Cont. 148 High Low Short No 0.009 2

18 1 18E33-4 2 0.552 0.022 Cont. 149 High Low Short No 0.010 2

18 1 18E35-15 2 0.518 0.020 Cont. 148 High Low Short No 0.011 2

18 1 18E35-19 2 0.552 0.022 Cont. 148 High Low Short No 0.012 2

18 1 18E35-17 2 0.521 0.021 Cont. 148 High Low Short No 0.014 2

18 1 18E33-5 2 0.514 0.020 Cont. 149 High Low Short No 0.015 2 18 1 18E33-3 2 0.470 0.019 Cont. 149 High Low Short No 0.015 2 18 1 18E37-30 2 0.512 0.020 Cont. 144 High Low Short No 0.030 2

19 1 19E45-1 2 0.470 0.019 Cont. 139 Low High Short No 0.035 2 19 1 19E45-3 2 0.527 0.021 Cont. 139 Low High Short No 0.036 2 19 1 19E49-30 2 0.486 0.019 Cont. 131 Low High Short No 0.039 2

19 1 19E48-22 2 0.425 0.017 Cont. 135 Low High Short No 0.048 2 19 1 19E48-23 2 0.511 0.020 Cont. 135 Low High Short No 0.054 2

19 1 19E48-28 2 0.492 0.019 Cont. 135 Low High Short No 0.064 2

19 1 19E48-27 2 0.521 0.021 Cont. 135 Low High Short No 0.075 2

19 1 19E49-34 2 0.429 0.017 Cont. 131 Low High Short No 0.076 2

20 1 20E32-38 2 0.508 0.020 Cont. 135 Low Low Short Yes 1.541 2 20 1 20E32-39 2 0.537 0.021 Cont. 135 Low Low Short Yes 2.744 2 20 1 20E28-11 2 0.530 0.021 Cont. 140 Low Low Short Yes 2.841 2 20 1 20E30-28 2 0.533 0.021 Cont. 139 Low Low Short Yes 3.602 2 20 1 20E32-40 2 0.518 0.020 Cont. 135 Low Low Short Yes 3.971 2 20 1 20E28-8 2 0.495 0.020 Cont. 140 Low Low Short Yes 4.463 2 20 1 20E32-36 2 0.483 0.019 Cont. 135 Low Low Short Yes 4.704 2 20 1 20E28-13 2 0.479 0.019 Cont. 140 Low Low Short Yes 4.864 2

21 1 21E5-21 2 0.556 0.022 Clean 40 High High Short No 2.314 2

21 1 21E3-2 2 0.572 0.023 Clean 40 High High Short No 2.848 2

21 1 21E5-20 2 0.530 0.021 Clean 40 High High Short No 2.899 2

21 1 21E3-6 2 0.575 0.023 Clean 40 High High Short No 3.047 2

21 1 21E5-18 2 0.556 0.022 Clean 40 High High Short No 3.179 2

21 1 21E4-9 2 0.552 0.022 Clean 40 Higli High Short No 3.517 2

21 1 21E5-19 2 0.572 0.023 Clean 40 High High Short No 3.694 2

21 1 21E5-16 2 0.543 0.021 Clean 40 High High Short No 4.783 2

B9 — Tape System 2
Set No.

Set Rep

specimen

No. TS

No.

Tape Thickness Surface Aoolication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

22 22E23-15 2 u.4yo 0.020 Clean 40 High Low Short Yes 5.808 2 22 ] 22E22-13 2 U.j24 0.021 Clean 40 High Low Short Yes 19.168 3 22 22E22-12 2 0.505 0.020 Clean 40 High Low Short Yes 21.317 3 22 1 22E22-11 2 0.521 0.021 Clean 40 High Low Short Yes 22.088 3 22 22E24-23 2 u. jUo A AOA U.UzU Clean 4U High Low Short Yes 23.525 1 22 22E22-10 2 n ^0

U.UZ 1 L-iean /I A4U i-iign Low Short Yes 27.515 1 22 1 22E23-21 2 U.UZU x^iean /I A4U hugn Low Short Yes 29.182 1 22 1 22E24-26 2 40H-V nign Low Short Yes 37.343 3

23 1 23E10-11 2 0 546 0 0?7 40 l_-OW nign Niffln Short Yes 7.941 2 23 1 23E10-10 2 Clean 40 Low nign Short Yes 8.239 2 23 1 23E11-20 2 0.562 0.022 Clean 40 Low High Short Yes 15.200 1 23 1 23E11-17 2 0.508 0.020 Clean 40 Low High Short Yes 22.729 1 23

I

23E9-3 2 U. JZ / U.UZ 1 Clean 4U/I A Low High Short Yes 25.156 1 23 23E9-6 2 U.-)Z4 n m 1 U.UZ 1 L-iean /I A4U Low High Short Yes 25.462 1 23 23E11-16 2 u. j4y A AOO U.VzZ Clean /t A4U Low High Short Yes 28.034 1 23 1 23E9-1 2 U.J 14 A ATA U.UzU Clean /I A4U Low High Short Yes 33,800 1

24 24E 18-25 2 (J. J 33 A AO 1 U.UZ 1 Clean /I A4U Low Low Short No 0.435 2 24 24E19-35 2 U.4t)j A A 1 C L-lean /I A4U Low Low Short No 0.457 2 24 1 24E19-33 2 0.488 0.019 Clean 40 Low Low Short No 0.477 2 24 1 24E18-28 2 0.515 0.020 Clean 40 Low Low Short No 0,571 2 24

J

24E 18-24 2 U.J 1 J U.UZU L-iean /I A4U Low Low Short No 0.653 2 24 24E16-8 2 u.4yu U.U 1 y

(""loon Clean /I A4U Low Low Short No 0.658 2 24 1 24E 18-22 2 U. J jU u.uzz dean /I A4U Low Low Short No 0.738 2 24 1 24E 19-29 2 U.J 1 J U.UZU L-iean 4U Low Low Short No 0,785 2

25 1 25H53-25 2 u.y / J U.Ujo com. 1 A Q 1 Hy Hign High Short Yes 3,043 2 25 ] 25H50-5 2

C\ QAQ u.y4y AU.UjAn/ com. 148 High High Short Yes 3.153 2 25 25H50-3 2 0.927 0.037 Cont. 148 High High Short Yes 3.735 2 25 1 25H53-26 2 0.949 0.037 Cont. 149 High High Short Yes 3.808 2 25

[

25H53-28 2 O.yi 1 U.UJ / Cont. 1 ACi i4y High High Short Yes 4.780 2 25 25H50-1 2 U.yoj A ATQ U.Ujo com. ^ AQ 145 High High Short Yes 6.233 2 25 I 25H54-34 2 u.yj J A AIQ U.Ujo cont. 14j High High Short Yes 14.334 2 25 I 25H54-29 2 A QQ/1 u.yy4 A A1Q u.ujy com. 1 A <; 14j High High Short Yes 22.218 2

26 I 26H33-9 2 u.yz 1 U.Ujo com. 1 4U High Low Short No 6.475 2 26 26H35-28 2 n coo u.oyz A AT U.Uj J com. 1 A 0 1 4y High Low Short No 6.492 2 26 26H33-11 2 0.879 0.035 Cont. 140 High Low Short No 6.496 2 26 26H32-7 2 0.883 0.035 Cont. 144 T T* 1_ High Low Short No 6.504 2 26 ; 26H35-22 2 0.879 0.035 Cont. 149 High Low Short No 6.518 2 26 26H32-2 2 0.908 0.036 Cont. 144 High Low Short No 6.598 2 26 26H35-25 2 0.826 0.033 Cont. 149 High Low Short No 6.606 2 26 26H35-23 2 0.857 0.034 Cont. 149 High Low Short No 6.649 2

BIO — Tape System 2
Set No.

Set Rep

specimen

No. TSNo.

Taoe Thickness Surface Aoplication Time-al- mm in Cond GS Press Temp Temp Prmier hours FM

27 27H45-9 2 0.924 A A"? 0.036 Cont. 135 Low High Short No 0.222 2 27 27H49-41 2 U.914 A A*? ^ U.UJo Com. 1 33 Low T T' L High Short No 0.268 2 27 27H45-8 2 0.889 0.035 Cont. 135 Low High Short No 0.275 2 27 1 27H46-16 2 0.918 0.036 Cont. 136 Low High Short No 0.298 2 27 27H46-15 2 0.883 0.035 Cont. 136 Low T T" 1^ High Short No 0.308 2 27 ) 27H49-40 2

r\ on U.»/o A A"? C (J.U35 Cont. 133 Low High Short No 0.343 2 27 27H46-18 2 A AT C Cont. 1 JO Low High Short No 0.351 2 27 27H49-37 2 u.yz / A A17 cont. 1 J J Low High Short No 0.373 2

28 1 28H26-3 2 PAnt v--oni. 1 4D Low Low Short Yes 10.150 2 28 1 28H27-9 2 U.Uj / Pont 1 J / Low Low Short Yes 17.279 2 28 1 28H26-1 2 0.899 0.035 Cont. 146 Low Low Short Yes 17.569 2 28 1 28H26-5 2 0.962 0.038 Cont. 146 Low Low Short Yes 21.064 2 28 28H27-10 2 n Qi

U.UjO v^oni. 1 J / Low Low Short Yes 21.982 2 28 ] 28H29-23 2 u.yuz U.UjD Pr.Tif 1 A A 1 44 Low Low Short Yes 27.257 2 28 28H29-26 2 n Q/i Q U.Uj / Pr>Tit com. 1 44 Low Low Short Yes 28.363 3 28 1 28H29-24 2 U.S /U A AT/l P/^M+ com. 1 A A I 44 Low Low Short Yes 33.172 2

29 29H3-12 2 A A'2 O U.Ujo Clean A A4U High High Short No 2.200 2 29 } 29H4-18 2 0.92 / A AO '7 U.UJ / Clean /I A4U High Lhgh Short No 3.421 2 29 29H3-13 2 0.927 0.037 Clean 40 High High Short No 3.867 2 29 1 29H4-15 2 0.946 0.037 Clean 40 High High Short No 4.332 2 29 29H2-4 2

1 AAA A A'JO u.ujy Clean /I A4U High High Short No 9.445 3 29 J 29H2-1 2 A OCO A ATT U.Uj / Clean /I A4U High High Short No 23.672 3 29 29H2-2 2 u.y /o A ATQ u.ujy Clean /I A4U High High Short No 46.380 1 29 29H2-7 2 A QT7 A AT? U.Uj / Clean ACi 4U Hign Hign Short No 49.770 1

30 30m5-41 2

A Q/1 Q U.S4o AU.UjAnJ Clean /I A4U Hign Low Short Yes 36.392 2 30 30H21-11 2 A Q/K A AT? U.Uj / Clean A A4U High Low Short Yes 38.536 3 30 1 30H25-42 2 0.876 0.035 Clean 40 High Low Short Yes 44.695 3 30 1 30H25-38 2 0.883 0.035 Clean 40 High Low Short Yes 47.728 1 30 30H21-10 2 A oon 0.889 A Al C U.Ujj Clean A A40 High Low Short Yes 51.359 3 30 J 30H20-5 2 Ami U.y 1

A A1 ^ U.Ujo Clean /I A4U High Low Short Yes 64.404 3 30 30H21-13 2 u.yz / A AT7 U.Uj / Clean ACl 4U High Low Short Yes 72.140 3 30 I 30H20-3 2 0. 1 i 1 A A'^ A u.uiy Clean A A4U High Low Short Yes 77.768 1

31 I 31H8-6 2 u.yoz A AIQ U.Ujo Clean /I A4U Low Hign Short Yes 22.348 1 31 I 31H9-12 2

1 AIT J .U 1 J A A/IA U.U4U Clean /I A4U Low Hign Short Yes 23.656 1 31 31H8-4 2 0.943 0.037 Clean 40 Low High Short Yes 24.527 1 31 31H10-20 2 A AO O U.UjS Clean A A4U Low High Short Yes 26.062 1 31 ; 31H9-10 2 0.994 0.039 Clean 40 Low High Short Yes 28.439 1 31 31H10-18 2 0.927 0.037 Clean 40 Low High Short Yes 32.514 1 31 31H10-15 2 0.879 0.035 Clean 40 Low High Short Yes 33.888 1 31 31H10-21 2 0.965 0.038 Clean 40 Low High Short Yes 34.092 1

B 1 1 — Tape System 2
Set

XT-,. No.

Set KepSpecimen

No. TS

No.

Tape Thickness Surface Aoolication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

32 1 32H18-31 2 1 01 S \J.\JH\J V.^lCan 40 Low Low Short No 2.460 2 32 1 32H18-35 2 1 00"? 0 O'^Q 40 Low Low Short No 2.462 2 32 1 32H18-32 2 0.960 0.038 Clean 40 Low Low Short No 2.542 2 32 32H18-33 2 0.997 0.039 Clean 40 Low Low Short No 2.659 2 32 32H18-30 2 0.977 0.038 Clean 40 Low Low Short No 3.622 2 32 32H19-39 2 0.957 0.038 Clean 40 Low Low Short No 5.132 2 32 1 32H19-38 2 0.970 0.038 Clean 40 Low Low Short No 6.765 2 32 1 32H19-36 2 0.973 0.038 Clean 40 T nw T nw Short No 6.837 2

49 1 49E2-32 2 0.521 0.021 Cont. 149 Hi eh Hi eh Long Yes 0.214 2 49 1 49E51-4 2 0.549 0 02? Cnnt 141 Hi ah Hi ah Long Yes 0.240 2 49 1 49E2-35 2 0.562 0.022 Cont. 149 High High Long Yes 0.246 2 49 49E51-1 2 0.524 0.021 Cont. 141 High High Long Yes 0.248 2

\

49nz-3 J I 0.533 0.021 Cont. 149 Hi eh Long Yes 0.327 2 49 49E51-6 2 0.556 0.022 Cont. 141 Hieh Hi eh Long Yes 0.348 2 49 1 49E51-7 2 0.514 0.020 Cnnt 141 Hiph Hi ah Long Yes 0.493 2 49 1 49E52-13 2 0 530 0 09 1 Cnnt rugii Hirugnah Long Yes 0.854 2

50 1 50E36-26 2 \j.Hyo 0 090 Pnnt T-Tioh tiign j_,OW Long No 0.007 2 50 1 50E36-25 2 0 090 v^UIlL. 1 AO^y Himgnah Low Long No 0.007 2 50 1 50E34-9 2 0.495 0.020 Cont. 143 High Low Long No 0.007 2 50 1 50E34-10 2 0.508 0.020 Cont. 143 High Low Long No 0.007 2 50

I

50E38-39 2 n S14 0 090 Tnnt 1 Af\ Hinigii ah T r\\i7 Long No 0.010 2 50 50E38-42 2 D '^DQ 0 090 Pnnt 1 46 Hi ah T r^AX^ Long No 0.010 2 50 1 50E38-38 2 VJ. J 1 H 0 090 Pnnt 1 4fi Hi ah T r^AX/ J_^U W Long No 0.015 2 50 1 50E38-36 2 0 09 1 Pnnt 1 4fS Hi ah T-L/*J W Long No 0.015 2

51 1 51E46-11 2 0 435 0 017 Pnnt 1 36 T nw Hi ah Long No 0.011 2

51 1 51E47-17 2 0 410 0 01^^ Pont 141 T r\iA^ w Hirugii ah Long No 0.017 2

51 1 51E47-19 2 0.467 0.018 Cont. 141 Low High Long No 0.017 2

51 51E50-41 2 0.422 0.017 Cont. 132 Low High Long No 0.021 2

51

\

51E47-15 2 U. J ^ 1 0 01 s 141 Low Hirugnah Long No 0.023 2

51 51E46-9 2 0VJ.HVJ AfCI/ 0 018 Pnnt 1 JO Low Hinignah Long No 0.024 2

51 1 51E50-37 2 0 017 Pnnt 1 "^9 JZ Low Hi1:11 gnah Long No 0.024 2 51 1 51E47-16 2 u.^o / 0 018 1 4

Low Hi oh Long No 0.025 2

52 1 52E29-19 2 0 091 Pnnt 14"^ T r\\\i

1 A ' V\ T r\\x7 Long Yes 0.995 2 52 1 52E31-30 2 n SIS 0 090 Pnnt 1 "IQ Low T r\\x/

J , uvv Long Yes 1.362 2 52 1 52E29-17 2 0.533 0.021 Cont. 143 Low Low Long Yes 1.372 2 52

[

52E29-20 2 U. jUj u.uzu L-oni. 1 A 1 Low Low Long Yes 1.932 2 52 52E27-2 2 0.568 0.022 Cont. 134 Low Low Long Yes 1.936 2 52 52E31-33 2 0.486 0.019 Cont. 139 Low Low Long Yes 2.327 2 52 52E31-35 2 0.559 0.022 Cont. 139 Low Low Long Yes 3.192 2 52 52E27-7 2 0.549 0.022 Cont. 134 Low Low Long Yes 5.577 2

B 12 — Tape System 2
Set No.

Set Rep

Specimen

No. TSNo. Taoe Thickness Surface Anolication Time-atTemp Primer

TT1> mm in Cond GS Press Temp hours I-M

53 53E41-19 2 0.410 0.016 Clean 40 High High No 7.670 9 53 53E39-6 2 0.441 0.017 Clean 40 High High No 77.999 2 53 53E39-7 2 0.403 0.016 Clean 40 High High T one No 29.888 2 53 1 53E41-20 2 0.495 0.020 Clean 40 High High Long No 5.678 2 53

[

53E39-4 2 0.473 0.019 Clean 40 High High Long No 92.899 2 53 53E40-14 2 0.445 0.018 Clean 40 High High Long No 1 1 .218 2 53 53E40-1

2 0.460 0.018 Clean 40 High High T onp No 31.991 2 53 53E40-12 2 0.489 0.019 Clean 40 High High Lone No 30.61

2

54 54E26-40 2 0.521 0.021 Clean 40 High Low Lone Yes 5.550 2 54 54E25-35 2 0.543 0.021 Clean 40 High Low Lone Yes 17.628 3 54 54E21-1 2 0.527 0.021 Clean 40 High Low T one Yes 25.262 3 54 1 54E21-5 2 0.543 0.021 Clean 40 High Low Long Yes 27.161 3 54

j

54E26-42 2 0.505 0.020 Clean 40 High Low Long Yes 27.569 3 54 54E21-6 2 0.552 0.022 Clean 40 High Low Yes 32.389 3 54 54E21-3 2 0.552 0.022 Clean 40 High Low T onp Yes 35.455 1 54 54E21-2 2 0.489 0.019 Clean 40 High Low T OTIC? Yes 39.701 1

55 55F44.16 2 0.505 0.020 Clean 40 Low High Yes 526.20 1 55 55E43-8 2 0.455 0.018 Clean 40 Low High Yes 537.15 1 55 55E44-17 2 0.445 0.018 Clean 40 Low High Yes 539.48 1 55 1 55E43-11 2 0.467 0.018 Clean 40 Low High Long Yes 587.00 1 55

J

55E42-5 2 0.422 0.017 Clean 40 Low High Long Yes 687.38 1 55 55E44-20 2 0.473 0.019 Clean 40 Low High Yes 690.46 1 55 55E42-2 2 0.419 0.017 Clean 40 Low High T one Yes 940.1 1 55 55F44-19 2 0.495 0.020 Clean 40 Low High T one? Yes 1057.6 1

56 56E20-37 2 0.518 0.020 Clean 40 Low Low No 0.376 2 56 56F20-39 2 0.528 0.021 Clean 40 Low Low No 0.428 2 56 56E17-16 2 0.508 0.020 Clean 40 Low Low No 0 447 2 56 1 56E20-38 2 0.513 0.020 Clean 40 Low Low Long No 0.496 2 56 56E20-36 2 0.495 0.019 Clean 40 Low Low Long No 0.571 2 56 56E15-7 2 0,513 0.020 Clean 40 Low Low Long No 0.595 2 56 56E15-4 2 0.530 0.021 Clean 40 Low Low Lons No 0.626 2 56 56E15-2 2 0.528 0.021 Clean 40 Low Low Lone No 0.722 2

57 57H52-18 2 0.937 0.037 Cont. 149 High High T ont? Yes 0.465 2 57 0.930 0.037 Cont. 140 High High Yes 1 .421 2 57 57H51-1

2 0.965 0.038 Cont. 140 High High Yes 1.426 2 57

;

57H52-19 2 0.908 0.036 Cont. 149 High High Long Yes 1.856 2

J / 0.937 0.037 Cont. 150 High High Long 1 Co 9 57 57H51-12 2 0.984 0.039 Cont. 140 High High Long Yes 7.450 2 57 57H52-15 2 0.886 0.035 Cont. 149 High High Long Yes 10.152 2 57 57H51-8 2 0.924 0.036 Cont. 140 High High Long Yes 11.887 2

B13 — Tape System 2
Set No.

Set RepSpecimen

No. TSNo. Tape Thickness Surface Aoolication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

58 58H34-18 2 0.978 0.039 Cont. 145 High Low T on£? No 6.392 2 58 58H36-31 2 0.933 0.037 Cont. 143 High Low T onff No 6.395 2 58 58H34-17 2 0.978 0.039 Cont. 145 High Low No 6.396 2 58 1 58H37-39 2 0.860 0.034 Cont. 143 High Low Long No 6.401 2 58 58H37-40 2 A c\r\o u.yOo O.UJo Cont. 1 A 'y 143 High Low Long No 6.418 2 58 58H37-38 2

O 1 o

u.y 1 o Lont. 1 /I o 143 High Low Long No 6.425 2 58 58H37-36 2 U.Ujo L-oni. 1/11 143 High Low Long No 6.427 2 58 58H36-29 2 V.yjV U.U J / L-oni. 143 High Low Long No 6.441 2

59 59H44-4 2 U.o4o A ATI Lont. 14U Low High Long No 0.056 2 59 59H47-22 2 0. /ol A AT 1 0.03

Cont. 1 '3

13 / Low High Long No 0.062 2 59 59H44-3 2 0.870 0.034 Cont. 140 Low High Long No 0.070 2 59 1 59H47-23 2 0.889 0.035 Cont. 137 Low High Long No 0.071 2 59 59H44-2 2 0.873 A A'? A 0.034 Cont. 140 Low High Long No 0.078 2 59 59H47-27 2 0.845 A A^ 0.033 Cont. 137 Low T T* —I. High Long No 0.100 2 59 59H48-34 2 0.838 A AO -y 0.033 Cont. 139 Low XT' 1 High Long No 0.106 2 59 59H48-35 2 0.819 A AT 0.032 Cont. 139 Low T T* ^T. High Long No 0.1 12 2

60 60H30-32

r\ no A A A'?n Lont. 13 / Low Low Long Yes 4,611 2 60 60H28-20 2 0.892 A A'5 C 0.035 Cont. TOO 133 Low Low Long Yes 4.796 2 60 60H28-16 2 0.930 0.037 Cont. 133 Low Low Lone Yes 1 1.184 2 60 1 60H31-36 2 0.870 0.034 Cont. 137 Low Low Long Yes 11.964 2 60

[

60H31-40 2 O.yjo A A'3 O O.UJo Cont. 13 / Low Low Long Yes 17.617 2 60 60H31-37 2 A one A A'5 C O.OJj Cont. 13 / Low Low Long Yes 20.612 3 60 60H30-34 2

r\ nn c 0.975 A A'? O 0.038 Cont.

1 O T 137 Low Low Long Yes 21.297 2 60 60H31-38 2 0.946 0.037 Cont. 137 Low Low Long Yes 21.855 3

61 61H40-19 2 A TAT 0.797 A AO 1 0.031 Clean A A40 High High Long No 36.351 3 61 , 61H39-1

2 A O 1 A 0.819 A AO O 0.032 Clean yt A40 High High Lone No 36.447 3 61 61H39-12 2 0.870 0.034 Clean 40 High High Long No 44.751 1 61 1 61H40-20 2 0.819 0.032 Clean 40 High High Long No 43.312 1 61

[

61H40-21 2 0.832 A AO O 0.033 Clean A A40 High High Long No 20.969 1 61 61H38-6 2 A O"? O 0.832 A AT T 0.0J3 Clean A A40 High tt: „i. High Long No 43.343 1 61 61H38-4 2 A OZ" -4 0.864 A AO A 0.034 Clean A A40 High High Long No 31.027 1 61 61H39-13 2 0.876 A A O C 0.035 Clean >1 A40 T T" TMl. High High Lone No 35.945 1

62 62H22-20 2 0.895 0.035 Clean A A40 T T' 1_ High Low Long Yes 20.571 2 62 62H22-19 2 A o T^ 0.822 A AO 0.032 Clean ,1 A40 High Low Long Yes 24.905 2 62 62H22-18 2 0.870 0.034 Clean 40 High Low Long Yes 31.276 3 62

]

62H24-32 0.902 0.036 Clean 40 High Low Long Yes 33.420 1 62 0.866 0.034 Clean 40 High Low Yes 35.454 1 62 62H22-21 2 0.933 0.037 Clean 40 High Low Long Yes 41.260 3 62 62H24-29 2 0.902 0.036 Clean 40 High Low Long Yes 54.360 3 62 62H23-22 2 0.914 0.036 Clean 40 High Low Long Yes 58.811 3

B14 — Tape System 2
Set No.

Set Rep

Specimen

No. TS

No.

Tape Thickness Surface Aoplication Time-atTemp Primer

TTF

mm in Cond GS Press Temp hours FM

o3 OJH4z-y z 0.841 0.033 Clean 40 Low High Long Yes Z.d4» I 63 0JH4Z-0 z 0.832 0.033 Clean 40 Low High Long Yes A AAA 4.444 z 63 DiH4/-lz z 0.838 0.033 Clean 40 Low Hi eh Long Yes J. 193 1 63 ! 63H42-7 2 0.832 0.033 Clean 40 Low High Long Yes 8.887 2 63 63H41-11 2 0.800 0.032 Clean 40 Low High Long Yes 53.690 1 6J DJri4 1 -J Z 0.835 0.033 Clean 40 Low High Long Yes A 1 OAT 1

1 6J ojH4 I -o Z 0.873 0.034 Clean 40 Low High Long Yes OJ.OOJ 1 OJ ojri4 1 - lU z 0.810 0.032 Clean 40 Low High Long I es DO. /U /

11

04 D4rl 1 0- 1 o

-1z 0.880 0.035 Clean 40 Low Low Long INO U.ojZ z9 04 04rll /-Zz z 0.915 0.036 Clean 40 Low Low Long INO z

04rl 1 o- 1 y z 0.920 0.036 Clean 40 Low Low Long INO Z 64 1 64H16-17 2 0.910 0.036 Clean 40 Low Low Long No 1.151 2 64 64H17-26 2 0.940 0.037 Clean 40 Low Low Long No 1 .242 2 64 64H17-27 2 0.943 0.037 Clean 40 Low Low Long No 1.375 2 64 64H14-3 2 0.920 0.036 Clean 40 Low Low Long No 1.615 2 64 64H14-6 2 0.945 0.037 Clean 40 Low Low Long No 2.326 2

B15 — Tape System 2

APPENDIX C. EXPERIMENT TO INVESTIGATE TSl VARIABILITY

As indicated in the main text (Section 4.4), variability in creep-rupture results was found among

Tape System 1 (TSl) sample sets prepared in Phases I and II of this industry-government

consortium study. To investigate the cause(s) of this variability, a full factorial (3 by 2) experiment

using three TSl tapes and two TSl primers was designed. The materials are listed in Table CI. Six

sample sets were prepared (i.e., TlPl, T1P2, T2P1, T2P2, T3P1, and T3P2). Note that these sets include replicate sets of the specimens that were used in Phase I (i.e., TlPl) and Phase II (i.e., T2P1) of the study. Tape 3 and primer 2 were obtained specifically for use in the investigations of

the TSl variability. In all cases, the primer was well stirred before application. Creep-rupture and

peel-strength measurements were conducted after the specimens were a minimum of 28 days old. The creep load was 9.3 N (2.1 Ibf).

Table CI. Description of TSl tapes and primers used in the investigation of TSl variability

Tape

Number Design." Description

Primer

Number Design." Description

Tape 1

Tape 2

Tape 3

Tl

T2

T3

First tape in the study:

• its age was about 22 months.

• it was the Phase I tape.

Second tape in the study:

• its age was about 6 months.

• it was the Phase II tape.

Third tape in the study:

• its age was about 1 month.

• it was obtained to be used in investigations of the TS

variability.

Primer 1

Primer 2

PI

P2

First primer in the study:

• its age was about 22 months.

• it was the Phase I and Phase II primer.

Second primer in the study:

• its age was about 2 months.

• it was obtained to be used in th Phase II investigations of the TSl variability.

"Design, indicates designation.

The results of the creep-rupture and peel-strength tests are summarized in Figures CI and C2,

respectively. The error bars represent one standard deviation; the letters above the error bars

represent the failure mode (A = adhesive; C = cohesive; M = mixed). Note that Figure CI has seven

bars, because the T2P1 data set is divided into two subsets—one for specimens that failed

adhesively (T2P1-A) and the other for those that failed in a mixed mode (T2P1-M).

CI. CREEP-RUPTURE RESULTS

Examination of Figure CI provides evidence that the TSl tape, and not the TSl primer, was

primarily responsible for the variability between the TSl Phase I and Phase II data sets discussed in

Section 4.4. Observe in Figure CI that the times-to-failure vary among the three tapes. In

particular, the T3P1 and T3P2 sample sets had mean times-to-failure that were slightly less than 300

hours, which was about a factor of six greater than the mean time-to-failure (about 50 hours) of the

CI
400

(03

O

uT

oc

300

200

100

<

lU

M

A

T1P1 T1P2 T2P1-M T2P1-A T2P2 T3P1 T3P2

Sample Set Number

Figure CI. Mean times-to-failure of the sample sets prepared to examine TSl tape variability.

(Tl, T2, and T3 indicate the three tapes, and PI and P2 indicate the two primers; the

failure modes are: C = cohesive, A = adhesive, and M = mixed cohesive/adhesive. In the case of T2P 1

, some specimens failed adhesively and some in a mixed mode; a

distinction between the two groups is shown by the -M and -A after the T2P1 sample

set number.)

2.5

: 2.0 -

(32 1.5

cc

I-

-I 1.0 h

ui

UJ

a.2 0.5

<

111

- 14

12 £

iio 5

z

UJ

»-

0)

- 8

- 2

T1P1 T1P2 T2P1 T2P2 T3P1

Sample Set Number

T3P2

UJ

UJ

a.<

UJ

Figure C2. Mean peel strength of the sample sets prepared to examine TSl tape variability.

(Tl, T2, and T3 indicate the three tapes, and PI and P2 indicate the two primers; the

failure modes are: C = cohesive and M = mixed cohesive/adhesive).

C2
TlPl and T1P2 sample sets. Moreover, the T2 specimens that failed adhesively (T2P1-A and

T2P2) had similar mean times-to-failure of about 12 hours to 14 hours; the difference was not

statistically significant. On the other hand, note also in Figure CI that, for the three pairs of sample

sets made with the two primers, the mean times-to-failure were not statistically different within the

pair (when the failure modes were the same). That is, no substantial effect due to primer was

observed.

The mean times-to-failure (about 50 hours) of the TlPl and T1P2 sample sets were not statistically

significantly different fi^om that obtained for the TS 1 sample set (about 44 hours) in Phase I (Table 7). As just noted, the creep-rupture tests of the TlPl specimen set was a repeat of the Phase

I test at 9.3 N (2.1 Ibf) using Tape System 1. This finding suggested that the TSl Phase I data were

reproducible, even using tape and primer that were almost 2 years old. Additionally, the finding

implied that the laboratory application technique had not been unknowingly altered—at least to the

point that the TSl Phase I results could not be reproduced.

C2. PEEL-STRENGTH RESULTS

It is evident in Figure C2 that little difference was observed between the mean peel-strengths of the

six sample sets. For the Tl, T2, and T3 sets (ignoring the primer), the mean peel strengths were

1.82 kN/m, 1.79 kN/m, and 1.93 kN/m (10.4 Ibfin, 10.2 IbCin, and 11.0 Ibfin), respectively. These

values were about the same as that found in the Phase I tests (Table 7). However, although the

mean strengths were similar for specimens made with the three tapes and two primers, the failure

modes were not the same in all six cases. The T1P1/T1P2 and T3P1/T3P2 specimens failed

cohesively; whereas the T2P1/T2P2 specimens failed in a mixed mode. This again implied a

difference in behavior due to tape and not primer.

C3. TAPE VARIABILITY

A fill! investigation of the reason(s) why the tape was primarily responsible for the variability

between the TSl Phase I and Phase II data sets was beyond the scope of the project. However,

load-elongation tests on the three tape (Tl, T2, and T3) were conducted, and mean values of tensile

modulus at 300 % elongation (longitudinal direction) are given in Figure C3. The error bars in the

plot represent one standard deviation of the mean. The mean values (six measurements) are 19 kPa,

32 kPa, and 30 kPa (2.8 Ibf/in^ 4.6 Ibfin^ and 4.4 Ibfin^), respectively. Although the differences were statistically significant, no practical significance was attached to these small differences. The

limited data suggest that differences in mechanical properties of the three tapes were not responsible

for the variability in creep-rupture and peel-strength between the sample sets made with the three

tapes.

C4. COMPARISON OF THE TSl PHASE II SPECIMENS WITH LIQUID-ADHESIVEBONDED-SPECIMENS

As indicated in the introduction, a main objective of the joint research program is to compare the

creep-rupture performance of tape-bonded and liquid-adhesive-bonded EPDM seams. Consistent

with this objective, a comparison may be made between the creep-rupture results of Phase I liquidadhesive-bonded (LA) specimens with the Phase II TSl specimens prepared when investigating the

C3
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Figure C3. Tape modulus (longitudinal direction) at 300 % elongation. (Tl, T2, and T3 indicate the

three tapes.)

TSl variability. The point of comparison is made for sample sets having the shortest mean times-tofailure under the 9.3 N (2. 1 Ibf) load.

In this regard, in Phase I, the mean times-to-failure for the three sets of liquid-adhesive-bonded

specimens (LA Replicate Set Nos. 3-5) with the shortest times-to-failure were 7.0 hours, 6.8 hours,

and 8.8 hours (fig. 1) [3]. In Phase II, sample sets T2P1-A and T2P2 had the shortest times-tofailure of those prepared for the TSl variability investigations (fig. CI). The values were about 12

hours and 14 hours, respectively. Although the five sample sets in question had times-to-failure

similar to each other, the Phase 11 TSl sets were statistically longer lived than the Phase I LA

sample sets.

C4 tirU.S. GOVERNMENT PRINTING OFFICE: I997 - 417-392/72666


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