Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 59 Performance Evaluation of Unexposed and Field-exposed Thermoplastic Polyolefin (TPO) Roof Membranes Roof Consultants Institute Jim Carlson1, Ana H. Delgado2, Ernie Rosenow1, K.C. Barnhardt1, and Ralph M. Paroli2 1Western States Roofing Contractors Association 2National Research Council of Canada, Institute for Research in Construction ABSTRACT Four test roofs were installed across the Western U.S. by the WSRCA in 2001 as part of its TPO Weathering Farm Project. An overview of the findings gleaned from the field, as the membranes now progress into their fifth year of weathering, will be presented. This will include field observations and field solar reflectivity testing data. In addition, laboratory results such as: breaking strength, elongation, thickness, glass transition temperature, thermogravimetry, and spectroscopy will be presented. Overall, this presentation is intended to provide roof consultants, roofing contractors, manufacturers, roof designers, and specifiers with updated technical information regarding TPO roof membranes. Attendees are expected to depart with an understanding of the WSRCA TPO Weathering Farm Project, TPO roof membranes in general, the problems with some of the earlier formulations, the successes regarding reflectivity, and other current pertinent information. SPEAKERS JIM CARLSON, technical director/principal consultant and founder of Building Envelope Technology & Research in Seattle, Washington, has been a member of RCI since 1988. Jim previously worked with the NRCA as its deputy director of technology and research. While with NRCA, Jim conducted the re-write of the NRCA Roofing & Waterproofing Manual, of which he authored several sections and co-authored others. Jim also co-authored the Repair Manual for Low-Slope Membrane Roofing Systems, conducted numerous roofing research projects, including joint projects with SPRI, ARMA, MRCA, and WSRCA, and authored many technical papers to benefit the roofing and waterproofing industry. Jim began his career in the roofing industry in the early 1970s working as an apprentice for a roofing contractor. Prior to his time with NRCA, Jim served as senior field engineer/roofing consultant for Wetherholt & Associates, a consulting engineering firm that specializes in roofing and waterproofing projects. Jim also serves as an officer with ASTM, technical advisor for WSRCA, co-advisor for the Midwest Roofing Contractors Association, and is an accomplished author and speaker for the industry. RALPH M. PAROLI is the director of the Building Envelope and Performance Program at the Institute for Research in Construction (IRC), National Research Council of Canada. Prior to this, he led the Roofing Materials and Systems Performance activity at IRC. He has been involved with spectroscopy and thermal analysis for nearly 20 years. As a researcher, Paroli has participated in and led government research projects in the characterization of roof system performance. Paroli is a chartered chemist with the Chemical Profession of Ontario. He is a member of the American Chemical Society, the Chemical Society of Canada, the International Union of Pure and Applied Chemistry, the Canadian Society for Analytical Sciences and Spectroscopy, the Society for Applied Spectroscopy (USA), ASTM, and RCI. In addition, he is a past president of the Spectroscopy Society of Canada and of the Canadian Thermal Analysis Society. He is a member of the Canadian Roofing Contractors Association’s National Technical Committee and the vice-Chair of ASTM D- 08. Paroli received his B.S. degree in analytical chemistry from the University of Concordia and his Ph.D. in physical/inorganic chemistry from the University of McGill, Montreal, Canada. Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 60 Proceeedings of the RCI 21st International Convention SUMMARY Western States Roofing Contractors Association’s (WSRCA) TPO Weathering Farm Project was initiated to “Examine weathering characteristics of thermoplastic polyolefin (TPO) roof membranes by exposing them to various weather conditions of four distinctly different climatic regions in the Western United States.” The project’s goal is: “To provide pertinent technical and performance information to the Western States Roofing Contractors Association membership, and the North American roofing industry at large, regarding TPO roof membranes’ attributes, their performance properties, and resistance to degradation due to the effects of weathering.” Although it is a western states focus, the results will be applicable to other regions in North America. Four different roofing manufacturers supplied the TPO roofing membranes (blind-labeled as Nos. 1 through 4). Sixteen out of the 32 membranes were unexposed and were used as a control. The other 16 (one from each manufacturer) have been exposed to weather on full-scale test roofs in Anchorage, Alaska; Las Vegas, Nevada; Seattle, Washington; and San Antonio, Texas. The thickness (sheet overall and coating over scrim), dimensional stability, water absorption, tensile test, elongation, glass transition temperature (Tg) and thermal stability (weight loss) of the TPO roof membranes were evaluated by mechanical testing, dynamic mechanical analysis (DMA), and thermogravimetry (TG). Results of the analyses showed that the mechanical and chemical properties investigated did not undergo significant changes after threeyear exposure. The five-year data is still being collected and analyzed, to be reported in the near future. BACKGROUND Forty-nine polyester/fiberreinforced TPO roof membrane samples were received from the WSRCA. They were obtained from exposure sites in four regions in the U.S., labeled as Alaska (AK), Las Vegas (LV), Seattle (SEA), and Texas (TX). Sixteen of the 32 samples were new and the rest had been exposed for up to three years. The suffix “u” was used for unexposed or new samples, whereas the suffix “e” was used for the exposed samples. One sample per manufacturer and exposure location was from a seam test cut. The top ply (weathered surface) was white for all samples. Note that the roll direction (machine and cross directions) was not specified on the samples when received. Therefore, using an optical microscope, the directions were identified in the laboratory by the shapes of the fiber bundles on the crosssection of the samples. The test site locations were chosen because they represent the four more diverse climatic regions of western North America (see Map 1). The locales and climates are: Las Vegas, Nevada, generally hot and dry; San Antonio, Texas, generally hot and humid; Anchorage, Alaska, generally cold and damp; Seattle, Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 61 Performance Evaluation of Unexposed and Field-exposed Thermoplastic Polyolefin (TPO) Roof Membranes Map 1 – Test site locations were chosen to represent four diverse climatic regions of western North America. Washington, moderate with wet and dry periods. The on-roof weathering and testing is unbiased, with all TPO membranes blind-labeled and laid out similarly in each of the four test roofs (see Map 2). FIELD OBSERVATIONS This TPO roofing research project has now entered into its fifth year of weathering, originally beginning the test roof installations with the more moderate of the four different climatic locations, in Seattle, Washington. Based on the visual field inspections (Photos 1A-D), all of the roofs appear to be performing well, despite the rather harsh exposure extremes. For example, the Anchorage, Alaska roof has experienced low temperatures in excess of -30°F (-34°C), and weeks of being covered with snow and ice, to highs in the +80°F (27°C), with sun; but not as much sun load as the Las Vegas, Nevada site that normally has 210 very sunny days per year and experiences rooftop temperatures in excess of +130°F (54°C). All seams remain welded, and all roofs are leak free, despite the maintenance traffic to which they are subjected, including one on a cabinet shop in Las Vegas and one on a hospital in Anchorage. The Las Vegas roof has swamp coolers mounted on curbs, which regularly need their filters changed due to the heavy dust from the saws and sanders inside the building and the volatile stain and paint fallout from the finishing shop area inside that exhausts various petroleum distillate fumes from power exhaust vents mounted on the roof. From the exposure to sun (e.g., ultraviolet radiation) and heat loads, combined with their thermal expansion and contraction differentials; to the ice, snow and rain, including wet-dry cycling, the maintenance traffic, and the air-borne dust and fallout – these 60-mil, white, TPO membranes are so far showing good inservice performance. Seam Integrity In general, all of the TPO membranes examined in the field to date have maintained their seam quality. All hot-air welded seams, which are randomly probed during the yearly inspections, are proving to have great weld integrity. Initially, a few seams on a couple of the roofs were thought to have opened slightly (approximately 1/16 to 1/4-inch) between the time the roofs were initially installed and the first years’ follow-up inspection. Transitions adjacent to a drain in Las Vegas were suspect last year. However, once the seams were inspected and touched-up (i.e., reheated and welded closed along the outer seam edge), the welds stayed closed. Therefore, it is now thought that these few initial seam edges were not originally welded as thoroughly (i.e., cold welds) as needed. Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 62 Proceeedings of the RCI 21st International Convention Map 2 – Roof layout. Seattle Alaska Photo 1 – Test roofs in order of installation: Seattle (A), Alaska (B), Las Vegas (C), and Texas (D). Las Vegas Texas Membranes Initially Loose, But Have Since Tightened Judging from the yearly field inspections and data collection, there has been some tightening of the sheets, which is visible at a few locations as bridging at roof-towall intersections and some roof-to-area divider transitions. The tightening is not unique to TPOs. It has also been observed over the years with PVC and EPDM roof membranes, which can tighten as they age. The cause of tightening, however, is different. Initially, and up through the third year of weathering, some of the TPO membranes were somewhat loose or baggy with some very apparent wrinkling (this could be due to time of inspection – i.e., morning). The Texas roof, which was installed slightly differently than the others (by first welding neighboring sheets, then installing the mechanical fasteners), did not exhibit the looseness that the other three roofs presented during their first, second, and to some extent, the third years of service. This would indicate that installation techniques and workmanship can significantly affect the overall appearance of the membrane. However, as all of the roofs have aged through their third and fourth years, most have tightened and are now laying quite smooth. There are isolated areas of bridging that have been identified and marked, and they will be monitored as this research and testing project progresses (See Photos 2 and 3). Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 63 Photo 2 (left) – Seattle test roof before three years of installation. Photo 3 (right) – Seattle test roof after three years of installation. Table 1 – Reflectivity values for TPO membranes before and after cleaning. Surface Characteristics and Color or Hue Another unique quality that has been observed is the surface condition of the TPO roof membrane sheets. Some of the sheets are noticeably dirtier than others, apparently accumulating dust and airborne particulate differently than their neighboring sheets. Research will hopefully determine if static charge(s) are different, potentially due in part to different polyisocyanurate insulation facers. Or it may show, if membrane surface roughness increases over time (for example, developing a rougher surface characteristic such as PVC, which may change from almost slick to rough – e.g., with surface crazing), thus making the membrane more prone to holding dust and airborne particles and visibly accumulating dirt, as all other roof membranes do over their years of service. Solar Reflectivity Reflectivity measurements shown in Table 1 were obtained on the roofs during the third-year (fourth-year in Seattle) inspections. Solar reflectivity measurements1 were conducted on both weathered areas and areas that had been cleaned (Photos 4 – 5). A comparison of two common cleaning methods was tested. Areas were wetted, scrubbed with stiffbristle push brooms or brushes, then rinsed, along with a side-byside comparison of pressure rinsing/“ washing.” In nearly all cases, the scrubbed areas produced a visually cleaner and a slightly more reflective surface. However, even before cleaning, all of the TPO roofs far surpassed the ENERGY STAR® reflectivity requirements for three-year-old roof membranes. At all the areas, solar reflectivity improved after cleaning, though no membrane returned to its original whiteness. It should be noted that mild cleaning procedures were used for testing, and that no strong detergents or cleaning chemicals were used to clean the TPO surface. Fifty-eight percent of the reflectivity component occurs in the nonvisible region of the solar spectrum. EXPERIMENTAL METHOD Mechanical Properties Visual inspection showed that the weathered surface of the samples was in good condition with neither pinholes nor crazes. Some of the field samples were dusty, so a wet paper towel was used to wipe the surface before testing. The following physical and mechanical properties of all the samples were measured. Thickness, Sheet Overall The overall sheet thickness of the polyester-reinforced roofing membranes was measured using a digital micrometer (ASTM D751- 00 [1]). Five measurements were taken at randomly-selected points over the sample surface to obtain a representative average. Thickness of Coating Over Scrim The thickness of coating over scrim was measured by modifying the optical method described in Annex A1 of ASTM D6878-03 [2]. A rectangular specimen of approximate dimensions of 50 mm x 5 mm (2 in. x 0.2 in.) was cut from each sample. A clean cut through Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 64 Proceeedings of the RCI 21st International Convention Photo 4 – Membrane after cleaning. Photo 5 – Reflectivity measurements. 1The task group wishes to acknowledge Ross Roberts and Firestone for their extra contributions of expertise, testing equipment, and travel expenses. the sheet was made on the long dimension of the specimen by cutting along the center of a fiber bundle using a sharp utility knife. The crosssection was placed under an optical microscope equipped with a CCD camera. Micrographs at 50X magnification were digitally captured by the camera and stored on a computer. The thickness of the weather surface at each fiber intersection was measured on the digitized micrograph, using image-analysis software. Linear Dimensional Change The linear dimensional change of the samples was measured based on ASTM D1204-02 [3]. The specimens were conditioned at 70 ± 2°C (158 ± 3°F) for six hours as specified by ASTM D6878-03 [2]. Only one specimen of dimensions 250 mm x 250 mm (10 in. x 10 in.) was cut from each sample. Before conditioning, each specimen was marked and measured at three equally spaced points along each side in both the machine (MD) and cross (XD) directions, using a digital calliper. The specimens were dusted with talc and sandwiched between two pieces of silicone-coated paper that were secured together with paperclips. The assemblies were placed in a convection oven at 70 ± 2°C (158 ± 3°F) for six hours. They were then removed from the oven and reconditioned in the laboratory at 23 ± 2°C (73 ± 4°F) and 50 ± 5% relative humidity for at least one hour before final measurements were made. The linear dimensional change is the change in dimension expressed as a percent of the original dimension. A positive linear dimensional change indicates expansion while a negative value denotes shrinkage. Water Absorption The resistance to water absorption was measured according to ASTM D471-98 [4] on the weathered surface of the samples only. The samples were cut into disks of 60 mm (2.4 in.) in diameter and initial weights recorded. The specimen was placed in the apparatus, weather-side up. The chamber was then filled with deionised water to a depth of approximately 15 mm (0.6 in.), which was equivalent to about 30 mL (1.8 in.3) in volume, and tightly sealed by a stopper. The assembly was placed in an oven at 70 ± 2°C (158 ± 3°F) for 166 hours. At the end of the immersion period, the apparatus was allowed to cool to room temperature in the laboratory for two to three hours. The specimen was released from the apparatus and excess surface water was removed by blotting with a filter paper. The final weights of the specimens were immediately measured. Tensile Properties The tensile properties of the samples were measured according to ASTM D751-00 [1], Procedure B – Cut Strip Test Method, instead of the Procedure A – Grab Test Method as specified by ASTM D6878-03 [2] due to the limited materials available. The samples were cut into specimens of 25 mm x 150 mm (1 in. x 6 in.) using a pneumatic die cutter. The specimens were tested in a universal testing machine at a constant crosshead speed of 5 ± 0.2 mm/s (12 ± 0.5 in./min). The gauge length of the specimens was 75 mm (3 in.). A minimum of five specimens was tested in both machine (MD) and cross (XD) directions except for some samples that had limited material. Chemical Properties Dynamic mechanical analysis (DMA) Sample preparation After cleaning the samples with wet paper towel, a piece of approximately 40 x 20 mm (1.6 x 0.8 in.) was cut from each of the “as received” samples. One exposed sample from each manufacturer was from a seam cut; therefore, a specimen was cut from top and bottom sheets and labeled as ‘t’ and ‘b’ (Figure 1). Unexposed and exposed specimens were conditioned in an air-circulating oven for one hour at 80 ± 2°C (176 ± 36°F) (as per ASTM D 6382-99) [5] to provide a consistent thermal Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 65 Figure 1 – Picture of the top and bottom sheets from a seam cut of exposed samples. history before testing. They were removed from the oven, stored in a desiccator, and allowed to relax for at least eight hours before conducting the analysis. A Rheometric Scientific RSA3 (now TA Instruments) Solid Analyzer equipped with an environmental controller and a dual cantilever geometry was used to measure the glass transition temperature (Tg) of the unexposed and exposed samples. Rectangular strips were cut with a utility knife and placed in the dual cantilever fixture. The specimen was cooled to -80°C (-112°F), the temperature was allowed to stabilize for five minutes and increased at 2°C/min (4°F/min) to the final temperature program. All pre-conditioned (control) specimens were run at least in duplicate. The test was conducted as per ASTM D 5418-01 [6]. Experimental parameters are given below: Geometry: Dual cantilever Sweep type: Dynamic Temperature Ramp Dimensions: Length: Fixed at 36.67 mm (1.44 in.) Frequency: 1 Hz (6.28 rad/sec) Temperature program: -80°C to 50°C (-112 to 122°F) Ramp Rate: 2°C (4°F) Soak Time: 1 minute Time per Measure: 1 minute Strain: 0.01-0.02% Autotension Mode: Off Autostrain Mode: On Strain Adjustment: 25-30% of current strain Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 66 Proceeedings of the RCI 21st International Convention Exposure Thickness Overall** Exposure Thickness Overall** Sample Time ThicknessChanges Sample Time Thickness Changes ID* (yrs) (mm)+ (mm) ID* (yrs) (mm)+ (mm) AK1 0 1.4 – AK3 0 1.5 – 1 1.4 0.0 1 1.5 0.0 3 1.5 0.1 3 1.5 0.0 AK2 0 1.4 – AK4 0 1.4 – 1 1.5 0.1 1 1.4 0.0 3 1.5 0.1 3 1.5 0.1 LV1 0 1.5 – LV3 0 1.4 – 1 1.5 0.0 1 1.4 -0.0 3 1.6 0.1 3 1.4 0.0 LV2 0 1.4 – LV4 0 1.5 – 1 1.4 0.0 1 1.4 -0.1 3 1.5 0.1 ` 3 1.4 -0.1 SEA1 0 1.4 – SEA3 0 1.5 – 1 1.4 0.0 1 1.5 0.0 3 1.4 0.0 3 1.5 0.0 SEA2 0 1.4 – SEA4 0 1.4 – 1 1.4 0.0 1 1.5 0.1 3 1.4 0.0 3 1.5 0.1 TX1 0 1.4 – TX3 0 1.5 – 1 1.4 -0.0 1 1.4 -0.1 3 1.4 -0.0 3 1.4 -0.1 TX2 0 1.5 – TX4 0 1.4 – 1 1.5 -0.0 1 1.4 -0.0 3 1.5 0.0 3 1.4 -0.0 Table 2 – Average thickness, sheet overall of unexposed, 1- and 3-year exposed TPO roof membranes. *AK = Alaska; LV = Las Vegas; SEA = Seattle; TX = Texas (1-4) = Manufacturer # +1 inch = 25.4 mm ASTM D 6878-03 specification: 1.0 mm (0.039 in) RESULTS AND DISCUSSION Thickness, Sheet Overall The overall sheet thickness of the samples is summarized in Table 2 and Figure 2. Each entry is the average and standard deviation of five individual measurements. The overall sheet thickness of the samples ranged from 1.35 -1.55 mm (0.053 -0.061 in.), which significantly exceeded the minimum requirement of 1.0 mm (0.039 in.) as specified in ASTM D6878 for new TPO membranes. The overall sheet thickness changed less than ±0.10 mm (0.004 in.) after exposure. Thickness of Coating Over Scrim The thickness of the top coating over the fiber intersection of the samples is summarized in Table 3 and Figure 3. Each entry is the average and standard deviation of six individual measurements. The thickness over scrim value represents the minimum coating thickness on the weathered surface of the samples. The coating thickness for all samples exceeded the minimum requirement of 0.305 mm (0.012 in.) as specified in ASTM D6878 for new TPO membranes. It ranged from 0.470 – 0.650 mm (0.018 – 0.026 in.) and 0.390 – 0.590 mm (0.015 – 0.023 in.) for the unexposed and exposed samples, respectively. The coating thickness reduced by 0.005 – 0.170 mm (0.0002 – 0.007 in.) after one year of service in the field. The change in top coating thickness was within the experimental error of the measurement method and thus considered insignificant for all samples but Sample LV1. Its top coating thickness over scrim dropped 0.167 mm (0.007 in.) after one year of exposure. In some cases, this variance may be due to the manufacturing tolerances. However, more data is required to see if this trend continues Linear Dimensional Change The linear dimensional change of the samples is summarized in Table 4. Each entry is the average and standard deviation of three individual measurements Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 67 Figure 2 – Thickness, sheet overall of TPO samples: Alaska, Las Vegas, Seattle, and Texas. on one specimen. The linear dimensional change of all samples was less than ±0.4%, which was within the maximum allowable limit specified in ASTM D6878 for new TPO membranes. No significant difference was observed between the unexposed and the exposed samples. This indicated that the samples remained dimensionally stable after one year of service in the field. Water Absorption The amount of water absorption of the samples is summarized in Table 5. Each entry is the average and standard deviation of three specimens unless otherwise specified. The water absorption changes by weight of all samples (see Figure 4) was less than ±0.4%, which was well within the maximum allowable limit of ±3% as specified in ASTM D6878 for new TPO mem- Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 68 Proceeedings of the RCI 21st International Convention Exposure Thickness Over Scrim** Exposure Thickness Over S c r i m * * Sample Time Thickness Changes Sample Time Thickness Changes ID* (yrs) (mm)+ (mm) ID* (yrs) (mm)+ (mm) AK1 0 0.529 – AK3 0 0.537 – 1 0.494 0.035 1 0.451 -0.086 3 0.461 0.068 3 0.445 -0.092 AK2 0 0.507 – AK4 0 0.555 – 1 0.475 -0.032 1 0.539 -0.016 3 0.388 -0.119 3 0.430 -0.125 LV1 0 0.643 – LV3 0 0.623 – 1 0.476 -0.167 1 0.501 -0.122 3 0.511 -0.132 3 0.497 -0.126 LV2 0 0.574 – LV4 0 0.551 – 1 0.536 -0.038 1 0.491 -0.060 3 0.519 -0.055 ` 3 0.458 -0.093 SEA1 0 0.492 – SEA3 0 0.584 – 1 0.488 -0.004 1 0.526 -0.058 3 0.430 -0.062 3 0.500 -0.084 SEA2 0 0.476 – SEA4 0 0.501 – 1 0.393 -0.083 1 0.477 -0.024 3 0.383 -0.093 3 0.400 -0.101 TX1 0 0.555 – TX3 0 0.552 – 1 0.486 -0.069 1 0.446 -0.106 3 0.554 -0.001 3 0.414 -0.138 TX2 0 0.616 – TX4 0 0.508 – 1 0.589 -0.027 1 0.498 -0.010 *AK = Alaska; LV = Las Vegas; SEA = Seattle; TX = Texas; (1-4) = Manufacturer # **Fiber (cut along XD fiber) +1 inch = 25.4 mm ASTM D 6878-03 specification: 0.305 mm (0.012 in) Table 3 – Average thickness, coating over scrim of unexposed, 1- and 3-year exposed TPO roof membranes. Figure 3a – Thickness, coating over scrim of TPO samples: Alaska and Las Vegas. branes. This indicated that the weathered surface of the samples was resistant to water absorption. It is interesting to note that all the exposed samples had positive water absorption values while some of the unexposed samples had negative water absorption values up to -0.15%; i.e., they lost weight after being in contact with water at 70°C (158°F) for seven days. It is suspected that the weight loss was due to heat exposure in the oven. To estimate the weight loss due to the heat exposure, two small rectangular specimens of dimensions 25 mm x 50 mm (1 in. x 2 in.) were cut from each sample and placed in a convection oven at 70 ± 2°C (158 ± 3°F) for seven days, the same temperature and exposure period as the water absorption test. The weight loss due to heat exposure only was calculated from the weights of the specimens before and after heating. The weight loss ranged from 0 – 0.25% with an average of about 0.1%. The measurement error of the electronic balance was ±0.001 g, which corresponded to about Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 69 *n/a = not enough material for testing ASTM D 6878-03 specification for membranes new: ±1% Table 4a – Linear dimensional change of unexposed, 1- and 3-year exposed TPO roof membranes (continued on next page). Figure 3b – Thickness, coating over scrim of TPO samples: Seattle and Texas. Exposure Linear Dimensional Change(%) Linear Dimensional Change (%) Sample Time (yrs) Machine Direction Change (%) Cross Direction Change (%) AK1 0 -0.10±0.04 – -0.09±0.02 – 1 n/a* – n/a* – 3 -0.05±0.03 0.05 -0.03±0.01 0.06 AK2 0 -0.23±0.04 – -0.26±0.06 – 1 -0.16±0.00 0.07 -0.12±0.02 0.14 3 -0.16±0.02 0.07 -0.07±0.01 0.19 AK3 0 -0.06±0.06 – -0.06±0.05 – 1 -0.09±0.00 -0.03 -0.03±0.00 0.03 3 -0.06±0.01 0.00 0.00±0.00 0.06 AK4 0 -0.16±0.06 – -0.04±0.02 – 1 -0.06±0.06 0.10 -0.05±0.00 -0.01 3 -0.07±0.01 0.09 0.00±0.00 0.04 LV1 0 0.18±0.01 – -0.05±0.02 – 1 -0.03±0.01 -0.21 -0.08±0.01 -0.03 3 -0.03±0.01 -0.21 0.04±0.00 0.09 LV2 0 -0.05±0.01 – -0.10±0.07 – 1 -0.06±0.02 -0.01 -0.13±0.00 -0.03 3 -0.11±0.02 -0.06 0.01±0.01 0.11 LV3 0 n/a* – n/a* – 1 -0.03±0.01 – -0.04±0.00 – 3 -0.02±0.00 – 0.03±0.01 – LV4 0 -0.12±0.04 – -0.03±0.01 – 1 -0.05±0.01 0.07 -0.02±0.01 0.01 3 -0.04±0.01 0.08 0.03±0.00 0.06 0.02% of the weight of the specimen (about 4.5 g). Therefore, within measurement error of the balance, this confirmed that the negative water absorption data came from weight loss of the samples due to heating. Since the samples lost weight due to heat exposure in the oven while gaining weight from water absorption at the same time, the final weight measurement in the water absorption test underestimated the actual weight gain due to water absorption. The actual water absorption values should be the sum of weight loss due to heat exposure and the water absorption data, based on final weight measurement (Table 5). The average weight losses due to heat exposure in the oven are low: 0.11% and 0.18% for the unexposed and the exposed samples, respectively. The measured water absorption data were less than ±0.4%. After adjusting the weight loss due to heat exposure, the actual water absorption would still be within the maximum allowable limit of ±3% for the samples tested. In other situations where the samples are sensitive to losing weight due to heat exposure, it is important to adjust the water absorption data accordingly. Tensile Test Tensile Response and General Observations The mechanical response of the samples under tensile loading was measured and displayed as force-displacement curves. They varied with manufacturers, test direction, and exposure. There were two types of samples made by manufacturer #2: AK2 and SEA2 consisted of black and white polymer matrix; while LV2 and TX2 had grey and white polymer matrix. They responded differently to tensile loading. For AK2 and SEA2 (black and white), after the reinforcement broke, the polymer matrix bore the load. Stress concentration was observed at fiber bundles running across the width of the specimen and cracks started to form and propagate in these areas until the specimen failed. The polymer plies remained intact where no fiber was present. The same failure mode was observed for the exposed samples in XD. However, the samples in MD changed failure mode after one year of field service. The specimen broke in the top ply, and the bottom ply continued to stretch and peel away from the top ply. The change in failure type possibly indicated that the bonding between the polymer plies was weakened after exposure. Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 70 Proceeedings of the RCI 21st International Convention Exposure Linear Dimensional Change(%) Linear Dimensional Change (%) Sample Time (yrs) Machine Direction Change (%) Cross Direction Change (%) SEA1 0 -0.06±0.01 – -0.12±0.02 – 1 -0.04±0.02 0.02 -0.09±0.02 0.03 3 -0.04±0.01 0.02 0.02±0.01 0.14 SEA2 0 -0.36±0.02 – -0.22±0.01 – 1 -0.08±0.06 0.28 -0.29±0.02 -0.07 3 -0.21±0.02 0.15 0.10±0.00 0.32 SEA3 0 n/a* – n/a* – 1 -0.05±0.03 – 0.00±0.02 – 3 -0.03±0.01 – 0.09±0.02 – SEA4 0 -0.19±0.04 – -0.06±0.03 – 1 -0.15±0.04 0.04 0.00±0.01 0.06 3 -0.07±0.01 0.12 0.05±0.03 0.11 TX1 0 0.05±0.02 – -0.03±0.04 – 1 -0.01±0.01 -0.06 -0.02±0.02 0.01 3 -0.01±0.00 -0.06 -0.04±0.01 -0.01 TX2 0 -0.15±0.04 – -0.04±0.02 – 1 -0.09±0.01 0.06 -0.08±0.04 -0.04 3 -0.07±0.01 0.08 -0.03±0.01 0.01 TX3 0 -0.09±0.03 – -0.05±0.02 – 1 -0.06±0.01 0.03 -0.04±0.01 0.01 3 0.00±0.01 0.09 -0.02±0.01 0.03 TX4 0 -0.13±0.00 – -0.09±0.02 – 1 -0.04±0.01 0.09 -0.10±0.02 -0.01 3 -0.03±0.02 0.10 0.00±0.01 0.09 Table 4b – Linear dimensional change of unexposed, 1- and 3-year exposed TPO roof membranes (continued from previous page). *n/a = not enough material for testing ASTM D 6878-03 specification for membranes new: ±1% Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 71 Measured Corrected Sample Exposure Water Change Water Change ID Time (yrs) Absorption % % Absorption % (%) AK1 0 -0.05 – 0.01 – 1 0.07 0.12 0.30 0.29 3 0.09 0.14 0.29 0.28 AK2 0 -0.12 – -0.09 – 1 0.05 0.17 0.19 0.28 3 0.10 0.22 0.19 0.48 AK3 0 -0.07 – 0.06 – 1 0.05 0.12 0.24 0.18 3 0.07 0.14 0.36 0.30 AK4 0 0.01 – 0.09 – 1 0.07 0.06 0.18 0.09 3 0.06 0.05 0.27 0.18 LV1 0 -0.15 – -0.05 – 1 0.08 0.23 0.13 0.18 3 0.23 0.38 0.31 0.36 LV2 0 -0.02 – -0.02 – 1 0.17 0.19 0.23 0.25 3 0.30 0.32 0.50 0.52 LV3 0 0.35 0.38 – 1 0.36 0.01 0.47 0.09 3 0.50 0.15 0.61 0.23 LV4 0 0.02 – 0.15 – 1 0.14 0.12 0.27 0.12 3 0.36 0.34 0.46 0.31 SEA1 0 0.11 – 0.17 – 1 0.08 -0.03 0.08 -0.09 3 0.24 0.16 0.39 0.22 SEA2 0 0.07 – 0.16 – 1 0.03 -0.04 0.15 -0.01 3 0.28 0.21 0.58 0.42 SEA3 0 0.24 – 0.27 – 1 0.04 -0.20 0.18 -0.09 3 0.18 -0.06 0.47 0.20 SEA4 0 0.06 – 0.09 – 1 0.08 0.02 0.19 0.10 3 0.22 0.16 0.56 0.47 TX1 0 -0.10 – -0.04 – 1 0.12 0.22 0.15 0.19 3 0.24 0.34 0.46 0.50 TX2 0 0.01 – 0.04 – 1 0.09 0.08 0.12 0.08 3 0.27 0.26 0.44 0.40 TX3 0 0.13 – 0.21 – 1 0.19 0.06 0.27 0.06 3 0.41 0.28 0.52 0.31 TX4 0 0.01 – 0.01 – 1 0.14 0.13 0.24 0.23 3 0.22 0.21 0.51 0.50 Table 5 – Water absorption values for unexposed, 1- and 3-yr exposed TPO roof membranes. Note: Negative weight change denotes weight loss. ASTM D 6878-03 specification: ±3% Figure 4: Water absorption changes of TPO samples. Water Absorption ±3% Allowed For LV2 and TX2 (grey and white), in MD, after the reinforcement broke, the polymer matrix did not stretch much before failure, with ultimate elongation around 100%. Exposure reduced the ultimate elongation further. In XD, the polymer matrix elongated over 200% before failure. It is suspected that the polymer matrix might have been strengthened or weakened preferentially during the manufacturing process of the membranes. The four failure types were the same at the beginning and the differences occurred after the reinforcement break, i.e. the differences reflected the tensile behavior of the polymer matrix. Weathering also affects polymer matrix predominantly as it was directly exposed to the elements. On the other hand, the tensile properties such as breaking strength and elongation at break are mainly controlled by the reinforcement. Therefore, outdoor exposure could have affected the polymer matrix (thus different failure types) in this case but the tensile properties remained relatively unchanged. However, if the polymer matrix continues to degrade, as it would be expected due to weathering effects, the reinforcement underneath the polymer ply will eventually be exposed and this may affect its performance. The tensile breaking strength and the elongation at break are summar i z e d i n Tables 6 and 7. Note t h a t procedure B – strip t e s t Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 72 Proceeedings of the RCI 21st International Convention Table 6 – Breaking strength of unexposed, 1- and 3-year exposed TPO roof membranes. *(MD) = Machine direction **1 Newton (N) = 0.2248 lbs +(XD) = Cross direction ASTM D 687803 specification: 976 N (220 lbf) is for grab method and it does not apply to this data, which is for the strip method. Sample Exposure Breaking Strength (MD)* Breaking Strength (XD)+ ID Time (yrs.) N** Change N** Change AK1 0 956 ± 38 – 922 ± 21 – 1 995 ± 13 39 904 ± 37 -18 3 985 ± 14 30 903 ± 19 -19 AK2 0 883 ± 36 – 735 ± 39 – 1 801 ± 30 -82 747 ± 25 12 3 715 ± 19 -168 682 ± 28 -53 AK3 0 896 ± 17 – 736 ± 50 – 1 919 ± 60 23 733 ± 16 -3 3 926 ± 21 30 701 ± 21 -35 AK4 0 1055 ± 27 – 849 ± 30 – 1 969 ± 18 86 838 ± 11 -11 3 974 ± 37 -81 853 ± 4 4 LV1 0 970 ± 40 – 808 ± 40 – 1 950 ± 41 -20 806 ± 29 -2 3 976 ±10 6 775 ± 18 -33 LV2 0 862 ± 30 – 748 ± 30 – 1 884 ± 40 22 742 ± 30 -6 3 913 ± 6 51 815 ± 23 67 LV3 0 876 ± 40 – 709 ± 10 – 1 815 ± 21 -61 773 ± 32 64 3 811 ± 28 -65 746 ± 28 37 LV4 0 951 ± 40 – 767 ± 10 – 1 964 ± 11 13 740 ± 17 -27 3 913 ± 24 -38 753 ± 4 -14 SEA1 0 958 ± 31 – 846 ± 25 – 1 995 ± 32 37 873 ± 39 27 3 929 ± 40 -29 857 ± 8 11 SEA2 0 801 ± 10 – 596 ± 17 – 1 827 ± 18 26 705 ± 29 109 3 857 ± 33 56 622 ± 32 26 SEA3 0 865 ± 20 – 677 ± 32 – 1 857 ± 29 -8 809 ± 20 132 3 897 ± 33 32 827 ± 8 150 SEA4 0 968 ± 40 – 827 ± 42 – 1 975 ± 51 7 771 ± 30 -56 3 1025 ± 36 57 842 ±13 15 TX1 0 961 ±29 – 819 ± 31 – 1 909 ± 33 -52 780 ± 19 -39 3 945 ± 5 16 746 ± 31 -73 TX2 0 823 ± 28 – 727 ± 31 – 1 858 ± 25 35 655 ± 36 -72 3 870 ± 35 47 731 ±24 4 TX3 0 912 ± 22 – 720 ± 25 – 1 831 ± 15 -81 740 ± 24 20 3 808 ± 7 -104 741 ± 25 21 TX4 0 962 ± 19 – 749 ± 31 – 1 964 ± 6 2 766 ± 18 17 3 940 ± 26 -22 680 ± 20 -69 method was used instead of procedure A – grab test method in ASTM D751 due to the lack of materials. The ASTM specification for tensile breaking strength of 976 N (220 lbf) was based on the grab test method; therefore, the value was put on the figures for reference only. However, samples were tested before and after exposure. Therefore, if the membrane material undergoes any changes after exposure, it is possible to compare the results obtained by the same method. The tensile breaking strengths of the samples were 800 – 1050 N (180 – 235 lbf) and 650 – 920 N (145 – 205 lbf) for MD and XD, respectively. They were generally lower than the ASTM specification of 976 N (220 lbf) because strip test method was used instead of the grab test method. As expected, the breaking strength in the MD was equal or stronger than the XD. In general, there was no significant difference between the unexposed and the exposed samples. One year of service in the field did not affect the tensile breaking strength of the samples. The breaking strength between the samples made by different manufacturers was similar, mostly within ±15%. The tensile elongations at break of the samples are 29 – 44% and 26 – 46% for MD and XD, which significantly exceeded the ASTM specification of 15%. They were similar for MD and XD. The difference between the unexposed and the exposed samples was generally small, less than ±20%. One exception was Sample SEA2u, whose elongation at break increased by about 45% after exposure. Unfortunately, due to the lack of samples, only one specimen was tested in the unexposed samples so its statistical validity is questionable. The elongation at break Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 73 Table 7 – Elongation at break of unexposed, 1- and 3-year exposed TPO roof membranes. *(MD) = Machine direction +(XD) = Cross direction ASTM D 687803 specification: 15% Sample Exposure Elongation at Break (MD)* Elongation at Break (XD)+ ID Time (yrs.) % Change % Change AK1 0 38.5 ± 4.7 – 39.0 ± 0.7 – 1 38.9 ± 0.9 0.4 34.2 ± 1.4 -4.8 3 39.9 ± 1.5 1.4 34.0 ± 1.6 -5.0 AK2 0 33.5 ± 3.2 – 27.3 ± 4.8 – 1 32.3 ± 2.3 1.2 32.4 ± 1.2 5.1 3 31.9 ± 2.5 1.6 27.3 ± 0.9 0.0 AK3 0 33.9 ± 4.3 – 38.9 ± 1.2 – 1 31.0± 0.8 -2.9 36.9 ± 1.2 -2.0 3 35.1 ± 0.4 1.2 32.1 ± 0.6 -6.8 AK4 0 32.9 ± 2.0 – 41.7 ± 2.0 – 1 30.5 ± 1.0 -2.4 42.9 ± 0.4 1.2 3 33.6 ± 1.5 0.7 40.8 ± 0.5 -0.9 LV1 0 39.4 ± 2.2 – 33.8 ± 1.1 – 1 38.1 ± 1.1 -1.3 30.9 ± 2.2 -2.9 3 36.8 ± 0.7 2.6 28.9 ± 0.6 -4.9 LV2 0 36.1 ± 1.4 – 26.8 ± 1.0 – 1 33.7± 2.3 -2.4 26.3 ± 1.0 -0.5 3 33.7 ± 1.0 -2.4 25.8 ± 0.8 -1.0 LV3 0 36.3 ± 1.1 – 29.6 ± 0.1 – 1 35.0 ± 1.2 -1.3 29.2 ± 1.8 -0.4 3 32.5 ± 1.1 3.8 25.7 ± 0.8 -4.0 LV4 0 32.1 ± 0.5 – 32.9 ± 1.4 – 1 30.8 ± 1.1 1.3 30.3 ± 1.7 -2.6 3 28.0 ± 0.7 4.1 28.9 ± 0.7 -4.0 SEA1 0 38.8 ± 3.0 – 41.3 ± 0.3 – 1 36.8 ± 2.7 -2.0 34.2 ± 1.1 -7.1 3 44.6 ± 0.9 5.8 33.9 ± 0.3 -7.4 SEA2 0 40.4 ± 1.2 – 47.0 ± 3.1 – 1 38.0 ± 1.9 -2.4 44.7 ± 2.0 -2.3 3 38.5 ± 1.0 -1.9 37.6 ± 0.8 -9.4 SEA3 0 43.8 ± 2.3 – 36.8 ± 1.4 – 1 40.4 ± 1.7 -3.4 41.3 ± 1.6 4.5 3 41.2 ± 0.6 -2.6 36.5 ± 0.8 -0.3 SEA4 0 34.2 ± 1.7 – 42.4 ± 1.0 – 1 32.2 ± 1.1 -2.0 41.3 ± 1.2 -1.1 3 32.3 ± 0.6 -1.9 41.1 ± 0.9 -1.3 TX1 0 39.5 ± 2.2 – 33.8 ± 1.7 – 1 40.2 ± 2.2 0.7 34.9 ± 1.7 1.1 3 39.8 ± 0.6 0.3 31.5 ± 0.7 -2.3 TX2 0 39.8 ± 0.7 – 32.5 ± 1.3 – 1 37.0 ± 1.8 -2.8 27.2 ± 1.8 -5.3 3 37.0 ± 0.8 -2.8 28.7 ± 1.7 -3.8 TX3 0 34.9 ± 1.0 – 39.3 ± 1.1 – 1 36.4 ± 0.5 1.5 36.8 ± 0.9 -2.5 3 32.9 ± 0.3 -2.0 29.2 ± 1.1 -10.1 TX4 0 41.4 ± 1.6 – 32.5 ± 1.4 – 1 33.8 ± 0.4 -7.6 31.1 ± 2.9 -1.4 3 44.1 ± 1.2 2.7 26.5 ± 0.8 -6.0 value between samples made by different manufacturers was similar, mostly within ±15%. Chemical Analysis Dynamic Mechanical Analysis (DMA) Figure 5A displays typical DMA curves for TPO. The figures shows E’ and E” are the storage and loss modulus, respectively and tan or the damping factor. Figure 5B shows how the Tg was obtained from the E’ and E” curves. The values were obtained from the intersect of two tangents on the storage modulus (E’int) curve as well as from the maximum of the loss modulus (E”max) curve. Due to the large amount of data, the data is not presented here. The Tg obtained storage modulus (E’int) and the maximum of the loss modulus (E”max) curves ranged from -48°C (-54°F) to -42°C (-44°F) and from -35 °C (-31°F) to -32°C (-26°F), respectively. The Tg obtained from the E’int follows a similar trend as that of the E”max; hence, only the latter will be discussed. Regardless of the manufacturer, the glass transition temperature Tg (E”max)] of the unexposed samples and those exposed in Alaska for one year is very similar. The Tg between the unexposed and exposed samples ranges between 0 and +2°C (0 and +4°F). Such Tg is well below the 8°C (16°F) limit recommended by the CIB/RILEM Committee [7] and suggests that one-year exposure to Alaska weather did not have a significant effect on the Tg of the TPO membranes. Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 74 Proceeedings of the RCI 21st International Convention Figure 5A (left) shows typical DMA plot. 5B (right) shows how the Tg was obtained from E’ and E” curves. Figure 6 (left) shows E” curves for an unexposed specimen from Manufacturer #1, while Figure 7 (right) shows the same for Manufacturer #2. Figure 6 shows the E” curves for specimens AK1Au, LV1Au, SEA1u, and TX1Au from Manufacturer #1. The curves for specimens LV1Au and TX1Au show the same maximum [(Tg of -32°C) (-26°F)], which is °C (8°F) higher than that from AK1Au and SEA1Au. The modulus value is slightly higher for the LV1A. The overlay of the E” curves for unexposed specimens from Manufacturer #2 shown in Figure 7 indicates that the Tg (E”max) is very similar for all specimens (-35 to -34°C) (-31°F to -29°F). The curves for AK2Au and SEA2Au specimens are almost identical throughout the temperature range of analysis but this is not the case for the LV2Au and TX2Cu specimens, especially above the Tg region where LV2Au and TX2Cu deviate from the other two curves. The E” curves for unexposed specimens from Manufacturer #3 (Figure 8) have their maximum at -35°C (-31°F). The curves are grouped in sets of two. One is AK3 and LV3 and the other is SEA3 and TX3. On the other hand, specimens from Manufacturer #4 (Figure 9) show similar curves, with exception of SEA4Cu, which shows slightly higher E” modulus value. The differences observed in the curves of the unexposed samples within the same manufacturer may be indicative of some changes during the manufacturing process or they are from different batches. It could also be due to storage location. Although the Tg of the membranes is very similar, it is possible that somehow the reinforcement was placed differently on the membrane. In fact, the reinforcement on the gray, black, and green side (ply) of the membranes does not look the same to the naked eye. For example, the weaving of the reinforcement on the AK1u membrane from Manufacturer #1 is different from that of SEA1u, LV1u, and TX1u membranes. In general, the bottom sheet (underlap) of an exposed roof membrane sample has a Tg closer to the unexposed sample because it is relatively shielded from the environmental factors than the top (exposed) sheet. If no chemical breakdown of the polymer chains (chain scission) occurs due to exposure, it would be expected that the unexposed or new sample(s) have a lower Tg value than the exposed sample. Changes in Tg lower than 5°C (9°F) after exposure may be considered not significant because the standard deviation of the individual measurements is ±2 (±4°F) experimental error, which corresponds to the temperature ramp of 2°C (4°F) used in the analysis. Specimens taken from the top sheet of pieces 2A (LV2Aet) and LV2D (LV2Ce) from Manufacturer #2 show a similar behavior. However, the change in Tg (-1°C) (-2°F) observed for these two specimens is even lower than that observed for those from Manufacturer #1. Although not shown, the E” curves for the unexposed specimens from these manufacturers overlay quite well that of the unexposed specimen. The DMA results showed, in general, that exposure at the four different locations did not affect the membrane material significantly. Regardless of the manufacturer and exposure location, the Tg of the samples is below the recommended 8°C (16°F) limit. These results are consistent with tensile test results. They also showed that membranes from the four manufacturers were not significantly affected by the Proceeedings of the RCI 21st International Convention Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 75 Figure 8 (top) shows E” curves for unexposed specimens from Manufacturer #3, while Figure 9 (bottom) shows an unexposed specimen from Manufacturer #4. exposure, with exception of LV1, which shows a reduction in thickness. CONCLUSION The test results have been presented in great detail. There are some items that are being closely watched, such as membrane tightening, surface color or hue, reflectivity, membrane thickness overall, thickness of the coating over the scrim, etc. WSRCA’s Low-slope Committee, the assigned TPO Task Group, and WSRCA in general intend to continue monitoring the findings from the field and the laboratory testing through the next round of test cuts and testing. However, it appears too early in the project for anyone to make predictions as to the life expectancy of the current generation of TPO roofing membranes, which appear to be weathering quite well on the four WSRCA TPO Weathering Farm test sites. REFERENCES 1. ASTM D751-00 Standard Test Method for Coated Fabrics 2. ASTM D6878-03 Standard Specification for Thermoplastic Polyolefin Based Sheet Roofing 3. ASTM D1204-02 Standard Test Method for Linear Dimensional Changes of Nonrigid Thermoplastic Sheeting or Film at Elevated Temperature 4. ASTM D471-98 Standard Test Method for Rubber Property – Effect of Liquids 5. ASTM D 6382-99 Standard Practice For Dynamic Mechanical Analysis and Thermogravimetry of Roofing and Waterproofing Membrane Material 6. ASTM D 5418-01 Standard Test Method for Measuring The Dynamic Mechanical Properties of Plastic using a Dual Cantilever Beam 7. Thermal Analysis Testing of Roofing Membranes Materials. Final Report of the Thermal Analysis Task Group RILEM 120- MRS/CIB W.83 Joint Committee on Membranes Roofing Systems, December 1995. ACKNOWLEDGEMENTS The authors wish to thank all those helping with this project. Participating contractors: Snyder Roofing, Kyle King and Tim Gardner of Snohomish, Washington; Industrial Roofing, Jesse Martin and Bill Kramer (former owner) of Anchorage, Alaska; American Roofing, Richard Higgs and Eddie Spalten of San Antonio, Texas; and Commercial Roofing, Dennis Conway and Bruce Martin of Las Vegas, Nevada. Participating manufacturers (in alphabetical order): Carlisle Syntec Inc., with project representative Randy Oberg; Firestone Building Products, represented by Jim Jannasch; Genflex Roofing Systems, represented by Mike Hubbard; and Stevens Roofing Systems, represented by Steve Moskowitz. WSRCA’s Low-Slope Technical Committee: Tom Bradford, chairman; Greg Bolt, co-chairman; Bill Baley; KC Barnhardt, executive liaison; Chuck Chapman, Chris Dean, Don Fry, Tom Johns, Christian Madsen, Gene Meyer, David Montross, Dennis Ryan. Dr. Karen Liu, Sebastian Evoniak, National Research Council of Canada. Carlson, Delgado, Rosenow, Barnhardt, and Paroli – 76 Proceeedings of the RCI 21st International Convention