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NCHRP Report 696: Performance of Corrugated Pipe Manufactured with Recycled Polyethylene Content (2011)
National Cooperative Highway Research Program (NCHRP)

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Thomas, Richard W, Cuttino, David, Transportation Research Board. "A.2.4 Percentage Black/Color + Ash (ASTM D4218)." NCHRP Report 696: Performance of Corrugated Pipe Manufactured with Recycled Polyethylene Content. Washington, DC: The National Academies Press, 2011.

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Page
56
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Page
56
Front Matter (R1-R11)
Summary (1-2)
Chapter 1 - Introduction (3-3)
Short-Term Properties (4-4)
Service Lifetime of PE (5-7)
The SIM for Predicting Creep and Creep Rupture (Stage I) Properties (8-11)
The FL-DOT Junction Test (12-12)
The Long-Term Oxidation (Stage III) Resistance (13-13)
Specifications (14-14)
Post-Industrial Recycled Polyethylene (15-15)
Post-Consumer Recycled High-Density Polyethylene (16-16)
PCR Mixed-Color Resin (17-17)
The Effects of Contamination (18-18)
The Effects of Melt Filtration (19-20)
The Effect of Silicone Rubber (21-23)
Phase 2 - Recycled-Resin Blends (24-25)
Blends Made with Mixed-Color PCR (26-27)
Blends Made with Natural PCR (28-29)
Blends Made with PIR-HD (30-31)
Index Test Results (32-33)
Stress-Crack Test Results (34-36)
Long-Term Tensile Strength by SIM (37-39)
Long-Term Creep Strain and Modulus by SIM (40-40)
Long-Term Stress-Crack Resistance (41-41)
Combined SIM (Stage I) and BFF (Stage II) Service-Lifetime Estimates (42-44)
The BFF Test for QC (45-45)
Designing Pipe with Recycled Content (46-46)
Proposed Draft Specifications (47-48)
Phase 2 - Recycled PE Blends (49-49)
Phase 3 - Pipe Made from Recycled-Resin Blends (50-53)
References (54-54)
Appendix A - Procedures and Test Methods (55-55)
A.2.4 Percentage Black/Color + Ash (ASTM D4218) (56-56)
A.2.6 Percentage Polypropylene (TRI Method) (57-58)
A.2.8 Flexural Modulus (ASTM D790) (59-59)
A.3.2 BAM Stress-Crack Test (TRI Method) (60-61)
A.3.3 BFF Test (TRI Method) (62-62)
A.3.4 Junction Test (FDOT FM 5-572) (63-63)
A.4.1 Stepped Isothermal Method (SIM) For Long-Term Creep Modulus and Strain (ASTM D6992) (64-64)
A.4.3 BFF Test for Long-Term Stress Crack Resistance (TRI Method) (65-68)
Appendix D - Pipe Containing Recycled HDPE (69-69)
Appendix E - Proposed Draft Standard Specification for PCR MCR High-Density PE Bottles for Use in AASHTO-Approved Corrugated Drainage Pipe (70-76)
Appendix F - Proposed Draft Standard for Recycled Content Containing HDPE Resin Formulations for Corrugated Pipe Made to AASHTO Standard M252-Recycled (77-84)
Appendix G - Proposed Draft Standard Specification for Recycled Content Containing HDPE Resin Formulations for Corrugated Pipe Made to AASHTO Standard M294-Recycled (85-93)
Appendix H - Proposed Draft Standard Specification for Corrugated Polyethylene Drainage Pipe Containing Recycled Polyethylene, 75- to 250-mm Diameter (94-108)
Appendix I - Proposed Draft Standard Specification for Corrugated Polyethylene Drainage Pipe Containing Recycled Polyethylene, 300- to 1,500-mm Diameter (109-129)
Abbreviations used without definitions in TRB publications (130-130)

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A-2 A.1 Procedures mold temperature was recorded and the cooling process begun. The mold temperature was lowered by slowly open- A.1.1 Melt Blending by Extrusion ing a needle valve with cooling water. The temperature was All blending and extruding was performed on a laboratory recorded every 30 seconds and the cooling was done at a rate line consisting of a Welding Engineers Model HT8-222-2251 of 15°C ± 2°C. Once the temperature was below 50°C, the Twin Screw Extruder, a custom-built cooling bath equipped mold was removed. with a chiller and circulator and a Berlyn Corporation Model HV1 Pelletizer. The extruder has counter-rotating screws at an A.2 Index Test Methods L:D ratio of 24:1. The extruder temperatures were set at 115°C (240°F) for the feed zone, and 177°C (350°F) for the mixing and A.2.1 Density (ASTM D1505) metering zones. The die temperature was also 177°C (350°F). The density of the samples was determined by ASTM D1505, The die was a single 6.35-mm (0.25-in.) diameter rod and the Standard Test Method for Density of Plastics by the Density- die was fitted with two, 1-in. diameter melt filter screen holders. Gradient Technique. The test is performed with the use of a All samples for extrusion were dry blended then gravity glass column filled in a specified procedure with isopropanol fed. The batch size was typically 2.2 lb (1 kg). The screw speed and water that creates a gradient of densities from around was set at 220 rpm, which produced an output rate of about 0.910 to 0.970 g/cm3. Standard glass density beads are placed 6.8 kg/hr (15 lb/hr). The residence time in the extruder was less in the column for calibration. Samples are cut into small pieces than 45 seconds. (1/16-in. diameter), degassed under vacuum in isopropanol, Samples of recycled regrind chips were melt blended twice and placed in the column. Once settled, the position is recorded and recycled reprocessed pellets were melt blended once. from a graduated scale on the glass column and the density All the experimental blends were melt blended three times calculated from the position of the standard beads. to ensure optimum blending. Virgin resins were also blended in the same manner to duplicate the heat history of the blends. It is worth mentioning that the processing conditions used A.2.2 Melt Flow Index and Flow Rate during this study are different than what is actually going on (ASTM D1238) in the recycled suppliers' plants or in the pipe manufacturers' The melt index was determined in accordance to ASTM plants. First of all, the twin screw mixes much better than a D1238, Standard Test Method for Flow Rates of Thermoplastics single screw, or even a high-length/diameter single screw. So, by Extrusion Plastometer. A sample of plastic was heated inside the blends studied herein were optimally blended. Secondly, the a standard-sized cylinder for a controlled amount of time. study on the effects of polypropylene (PP) might not translate Then, a weight was applied, forcing the molten plastic through well to the plants because the PP may not be as well blended a standard die. The mass of plastic that is extruded through the as in the study. And thirdly, the twin screw processing is very die in a specific period of time was reported. Two conditions gentle compared to a large single screw. So, even though there were used for the polyethylene samples in this study. The first were no signs of oxidation in the study on the twin screw, oxi- were a temperature of 190°C and a load of 2.16 kg (Melt dation may still be an important consideration in the plants. Index) and the second were a temperature of 190°C and a load of 21.6 kg (Flow Rate). The results are reported as grams per A.1.2 Plaque Preparation (ASTM D4703) 10 minutes. The melt flow tests were performed on pellets after melt Sample plaques were prepared according to ASTM D4703, blending. Practice for Compression Molding Thermoplastic Materials into Test Specimens, Plaques, or Sheets on a Pasadena Hydraulic Industries Model P215H Platen Press. Two sizes of plaques A.2.3 Percentage Volatiles (TRI Method) were prepared. The plaque used for the BAM test specimens Duplicate 2.000 g ± 0.100 g samples were placed in an alu- was 15.24 cm × 15.24 cm × 1.27 mm (6 in. × 6 in. × 0.05 in.). minum weighing boat and heated at 175°C for 1 hour in a The plaque used for all other tests was 17.78 cm × 17.78 cm × forced air oven. Upon cooling, the final weight was obtained 1.9 mm (7 in. × 7 in. × 0.075 in.). The smaller mold used 50g and the percentage volatiles were calculated. This test was of pellets while the larger one used 75g. performed on the as-received pellets, before melt blending. The open cavity mold was charged with pipe pieces about 5 cm × 5 cm in between two Mylar release sheets and placed A.2.4 Percentage Black/Color Ash in the press, which was preheated to 190°C. Once the mold (ASTM D4218) reached 160°C, the set-point temperature was reduced to 177°C and the mold quickly pressed to 20.68 MPa (3000 psi). This was done by the muffle furnace method described in After the plastic was allowed to relax for at least 5 minutes, the ASTM D4218, Test Method for Determination of Carbon Black