NTPEP Evaluation of Asphalt Release Agents

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1 Standard Practice for NTPEP Evaluation of Asphalt Release Agents AASHTO Designation: [ARA 14-01] American Association of State Highway and Transportation Officials 444 North Capitol Street N.W., Suite 249 Washington, D.C

2 Standard Practice for NTPEP Evaluation of Asphalt Release Agents AASHTO Designation: [ARA 14-01] INTRODUCTION The National Transportation Product Evaluation Program (NTPEP) was established to minimize the amount of duplicative testing of transportation materials performed by AASHTO member states by providing a process where manufacturers submit their products to NTPEP for laboratory and/or field testing. The results of the testing are then shared with member Departments for their use in product quality verification. This practice provides the NTPEP member departments information on the asphalt release agents testing program. In keeping with the NTPEP philosophy of purely testing materials, no conclusions are provided with the test results. The evaluation of the test results is left up to each member department. Texas is the lead state and is responsible for the oversight of the testing program for the asphalt release agents. 1. SCOPE 1.1 This standard practice covers the requirements and testing criteria for the National Transportation Product Evaluation Program (NTPEP) evaluation of asphalt release agents. The National Transportation Product Evaluation Program (NTPEP) serves the member departments of the American Association of State Highway and Transportation Officials (AASHTO). 1.2 The results of this program may be used for product quality verification by individual member Departments. If used for quality verification, a letter of certification from the asphalt release agent manufacturer indicating testing was conducted by NTPEP that supports published values may be required by member Departments. 1.3 This standard practice may involve hazardous materials, operations, and equipment. It does not purport to address all safety problems associated with its use. It is the responsibility of the user of this standard practice to establish the appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. REFERENCED DOCUMENTS 2.1 AASHTO Standards: AASHTO M 320, Performance-Graded Asphalt Binder AASHTO M 323, Superpave Volumetric Mix Design ASTM Standards AASHTO T 85, Specific Gravity of and Absorption of Coarse Aggregate AASHTO T 200, ph of Aqueous Solutions with the Glass Electrode NTPEP ARA AASHTO

3 2.2 ASTM Standards: 2.3 Other References ASTM D 92, Test Method for Flash and Fire Points by Cleveland Open Cup Tester ASTM D 93, Flash Point by Pensky-Martens Closed Cup Tester ASTM D 1193, Standard Specification for Reagent Water ASTM D 1475, Density of Liquid Coatings, Inks, and Related Products ASTM D 2369, Volatile Content of Coatings ASTM D 3625, Standard Practice for Effect of Water on Bituminous-Coated Aggregate Using Boiling Water ASTM E 502, Selection and Use of ASTM Standards for the Determination of Flash Point of Chemicals by Closed Cup Methods ASTM E 1252, Practice for General Techniques for Obtaining Infrared Spectra for Qualitative Analysis Resource Conservation and Recovery Act (RCRA) Hazardous Waste Code of Federal Regulations (CFR), Title 40, Part 261, Subpart D, List of Hazardous Waste. CFR Title 29, Hazard Communication. 3. SUMMARY OF PRACTICE Asphalt release agent manufacturers will be permitted to submit their products to be tested and evaluated on a quarterly basis (January, April, July and October). These products are evaluated and laboratory tested by a NTPEP contracted laboratory. Test result data is entered into the webbased NTPEP DataMine program. 4. SIGNIFICANCE AND USE This standard practice utilizes laboratory testing to evaluate asphalt release agents relating to the following: Susceptibility of stripping of asphalt from aggregates in truck beds and on other paving equipment when using asphalt release agents. Susceptibility of a hot mix asphalt (HMA) mixture adhering to the beds of haul trucks or paving equipment when using asphalt release agents. Susceptibility of hot asphalt binders adhering to plant and paving equipment, rakes, shovels, etc. when using asphalt release agents. This practice is intended to only determine the properties of these materials. Acceptability of each material, based upon the data generated as a result of the testing and evaluation in this practice, is the responsibility of the user. NTPEP ARA AASHTO

4 5. APPLICATION FOR PRODUCT TESTING 5.1 Submittal of Product Evaluation Form(s) and other information. The manufacturer will submit an electronic Product Evaluation Form (epef) to the NTPEP Manager through DataMine ( For each product submitted, the manufacturer will be asked to provide a Rank Order List, product literature, MSDS information, and payment. After review of the PEF(s) for completeness and accuracy, the NTPEP Manager will work with the lead state Coordinator to decide on the products to be tested. The decision will be based upon the number of total products submitted for testing by all the manufacturers and their rank order lists. The NTPEP Manager will then advise the manufacturer within two weeks of receipt of the PEF the products approved for testing. Note 1 At times, it may be necessary to limit the number of submittals from each manufacturer for an evaluation period to maintain a manageable work load. Any decision by the technical committee to limit submittals for a cycle will be based on the testing capacity of the contracted laboratory(s). 5.2 Assignment of Test Number A test number shall be assigned to each product approved for testing. The test number shall indicate the Asphalt Release Agent designation (ARA), the year of submission, the submission cycle, and a sequential sample number (ARA-Year-Cycle-Sample No.). For example: ARA would be assigned to an asphalt release agent submitted in 2010 for cycle 2 and was the 4 th product submitted. Note 2 Asphalt Release Agent (ARA) numbers that are assigned to a Manufacturer s product will not change for the life of the test. The Product Name that the manufacturer gives the product at the time of application will be allowed to change until the first data is issued to the manufacturer for review. Once this report is submitted to the manufacturer for review, no changes to the product name will be allowed. Note 3 Product Evaluation Form(s) Submittal Deadlines - Product Evaluation Forms (PEF) shall be submitted electronically in DataMine by the deadline set forth by the NTPEP Manager in order for testing to commence in January, April, July, and October (Testing Cycle 1, 2, 3 and 4, respectively) of the year in which evaluation is to begin. The deadline will be on the closest normal business day a minimum of three weeks prior to commencing testing. 6. EVALUATION OF ASPHALT RELEASE AGENTS 6.1 The testing protocols for Asphalt Release Agents are described beginning in Section 10. With the exception of the Infrared Spectra test, all other tests will be performed and reported in triplicate to comply with repeatability requirements. 6.2 The evaluation laboratory(s) shall be selected by the technical committee and may be the lead testing state, a NTPEP member state's laboratory, and/or a private independent laboratory. 6.3 Field evaluation will not be conducted under this work plan. However, state DOTs may require and conduct field evaluations of materials at their discretion. 7. MANUFACTURER'S DOCUMENTATION 7.1 Upon submittal to the NTPEP, the manufacturer shall supply certified documentation showing the brand name and designation; the composition or description of the asphalt release agent; the NTPEP ARA AASHTO

5 manufacturer s recommended dilution ratio; the product formulation (fingerprint); the Material Safety Data Sheets (MSDS); and the manner in which the material will be identified on containers. Multiple dilution ratios may be submitted for different applications but limited to five (5) per product. Each dilution ratio will require a new product submission per Section This work plan is intended to address asphalt release agents which protect worker safety and which have low environmental impact. The manufacturer shall submit documentation that asphalt release agents acceptable for submission: Contain components that do not exceed the acceptable limits and shall contain no polychlorinated byphenyls (PCBs), Have a rating no higher than zero (0) for all National Fire Protection Association (NFPA) Hazard Codes. If using the Hazardous Materials Identification System (HMIS), a rating no higher than one (1) is acceptable for Health and a zero (0) is required for both Flammability and Reactivity codes, Do not contain flammable materials, solvents, or petroleum elements, and Have a flash point greater than 400 F (204 C) on the undiluted product as measured by ASTM D 93. If no flash point is observed up to 400 F (204 C) due to boiling of the material in the closed cup test (ASTM D 93), open cup flash point testing per ASTM E 502 and D 92 is required. Submit a letter and the test data from both tests in the application. If no flash point is observed in either test, report the Flash Point in the application as None. 7.3 The manufacturer shall indicate when this is a re-submittal, either due to a product change as described in Section 8.2 or due to the 3-year time requirement described in Section The manufacturer shall certify that, unless NTPEP is notified as described in Section 8.1, material furnished under the submitted brand name and designation will be of the same composition and formulation as originally evaluated by NTPEP. 8. PRODUCT CHANGES 8.1 Product Changes If the manufacturer changes the formulation, composition, or concentration, or alters the physical properties of a product previously evaluated by NTPEP, but maintains the same reported name, the manufacturer must notify NTPEP, regardless of whether or not they elect to re-submit the product for testing. The web-based test report will then be revised to note when a previously reported product has a new formulation which has not been evaluated by NTPEP. Note 4 It is recommended that users of the test data require a written certification from the manufacturer stating supplied product is identical to that most recently tested by NTPEP. 8.2 Product Changes (re-submitted) Submitted products, previously evaluated by NTPEP and reported under the same name, but which have had formulation, composition, or concentration changes, or alterations to its physical properties, will be treated as though it were new and not previously evaluated. 9. SAMPLING 9.1 After receipt of the approved submittals, the lead testing state will contact the manufacturer to request random sampling for each material or type to be tested. The sample may be taken from anywhere that is convenient (drums, totes or bulk), provided that it is a random sample that represents a production run of the material. NTPEP ARA AASHTO

6 9.2 Each sample shall consist of 1 gallon (4 liters) of product in a container identified by the manufacturer and shipped along with a Material Safety Data Sheet (MSDS) to the testing laboratory following the instructions of the lead testing state. The sample container shall be labeled. The sample container must show the manufacturer s production labeling, product name, date of manufacture, and batch or lot number. 9.3 Each product must be submitted full strength. Full strength is defined as the strongest concentration of the product available for sale and delivery to customers. Any dilution ratio submitted in the PEF will be diluted from the submitted full strength concentration by the NTPEP Testing Laboratory for testing of both concentrations as stated in Sections and LABORATORY TESTING 10.1 All equipment used for testing under this work plan shall be as described in the test procedures, and shall be calibrated or verified according to applicable AASHTO standards. The testing laboratory will maintain a Quality Control Manual describing calibration and training procedures and schedules. The laboratory shall insure that all applicable standards are available to its technicians and verify that the correct versions of those standards are being used. The Quality Control Manual and all records of training and calibration activities related to asphalt release agent testing for the NTPEP program shall be available for inspection by NTPEP Standard laboratory conditions are defined as a temperature of 77 F ± 7 F (24 C ± 4 C) and a relative humidity of 50 ± 10%. All tests, with the exception of the Infrared Spectra, will be performed in triplicate (3 replicates) Day Asphalt Stripping Test to evaluate the susceptibility of stripping of asphalt from aggregates in truck beds and on other paving equipment when using asphalt release agents Apparatus Eight (8) 1 pt. (0.5 L) glass canning jars or equivalent with a lid for sealing Oven capable of attaining a temperature of 302 ºF (150 ºC) or more Balance, readable to 0.1 g and accurate to 0.5 g White filter paper Materials Use the following materials: Either a plant- or a laboratory-mixed sample of hot mix asphalt (HMA) meeting the following requirements: Table 3 requirements for 1/2 in. (12.5 mm) nominal aggregate size as detailed in AASHTO M 323, Superpave Volumetric Mix Design. Contains an asphalt equivalent to a PG (modified) and a PG (non-modified) as defined in AASHTO M 320, Performance-Graded Asphalt Binder. Two mixes, each containing one of the above asphalt grades, will be produced and used for testing. The percent absorption of the coarse aggregates in the HMA shall be less than 0.5% when computed according to AASHTO T 85, Specific Gravity of and Absorption of Coarse Aggregate. Tested and passes ASTM D 3625 with zero (0) percent stripping Reagent water, ASTM D 1193 Type II Procedure Obtain a representative sample of hot mix asphalt (HMA) mixture. Heat the mixture to 290 ºF (143 ºC). NTPEP ARA AASHTO

7 Split 0.66 lbs. (300 g) of mix into 6 equal amounts of 0.11 lbs. (50 g) each and place into 6-1 pt. (0.5 L) glass jars. Weigh the amount of each 0.11 lbs. (50 g) split sample of mix, prior to placing in the glass jars, to the nearest 0.1 g and record as Wi Place a minimum of 3 fl. oz. (100 ml) of the asphalt release agent at full strength into each of 3 glass jars containing the hot mix asphalt (HMA) mixture described in Section making sure the mixture is completely covered by the asphalt release agent Pour the asphalt release agent at full strength into 1 jar to the same level as those in Section above and use as the control sample Prepare approximately 9 fl. oz. (300 ml) of asphalt release agent diluted with reagent water to the concentration recommended by the manufacturer Place a minimum of 3 fl. oz. (100 ml) of the asphalt release agent at the diluted strength into the remaining 3 glass jars containing the hot mix asphalt (HMA) mixture described in Section above making sure the mixture is completely covered by the asphalt release agent Pour the asphalt release agent at the diluted strength into 1 jar to the same level as those in Section above and use as the control sample Cover the 8 samples and leave them undisturbed for 168 ± 2 hours At the end of the specified time and retaining the mix and liquid in the jars, compare the color of each replicate of asphalt release agent samples to the control samples Weigh each of 6 white filter papers and record to the nearest 0.1 g Place a white filter paper, strong enough to support the weight of the HMA mixture and asphalt release agent liquid without tearing or ripping, into a No. 10 (2 mm) sieve. Another sieve size relatively close to this size may be used. Pour one replicate of the full strength sample onto the filter paper, and with room temperature tap water, lightly rinse the HMA sample over the filter and sieve until the HMA mixture is clean. Repeat with the other 2 full strength replicates and all 3 of the diluted strength replicates Place all 6 of the washed HMA sample and filter paper replicates in an oven at 140 ± 5 F (60 ± 3 C) for 24 hours. Remove the replicates, allow to cool to room temperature, weigh, and record the mass to the nearest 0.1 g. Subtract the initial weight of each filter paper from the combined weight of each mix + filter paper replicate and record to the nearest 0.1 g as Wf Visually observe the aggregate (coarse and fine) for retained bitumen coating for all 6 replicates. Any thin, brownish, translucent areas are to be considered fully coated. Examination of the sample under a light and with low magnification may aid in the visual observation of retained coating Rate the full and the diluted strength asphalt release agent replicates according to the following rating system: No Stripping No stripping or discoloration occurred. Slight Stripping Discoloration of the asphalt release agent. Moderate Stripping Discoloration and stripping of the fine aggregate. Severe Stripping Discoloration, stripping of the coarse and fine aggregate Calculate the percent loss or gain of the initial sample mass as follows: NTPEP ARA AASHTO

8 Where: W is the percent change in the HMA sample mass in percent, Wi is the initial mass of the HMA sample to the nearest 0.1 g (from Section ), Wf is the final mass of the HMA sample after dry back to the nearest 0.1 g (Section ) Report Report the visual stripping rating that is noted for both the full and diluted strength asphalt release agent replicates, and the dilution ratio used. Also report the percent loss or gain, W, of each replicate Repeat all steps in Sections and for the other asphalt grade not selected for the first round of testing Mixture Slide Test to evaluate the susceptibility of a hot mix asphalt (HMA) mixture adhering to the beds of haul trucks or paving equipment when using asphalt release agents Apparatus Oven capable of attaining a temperature of 302 ºF (150 ºC) or more A 0.1 ft. 3 ( cm 3 ) unit weight bucket filled with sand to a weight of 10 lbs. (4.5 kg) One 16 gage steel or aluminum plate, 12 x 12 in. (305 x 305 mm) to 18 x 18 in. (457 x 457 mm), with a textured surface that simulates the inside of an average truck bed used for hauling hot mix asphalt (HMA) mixtures Balance, readable to 0.1 g and accurate to 0.5 g Waxed paper Spray bottle used to apply the release agent. A pressure sprayer with a variable nozzle may be required for asphalt release agents that are too viscous to be sprayed from the spray bottle Materials Use the following materials: Either a plant- or a laboratory-mixed sample of hot mix asphalt (HMA) meeting the following requirements: Procedure Table 3 requirements for 1/2 in. (12.5 mm) nominal aggregate size as detailed in AASHTO M 323, Superpave Volumetric Mix Design. Contains an asphalt equivalent to a PG (warmer climates) and a PG (colder climates) as defined in AASHTO M 320, Performance-Graded Asphalt Binder. Two mixes, each containing one of the above asphalt grades, will be produced and used for testing. The percent absorption of the coarse aggregates in the HMA shall be less than 0.5% when computed according to AASHTO T 85, Specific Gravity of and Absorption of Coarse Aggregate Obtain a representative sample of hot mix asphalt (HMA) mixture. Heat a minimum of 3.53 lbs. (1600 g) of mixture to 290 ºF (143 ºC) for 45 to 60 minutes Place a 0.1 ft. 3 ( cm 3 ) unit weight bucket filled with sand to a weight of 10 lbs. (4.5 kg) in an oven and heat to 290 ºF (143 ºC) for 45 to 60 minutes Spray the metal plate placed in the horizontal direction with the asphalt release agent at the recommended dilution rate so that the surface is evenly coated. NTPEP ARA AASHTO

9 Allow the metal plate to stand undisturbed for 5 minutes Weigh the metal plate to the nearest 0.1 g and record Place 500 ± 10 g of the mixture on the metal plate Place a sheet of waxed paper on top of the mixture Place the sand filled bucket on top of the waxed paper and mixture Allow the mixture and the sand filled bucket to stand for 1 hour ± 5 minutes Remove the bucket from the top of the mixture Tilt the metal plate to approximately a 45 angle and tap the plate three times on the table to help loosen the mixture from the plate. Allow the mixture to fall freely to the table. Discard this mixture. Do not remove any mixture remaining on the plate. Weigh the metal plate to the nearest 0.1 g and record Repeat Steps through two additional times, without re-spraying or removing retained mixture on the metal plate Weigh the metal plate to the nearest 0.1 g and record Calculate the amount of binder that remains adhered to the plate to the nearest 0.1 g. Use the following formula: Amount of binder = Final weight of plate initial weight of plate Report Report the amount of binder in grams that remained adhered to the plate Repeat all steps in Sections and for the other asphalt grade not selected for the first round of testing Asphalt Performance Test to determine the susceptibility of hot asphalt binders adhering to plant and paving equipment, rakes, shovels, etc. when using asphalt release agents Apparatus Oven capable of attaining a temperature of 302 ºF (150 ºC) or more One 16 gage steel or aluminum plate, 12 x 12 in. (305 x 305 mm) to 18 x 18 in. (457 x 457 mm), with a textured surface that simulates the inside of an average truck bed used for hauling hot mix asphalt (HMA) mixtures Balance, readable to 0.1 g and accurate to 0.5 g Spray bottle used to apply the asphalt release agent. A pressure sprayer with a variable nozzle may be required for asphalt release agents that are too viscous to be sprayed from the spray bottle. A 1 qt. (1 L) metal container, large sample pan, scoop, spatula, etc Materials Use a PG (warmer climates) and a PG (colder climates) or equivalent asphalt binder only Procedure NTPEP ARA AASHTO

10 Pour the binder into a 1 qt. (1 L) container and place the container into a 290 ºF (143 ºC) oven for 45 ± 5 minutes Spray the metal plate with the asphalt release agent at the recommended dilution rate and provide an even coating Allow the metal plate to stand undisturbed for 5 minutes Weigh the metal plate to the nearest 0.1 g and record Remove the asphalt binder from the oven and stir for 30 ± 5 seconds Pour 20 ± 2 g of asphalt binder on the metal plate. Return the 1 qt. (0.95 L) container to the oven Allow the binder to cool to touch (normally 5 minutes). Using a small spatula, lift up one edge of the binder and attempt to remove the remainder of the binder with one continuous pull Weigh the metal plate to the nearest 0.1 g and record. Record the Pour Number Calculate the percent of binder that remains adhered to the plate to the nearest 0.1 %. Use the following formula: PlateWeight ( g) with retained Binder Initial PlateWeight ( g) % Binder 100 Poured Binder Weight ( g) Repeat Steps through until percent binder is at least 10.0% Report Report the pour number and the percent binder for each pour Repeat all steps in Sections and for the other asphalt grade not selected for the first round of testing Product Formulation ( Fingerprint ) Infrared Spectra A reference infrared spectrum shall be obtained from a representative sample in accordance with ASTM E 1252, with a resolution of at least 4 cm -1 and a range of 4000 cm -1 to 600 cm -1. This reference spectrum shall be used for future comparison to verify that no change in formulation has been made Percent Solids The percent solids shall be obtained from a representative sample in accordance with ASTM D Specific Gravity The specific gravity shall be obtained from a representative sample in accordance with ASTM D ph The ph shall be obtained from a representative sample in accordance with AASHTO T REPORTING OF TEST DATA 11.1 Test result data will be compiled and made available to all participating states and testing companies through the AASHTO/NTPEP DataMine. This report will include data only. No judgment as to a product s acceptability will be made in this report. End user participants will establish individual criteria for product acceptability. NTPEP ARA AASHTO

11 11.2 The final report issued by the technical committee will contain the test data generated by the contracted NTPEP laboratory(s) Test results will be reported to the NTPEP Manager in the web-based data base DataMine as follows: Once the data is reported to the Manager, he will forward each manufacturer s data for their review. Once the manufacturer completes the review and accepts the data, the NTPEP Manager will release the data to the public DataMine This web-based data base can be accessed through the AASHTO-NTPEP web site link at http;//data.ntpep.org Timeline for Asphalt Release Agent Evaluation and Reporting of Data The host state DOT shall conduct four cycles of Laboratory testing per calendar year. Submittal package shall be maintained on the NTPEP webpage. Deadlines for submittal of samples are as follows (actual date will be the closest normal business date): o Cycle 1 January 1 o Cycle 2 April 1 o Cycle 3 July 1 o Cycle 4 October 1 60 calendar days after Test start date completion of laboratory testing. 65 calendar days after Test start date completion of test results review and submission to the Lead State. 75 calendar days after Test start date completion of test results review and submission to the Manufacturer. Results released to Public (pending manufacturer approval) within 100 days after sample test start date. Product listing shall be valid for three (3) years after the initial submission. 12. TEST REPORT REVIEW AND TEST RESULT APPEALS Each NTPEP contract laboratory will submit the DataMine data to the lead state Coordinator and the NTPEP Manager within 20 business days after completion of all testing. Each manufacturer will receive a copy of the portion of the report dealing with their specific products. The manufacturer will review the data and may appeal the results of the testing program in accordance with the AASHTO/NTPEP appeals procedures. An appeal must be submitted within 6 months from the date of reporting by the testing facility. Re-testing of the materials will be performed by the NTPEP contract laboratory, and only on the relevant sample and parameter being questioned. No additional sample material will be received for re-testing. The contract laboratory will provide results of the re-test within 20 business days. Prior to re-test, the manufacturer making the appeal shall submit a fee to NTPEP to cover the costs of re-testing. Should the results of the re-test uphold the appeal, the fee shall be reimbursed to the submitting manufacturer. Upon agreement between the manufacturer appealing the test results and the NTPEP Manager, either the original set or re-test set of data shall be published. 13. RESUBMITTAL TESTING FREQUENCY Resubmittal of a previously tested product must be accomplished once every three (3) years. If resubmittals have not been received by the end of the third year, then the product will be removed from DataMine. The manufacturer may elect to resubmit products earlier than 3 years for full testing to fulfill member state's requirements to be maintained on their qualified products list (QPL). NTPEP ARA AASHTO

12 Note 5 - Some state DOTs require asphalt release agents to undergo resubmittal testing after a different specified time. 14. TESTING FEES Testing fees are to be paid at time of application. Fees paid by the manufacturer will not be refunded once testing begins. Note 6 - A re-test fee for challenged results shall be paid by the manufacturer. This fee is refundable if retesting upholds the challenge. Fee is to be paid only if the original test results are found to be accurate. 15. KEYWORDS Asphalt release agents; DataMine; NTPEP NTPEP ARA AASHTO