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STP 204-2

       Standard Test                              Section:    ASPHALT MIXES
     Procedures Manual                             Subject:   ASPHALT CONTENT BY CENTRIFUGE
                                                                  EXTRACTION


1.    SCOPE

       1.1.   Description of Test

              The method described is a procedure used to determine the asphalt content of asphalt-
              aggregate mixtures.

       1.2.   Application of Test

              The asphalt content of asphalt-aggregate mixtures as determined by the described test
              method is used for product acceptance, quality assurance, process quality control and
              research activities.

       1.3.   Units of Measure

              The asphalt content is expressed as a percent by dry weight of extracted aggregate
              corrected for asphalt mix moisture content and extractor error.

2.    APPARATUS AND MATERIALS

       2.1.   Equipment

              Centrifuge extractor with a bowl approximating that shown in Figure 1 of ASTM D 2172 -
              Standard Test Methods for Quantitative Extraction of Bitumen Paving Mixtures. The
              extractor will be capable of accepting between 500 g and 2000 g of asphalt mix. The
              extractor must be capable of rotating the bowl at controlled variable speeds up to 3600
              rpm.

              The apparatus should be equipped with explosion proof features and installed in a fume
              hood or an effective surface exhaust system to provide ventilation.

              Tachometer to check rpm of extractor bowl.

              Paper or felt filter rings to be placed on the rim of the bowl and beneath the bowl lid.

              Scale capable of weighing to 2500 g at a 0.1 g accuracy.

              Heating equipment such as electric stove.




 Date: 1994 09 20                                                                    Page 1 of 6
Standard Test Procedures Manual                                                STP 204-2
Section:                                               Subject:
     ASPHALT MIXES                                    ASPHALT CONTENT BY CENTRIFUGE
                                                              EXTRACTION

                  Thermometer capable of measuring temperature between 50o C and 150o C.

                  250 ml cup or beaker.

                  Torque wrench capable of producing 35 N.m of torque.

                  Hand Tools - spatula, small brush, scoop, large pan for collection of a representative
                  asphalt mix sample, pan for test sample.

                  Container for collection of asphalt laden solvent thrown from the bowl during extraction.

           2.2.   Materials

                  Solvents - suggested materials are chlorothene or trichloroethylene.

           2.3.   Sample To Be Tested

                  Obtain representative samples of the asphalt-aggregate mixture. Asphalt mix samples will
                  be collected in accordance with STP 103 - SAMPLING ASPHALT MIXES. Asphalt
                  concrete samples will be collected in accordance with STP 204-5 ASPHALT
                  CONCRETE SAMPLES OBTAINED BY CORING.

           2.4.   Data Required

                  Sample information including date, time, sample number, sampling location, sampled by,
                  tested by, contract number, control section, contractor, asphalt type, aggregate type,
                  extractor make, model and serial number.

3.         PROCEDURE

           3.1.   Equipment Preparation

                  Ensure extractor bowl, hand tools and sample containers are cleaned of all residual asphalt
                  and aggregate materials and dry before commencing the test.

                  Check extractor rpm to ensure that a maximum of 3600 rpm is being achieved.




      Page: 2 of 6                                                                       Date: 1994 09 20
Standard Test Procedures Manual                                               STP 204-2
Section:                                                Subject:
 ASPHALT MIXES                                        ASPHALT CONTENT BY CENTRIFUGE
                                                              EXTRACTION
           3.2.   Sample Preparation

                  Collect representative samples as described in section 2.3 above. Sample size will depend
                  on the extractor bowl size. Larger samples will give more accurate results. Weigh the
                  asphalt mix and record as "weight of asphalt mix".

                  A sample of asphalt mix is required to determine the moisture content of the asphalt mix.
                  Sample size and preparation are described in STP 204-1, MOISTURE CONTENT BY
                  OVEN DRYING.

           3.3.   Test Procedure

                  Turn ventilation equipment on and adjust for maximum suction from the extractor and
                  enclosure.

                  Spread the asphalt mix sample evenly in the bowl. Cover the sample with the specified
                  solvent. Rotate the bowl back and forth gently by hand to distribute solvent and asphalt
                  mix evenly in the bowl.

                  Place two filter rings on the bowl rim and secure the bowl cover plate on
                  top of the filter papers. Tighten the cover using a torque wrench up to a
                  maximum torque of 17 N*m. Ensure that for all subsequent extractions the
                  bowl cover plate is tightened with the same torque.

                  Allow the material to soak for 5 minutes before the first centrifuge is begun.

                  Begin centrifuging slowly, increasing bowl speed slowly to a maximum of 3600 rpm.
                  When the asphalt-solvent effluent stops flowing from the extractor, turn off the motor,
                  slow and stop the bowl using the braking mechanism.

                  Add approximately 250 ml of solvent to the bowl and repeat the above described
                  procedure. The procedure should be repeated until the extracted effluent has a light
                  yellow straw colour. This is usually accomplished in 4 to 6 washings.

                  After the final wash, remove the filler screw and cover plate. Remove the filters carefully,
                  clean the extracted aggregate from the filter papers and bowl and place in a clean pan.

                  The recommended drying procedure is to place the extracted aggregate in an oven at a
                  controlled temperature of 120o C and dry to a constant weight. Establish the required
                  drying time by weighing after repeated heating and cooling until the weight is constant.
                  To prevent burning of the mineral particles, do not heat the aggregate above 120o C.




Date: 1994 09 20                                                                       Page: 3 of 6
Standard Test Procedures Manual                                             STP 204-2
Section:                                                Subject:
     ASPHALT MIXES                                      ASPHALT CONTENT BY CENTRIFUGE
                                                                    EXTRACTION
                  In a field quality control setting, the extracted aggregate may be dried on a hot plate or
                  stove burner element. The method is more subject to burning of the mineral particles and
                  is a less desirable method.

                  After cooling, weigh the dried aggregate to the nearest 0.1 g. Dry aggregate may absorb
                  moisture from the air. Determine the mass of the extracted aggregate immediately upon
                  cooling to ambient temperature. Record the weight of the dry extracted aggregate to the
                  nearest 0.1 g.

4.         RESULTS AND CALCULATIONS

           4.1.   Collection of Test Results

                  The following data is required:

                  - Weight of asphalt mix before extraction to the nearest 0.1 g

                  - Weight of dried aggregate after extraction to the nearest 0.1 g

                  - Moisture content of the asphalt mix as determined by STP 204-1,
                    MOISTURE CONTENT BY OVEN DRYING

                  - Extractor correction as determined by STP 204-23, EXTRACTION AND MOISTURE
                            CORRECTIONS

           4.2.   Calculations

                  Uncorrected Asphalt Content = (wt. of asphalt mix - wt. of dry agg.) x 100
                  (Calculated to the nearest .01%)     wt. of dry aggregate

                  Corrected Asphalt Content = Uncorrected Asphalt Content (%) - Moisture
                                             Content (%) + Extractor Error (%)

                  NOTE: 1) The corrected asphalt content should be rounded to the nearest 0.1%.

                         2) Refer to STP 204-23 "Extraction and Moisture Corrections" to determine the
                            proper type of extractor correction to be used.




      Page: 4 of 6                                                                    Date: 1994 09 20
Standard Test Procedures Manual                                              STP 204-2
Section:                                               Subject:
 ASPHALT MIXES                                        ASPHALT CONTENT BY CENTRIFUGE
                                                              EXTRACTION

5.         CALIBRATIONS AND REPEATABILITY

           5.1.   Equipment Calibration

                  Periodical checking of extractor rpm should be conducted.

                  Each time extractor or operators are changed, a new extraction correction should be done.
                  The extractor correction test should have the same number of washings as used in the
                  actual extracted sample.

                  Extraction corrections should also be done for each asphalt mix design or approved job
                  mix formula.

           5.2.   Tolerances and Repeatability

                  Tolerances for repeatability and reproducibility are specified below:

                  Single Operator: two tests on the same sample should not vary by more than
                                   + .1%

                  Multiple Operator: two tests on the same sample shall not vary by more than
                                     + .2%

           5.3.   Sources of Error

                  Incomplete washing of the asphalt from the mix.

                  Non-consistent torques applied to the bowl cover plate.

                  Loss of mineral aggregate particles when transferring from extractor bowl and filter papers
                  to pan.

                  Not doing moisture and extraction corrections.

                  Not meeting the specified rpm requirements on the extractor.

                  Overheating the aggregate during drying.




Date: 1994 09 20                                                                      Page: 5 of 6
Standard Test Procedures Manual                                            STP 204-2
Section:                                              Subject:
     ASPHALT MIXES                                  ASPHALT CONTENT BY CENTRIFUGE
                                                            EXTRACTION
6.         ADDITIONAL INFORMATION

           6.1.   Sample Retention

                  The extracted aggregate may be retained for gradation analysis using STP 204-4, SIEVE
                  ANALYSIS.

           6.2.   Safety

                  Provide good ventilation as solvent fumes may be injurious to your health. Propane stoves
                  should not be used in laboratories where chlorothene and trichloroethylene solvents are
                  being used.




      Page: 6 of 6                                                                  Date: 1994 09 20
Standard Test Procedures Manual                                              STP 204-2
  Section:                                            Subject:
   ASPHALT MIXES                                    ASPHALT CONTENT BY CENTRIFUGE
                                                            EXTRACTION
APPROVAL SHEET

New       Revision X Date of Previous Document 92-12-10
Effective Date: 94-12-21
Description of Revision (Reason for Revision):
 Removed requirement of applying 17 N*m torgue to the extractor lid. Referred to it as a maximum torgue.
Added note to ensure that the same torque be applied for all extractions

Review/Implementation Process:
 Reviewed by the End Product Specification Committee and Technical
 Standards and Policies Branch.

Other Manuals/Policies Affected:
 Nil

Follow Up/Training Required:
 Nil

Comments/Concerns/Implications (Budget/Environment/Stakeholders):



Prepared by        D. MacLeod                       94-09-20
                                      Date

Recommended by      D. MacLeod                          94-09-20
           Materials Standards Engineer      Date


Approval Recommended by R.A. Widger                              94-12-20
             Senior Materials Engineer       Date


Approved by          A.R. Gerbrandt                 94-12-21
              Dir., Technical Standards & Policies Br. Date


                                             Electronic File Updated        95-01-31

                                             Update Mailed                             - -




 Date: 1994 09 20                                                                      Page: 7 of 6

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Bitumen extraction saskatchewan

  • 1. STP 204-2 Standard Test Section: ASPHALT MIXES Procedures Manual Subject: ASPHALT CONTENT BY CENTRIFUGE EXTRACTION 1. SCOPE 1.1. Description of Test The method described is a procedure used to determine the asphalt content of asphalt- aggregate mixtures. 1.2. Application of Test The asphalt content of asphalt-aggregate mixtures as determined by the described test method is used for product acceptance, quality assurance, process quality control and research activities. 1.3. Units of Measure The asphalt content is expressed as a percent by dry weight of extracted aggregate corrected for asphalt mix moisture content and extractor error. 2. APPARATUS AND MATERIALS 2.1. Equipment Centrifuge extractor with a bowl approximating that shown in Figure 1 of ASTM D 2172 - Standard Test Methods for Quantitative Extraction of Bitumen Paving Mixtures. The extractor will be capable of accepting between 500 g and 2000 g of asphalt mix. The extractor must be capable of rotating the bowl at controlled variable speeds up to 3600 rpm. The apparatus should be equipped with explosion proof features and installed in a fume hood or an effective surface exhaust system to provide ventilation. Tachometer to check rpm of extractor bowl. Paper or felt filter rings to be placed on the rim of the bowl and beneath the bowl lid. Scale capable of weighing to 2500 g at a 0.1 g accuracy. Heating equipment such as electric stove. Date: 1994 09 20 Page 1 of 6
  • 2. Standard Test Procedures Manual STP 204-2 Section: Subject: ASPHALT MIXES ASPHALT CONTENT BY CENTRIFUGE EXTRACTION Thermometer capable of measuring temperature between 50o C and 150o C. 250 ml cup or beaker. Torque wrench capable of producing 35 N.m of torque. Hand Tools - spatula, small brush, scoop, large pan for collection of a representative asphalt mix sample, pan for test sample. Container for collection of asphalt laden solvent thrown from the bowl during extraction. 2.2. Materials Solvents - suggested materials are chlorothene or trichloroethylene. 2.3. Sample To Be Tested Obtain representative samples of the asphalt-aggregate mixture. Asphalt mix samples will be collected in accordance with STP 103 - SAMPLING ASPHALT MIXES. Asphalt concrete samples will be collected in accordance with STP 204-5 ASPHALT CONCRETE SAMPLES OBTAINED BY CORING. 2.4. Data Required Sample information including date, time, sample number, sampling location, sampled by, tested by, contract number, control section, contractor, asphalt type, aggregate type, extractor make, model and serial number. 3. PROCEDURE 3.1. Equipment Preparation Ensure extractor bowl, hand tools and sample containers are cleaned of all residual asphalt and aggregate materials and dry before commencing the test. Check extractor rpm to ensure that a maximum of 3600 rpm is being achieved. Page: 2 of 6 Date: 1994 09 20
  • 3. Standard Test Procedures Manual STP 204-2 Section: Subject: ASPHALT MIXES ASPHALT CONTENT BY CENTRIFUGE EXTRACTION 3.2. Sample Preparation Collect representative samples as described in section 2.3 above. Sample size will depend on the extractor bowl size. Larger samples will give more accurate results. Weigh the asphalt mix and record as "weight of asphalt mix". A sample of asphalt mix is required to determine the moisture content of the asphalt mix. Sample size and preparation are described in STP 204-1, MOISTURE CONTENT BY OVEN DRYING. 3.3. Test Procedure Turn ventilation equipment on and adjust for maximum suction from the extractor and enclosure. Spread the asphalt mix sample evenly in the bowl. Cover the sample with the specified solvent. Rotate the bowl back and forth gently by hand to distribute solvent and asphalt mix evenly in the bowl. Place two filter rings on the bowl rim and secure the bowl cover plate on top of the filter papers. Tighten the cover using a torque wrench up to a maximum torque of 17 N*m. Ensure that for all subsequent extractions the bowl cover plate is tightened with the same torque. Allow the material to soak for 5 minutes before the first centrifuge is begun. Begin centrifuging slowly, increasing bowl speed slowly to a maximum of 3600 rpm. When the asphalt-solvent effluent stops flowing from the extractor, turn off the motor, slow and stop the bowl using the braking mechanism. Add approximately 250 ml of solvent to the bowl and repeat the above described procedure. The procedure should be repeated until the extracted effluent has a light yellow straw colour. This is usually accomplished in 4 to 6 washings. After the final wash, remove the filler screw and cover plate. Remove the filters carefully, clean the extracted aggregate from the filter papers and bowl and place in a clean pan. The recommended drying procedure is to place the extracted aggregate in an oven at a controlled temperature of 120o C and dry to a constant weight. Establish the required drying time by weighing after repeated heating and cooling until the weight is constant. To prevent burning of the mineral particles, do not heat the aggregate above 120o C. Date: 1994 09 20 Page: 3 of 6
  • 4. Standard Test Procedures Manual STP 204-2 Section: Subject: ASPHALT MIXES ASPHALT CONTENT BY CENTRIFUGE EXTRACTION In a field quality control setting, the extracted aggregate may be dried on a hot plate or stove burner element. The method is more subject to burning of the mineral particles and is a less desirable method. After cooling, weigh the dried aggregate to the nearest 0.1 g. Dry aggregate may absorb moisture from the air. Determine the mass of the extracted aggregate immediately upon cooling to ambient temperature. Record the weight of the dry extracted aggregate to the nearest 0.1 g. 4. RESULTS AND CALCULATIONS 4.1. Collection of Test Results The following data is required: - Weight of asphalt mix before extraction to the nearest 0.1 g - Weight of dried aggregate after extraction to the nearest 0.1 g - Moisture content of the asphalt mix as determined by STP 204-1, MOISTURE CONTENT BY OVEN DRYING - Extractor correction as determined by STP 204-23, EXTRACTION AND MOISTURE CORRECTIONS 4.2. Calculations Uncorrected Asphalt Content = (wt. of asphalt mix - wt. of dry agg.) x 100 (Calculated to the nearest .01%) wt. of dry aggregate Corrected Asphalt Content = Uncorrected Asphalt Content (%) - Moisture Content (%) + Extractor Error (%) NOTE: 1) The corrected asphalt content should be rounded to the nearest 0.1%. 2) Refer to STP 204-23 "Extraction and Moisture Corrections" to determine the proper type of extractor correction to be used. Page: 4 of 6 Date: 1994 09 20
  • 5. Standard Test Procedures Manual STP 204-2 Section: Subject: ASPHALT MIXES ASPHALT CONTENT BY CENTRIFUGE EXTRACTION 5. CALIBRATIONS AND REPEATABILITY 5.1. Equipment Calibration Periodical checking of extractor rpm should be conducted. Each time extractor or operators are changed, a new extraction correction should be done. The extractor correction test should have the same number of washings as used in the actual extracted sample. Extraction corrections should also be done for each asphalt mix design or approved job mix formula. 5.2. Tolerances and Repeatability Tolerances for repeatability and reproducibility are specified below: Single Operator: two tests on the same sample should not vary by more than + .1% Multiple Operator: two tests on the same sample shall not vary by more than + .2% 5.3. Sources of Error Incomplete washing of the asphalt from the mix. Non-consistent torques applied to the bowl cover plate. Loss of mineral aggregate particles when transferring from extractor bowl and filter papers to pan. Not doing moisture and extraction corrections. Not meeting the specified rpm requirements on the extractor. Overheating the aggregate during drying. Date: 1994 09 20 Page: 5 of 6
  • 6. Standard Test Procedures Manual STP 204-2 Section: Subject: ASPHALT MIXES ASPHALT CONTENT BY CENTRIFUGE EXTRACTION 6. ADDITIONAL INFORMATION 6.1. Sample Retention The extracted aggregate may be retained for gradation analysis using STP 204-4, SIEVE ANALYSIS. 6.2. Safety Provide good ventilation as solvent fumes may be injurious to your health. Propane stoves should not be used in laboratories where chlorothene and trichloroethylene solvents are being used. Page: 6 of 6 Date: 1994 09 20
  • 7. Standard Test Procedures Manual STP 204-2 Section: Subject: ASPHALT MIXES ASPHALT CONTENT BY CENTRIFUGE EXTRACTION APPROVAL SHEET New Revision X Date of Previous Document 92-12-10 Effective Date: 94-12-21 Description of Revision (Reason for Revision): Removed requirement of applying 17 N*m torgue to the extractor lid. Referred to it as a maximum torgue. Added note to ensure that the same torque be applied for all extractions Review/Implementation Process: Reviewed by the End Product Specification Committee and Technical Standards and Policies Branch. Other Manuals/Policies Affected: Nil Follow Up/Training Required: Nil Comments/Concerns/Implications (Budget/Environment/Stakeholders): Prepared by D. MacLeod 94-09-20 Date Recommended by D. MacLeod 94-09-20 Materials Standards Engineer Date Approval Recommended by R.A. Widger 94-12-20 Senior Materials Engineer Date Approved by A.R. Gerbrandt 94-12-21 Dir., Technical Standards & Policies Br. Date Electronic File Updated 95-01-31 Update Mailed - - Date: 1994 09 20 Page: 7 of 6