ASTM D4-86(2004)

Standard Test Method for Bitumen Content

ABSTRACT
This test method covers the determination of bitumen content in materials containing at least 25 % bitumen. The sample shall be representative, and if it contains more than 2 % of water it shall be dehydrated. The procedures for the determination of bitumen content in materials are presented in details.
SCOPE
1.1 This test method covers the determination of bitumen content in materials containing at least 25 % bitumen. Bitumen content may usually be expeditiously and accurately determined by Procedure No. 1, Section 7. However, some bituminous materials containing finely divided mineral matter may clog the filter or the mineral residue may not be easily retained, in which cases Procedure No. 2, Section 8, shall be followed.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability and regulatory limitations prior to use. For specific precautionary information, see Section 4.

General Information

• Status: Historical
• Publication Date: 30-Jun-2004
• ICS: 91.100.50 - Binders. Sealing materials
• Technical Committee: D08 - Roofing and Waterproofing
• Drafting Committee: D08.03 - Surfacing and Bituminous Materials for Membrane Waterproofing and Built-up Roofing

Relations

• Replaces: ASTM D4-86(1998) - Standard Test Method for Bitumen Content
• Effective Date: 01-Jul-2004
• Replaced By: ASTM D4-86(2010) - Standard Test Method for Bitumen Content
• Effective Date: 01-May-2010
• Referred By: ASTM C990-09(2019) - Standard Specification for Joints for Concrete Pipe, Manholes, and Precast Box Sections Using Preformed Flexible Joint Sealants
• Effective Date: 01-Jul-2004
• Referred By: ASTM C990M-09(2019) - Standard Specification for Joints for Concrete Pipe, Manholes, and Precast Box Sections Using Preformed Flexible Joint Sealants (Metric) (Withdrawn 2024)
• Effective Date: 01-Jul-2004
• Referred By: ASTM D450/D450M-07(2018) - Standard Specification for Coal-Tar Pitch Used in Roofing, Dampproofing, and Waterproofing
• Effective Date: 01-Jul-2004
• Referred By: ASTM D6511/D6511M-18 - Standard Test Methods for Solvent Bearing Bituminous Compounds
• Effective Date: 01-Jul-2004
• Referred By: ASTM D7553-15(2021) - Standard Test Method for Solubility of Asphalt Materials in N-Propyl Bromide
• Effective Date: 01-Jul-2004
• Referred By: ASTM D5643/D5643M-06(2018) - Standard Specification for Coal Tar Roof Cement, Asbestos Free
• Effective Date: 01-Jul-2004
• Referred By: ASTM D2042-22 - Standard Test Method for Solubility of Asphalt Materials in Trichloroethylene or Toluene
• Effective Date: 01-Jul-2004

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:D4–86(Reapproved2004)
Standard Test Method for
Bitumen Content
This standard is issued under the fixed designation D4; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense. Although this test method was withdrawn by the
Society in June 1966 at the request of Committee D04, the Committee on Standards has approved its reinstatement under the jurisdiction
of Committee D08 on the basis that Procedure No. 2 still applies to their interest. Procedure No. 1 has been replaced by Method D 2042,
Test for Solubility of Asphalt Materials in Trichloroethylene.
4 5
1. Scope 3.2 Celite Analytical Filter Aid (CAFA), dried to constant
mass at 105°C and stored in a tightly stoppered container.
1.1 This test method covers the determination of bitumen
3.3 Beakers—One 30-mLbeaker, Griffin low-form, and one
content in materials containing at least 25 % bitumen. Bitumen
150-mL beaker, Griffin low-form.
content may usually be expeditiously and accurately deter-
3.4 Carbon Disulfide, cp.
mined by Procedure No. 1, Section 7. However, some bitumi-
nous materials containing finely divided mineral matter may
NOTE 1—For filled asphaltic materials, trichloroethylene may be di-
clogthefilterorthemineralresiduemaynotbeeasilyretained, rectly substituted for carbon disulfide if desired. However, carbon disul-
fide shall be used in referee testing.
in which cases Procedure No. 2, Section 8, shall be followed.
1.2 This standard does not purport to address all of the
3.5 Filtering Flask, with crucible adapter.
safety concerns, if any, associated with its use. It is the
3.6 Drying Oven.
responsibility of the user of this standard to establish appro-
3.7 Bunsen Burner or Muffle Furnace.
priate safety and health practices and determine the applica-
3.8 Suction Pump.
bility and regulatory limitations prior to use. For specific
3.9 Analytical Balance.
precautionary information, see Section 4.
3.10 Desiccator.
3.11 Evaporating Dish.
2. Referenced Documents
3.12 Watch Glasses.
2.1 ASTM Standards:
D370 Practice for Dehydration of Oil-Type Preservatives 4. Safety Precautions
E177 Practice for Use of the Terms Precision and Bias in
4.1 Carbondisulfideisextremelyflammable.Thevaporwill
ASTM Test Methods
oftenignitespontaneouslyoncontactwithahotsurfacesuchas
a hot plate, oven, or radiator. When using this solvent, be sure
3. Apparatus, Reagents, and Materials
that the filtration is conducted under a hood and well away
3.1 Filtering Crucible, porcelain, high-form, 25 to 40-mL
fromflameorothersourcesofheat.Beforeplacingcruciblesor
capacity, with fine-porosity bottom, 7-µm maximum porosity.
other containers in the oven, all traces of carbon disulfide
should be removed (as indicated by the disappearance of all
1 odor). Otherwise, the vapors will ignite. Carbon disulfide is
This test method is under the jurisdiction ofASTM Committee D08 on Roofing
also very irritating to the skin and direct contact should be
and Waterproofing and is the direct responsibility of Subcommittee D08.03 on
Surfacing and Bituminous Materials for Membrane Waterproofing and Built-up
avoided.
Roofing.
Current edition approved July 1, 2004. Published July 2004. Originally approved
5. Preparation of Sample
in 1911. Last previous edition approved in 1998 as D4 – 86 (1998). DOI: 10.1520/
D0004-86R04. 5.1 The sample shall be representative, and if it contains
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
more than 2 % of water it shall be dehydrated in accordance
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
with Test Method D370. If the material is hard and brittle, it
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Selas grade 01, size FC 30 or FC 40, or equivalent. Available from various
laboratory supply houses such as Fisher Scientific. An alternative is Royal Berlin Trademark of Manville Corp.
2A2 (size equivalent to FC 40) from Fish Schurman Corp., 70 Portman Road, New Use Celite 211 Analytical Filter Aid from Fisher Scientific, Pittsburgh, PA, or
Rochelle, NY 10802. Celite 505 from Manville Corp., Denver, CO.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4–86 (2004)
accordancewiththeproceduredescribedinthe1937ReportofCommittee
may be ground and dried at a temperature below the tempera-
D04 on Road and Paving Materials.
ture of volatilization of the material.
7.6 If there is any question involving the amount of mineral
6. Crucible Preparation
matterthatmayhavepassedthroughthefilter,acorrectionmay
be determined as described in 8.5.
6.1 If the crucible, after thorough cleaning (see 6.2), has
been used for less than six determinations, clean it as follows:
8. Procedure No. 2
Remove the CAFA mat completely, wash the crucible with
distilled water, dry, and ignite in a muffle furnace for1hat
8.1 Weigh approximately2gofthe sample into a tared
about 800°C. Cool the crucible slowly by placing it in a drying
50-mL beaker. Add to the beaker about 0.5 g, weighed to the
ovenfor1hafterremovalfromthefurnacetopreventcracking
nearest 0.001 g, of freshly dried CAFA. Cover with about 25
and place it in a desiccator while still warm.
mLof carbon disulfide and stir the filter aid into the liquid. Let
6.2 After the crucible has been used for six determinations,
stand, covered with a watch glass, at least 1 h, stirring
remove any residual ash from pores in the filtering area by
occasionally in order to dissolve the sample completely.
boiling in 1 + 1 hydrochloric acid. Then boil the crucible in
8.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,
distilled water, thoroughly back wash with distilled water, dry,
filtering crucible. Distribute the Celite evenly over the bottom.
and ignite as in 6.1.
ImmediatelyweighandrecordthemassofcrucibleplusCelite.
8.3 Immediately before starting the filtering process, stir the
7. Procedure No. 1
filter aid into the liquid.Wet the CAFAmat in the crucible with
carbon disulfide. Pour the solution from the beaker onto the
7.1 Weigh approximately2gofthe sample (size sample to
pad, filling the crucible to the top. Apply light suction and, as
obtain 0.1 to 0.3 g of insoluble matter) into a tared 150-mL
the liquid filters through, pour the remaining contents of the
beaker and add 100 mL of carbon disulfide to the beaker in
50-mL beaker into the crucible. Wash the beaker with a small
small portions, with continuous agitation, until all lumps
amount of carbon disulfide and transfer all sediment from the
disappear and nothing adheres to the beaker. Cover the beaker
beaker to the mat. Do not allow the CAFAmat to dry out until
with a watch glass and set it aside for 15 min.
filtration is complete. Wash with carbon disulfide until the
7.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,
filtrate is substantially colorless, then apply strong suction
...