ASTM D4-86(2018)

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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability and regulatory limitations prior to use. For specific precautionary information, see Section 4.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Apr-2018
• 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(2010) - Standard Test Method for Bitumen Content
• Effective Date: 01-May-2018
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E177-04e1 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-06 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-90a(2002) - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 10-Jan-2002
• 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-May-2018
• Referred By: ASTM D6511/D6511M-18 - Standard Test Methods for Solvent Bearing Bituminous Compounds
• Effective Date: 01-May-2018
• Referred By: ASTM D5643/D5643M-06(2018) - Standard Specification for Coal Tar Roof Cement, Asbestos Free
• Effective Date: 01-May-2018
• Referred By: ASTM D450/D450M-07(2018) - Standard Specification for Coal-Tar Pitch Used in Roofing, Dampproofing, and Waterproofing
• Effective Date: 01-May-2018

Overview

ASTM D4-86(2018) is the internationally recognized standard test method for determining the bitumen content in materials containing at least 25% bitumen. Developed by ASTM International, this standard provides procedures for quantifying bitumen in various substances, particularly those used in roofing, paving, and waterproofing applications. The method ensures reliability and accuracy, utilizing precise laboratory practices and robust safety guidance.

Key Topics

• Scope of Application: ASTM D4-86(2018) applies to materials with bitumen content of 25% or greater. It is particularly relevant for industry sectors requiring precise composition analysis of bituminous materials.
• Procedures: Two main procedures are described:
  • Procedure No. 1 is generally used for most sample types, allowing for efficient determination of bitumen content.
  • Procedure No. 2 is intended for samples with finely divided mineral matter, as these may clog filters or carry mineral residues not easily retained.
• Sample Preparation: Ensures samples are representative. If moisture exceeds 2%, samples must be dehydrated before testing.
• Safety and Environmental Considerations: The use of volatile, flammable, and irritant reagents such as carbon disulfide requires strict adherence to safety protocols, including proper ventilation and personal protective equipment.
• Measurement Units: All results and procedures are standardized in SI units, ensuring consistency across laboratories and international boundaries.
• Precision and Bias: Assessment of within-laboratory and between-laboratory variability is included, supporting quality control and reliable comparison of results.

Applications

The ASTM D4-86(2018) standard provides critical value for various practical uses:

• Quality Control in Manufacturing: Ensures bituminous materials meet specified bitumen content, which is crucial for properties such as binding, waterproofing, and durability.
• Construction Materials Testing: Used by laboratories and construction companies to assess bulk materials for roofing membranes, asphalt pavements, and waterproofing applications.
• Regulatory Compliance: Supports adherence to government and industry regulations concerning material composition in road and infrastructure projects.
• Research and Development: Facilitates laboratory research for new material formulations by offering a reliable method for quantifying bitumen.

Related Standards

For comprehensive quality assurance and materials analysis, the following ASTM standards are closely related:

• ASTM D2042: Standard Test Method for Solubility of Asphalt Materials in Trichloroethylene (now used in place of D4 Procedure No. 1 for some applications).
• ASTM D370/D370M: Practice for Dehydration of Oil-Type Preservatives, referenced for sample preparation in ASTM D4.
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods, used for interpreting and ensuring accuracy of laboratory results.

Summary

ASTM D4-86(2018) ensures accurate determination of bitumen content in high-bitumen materials, underpinning quality and durability in construction and paving industries. Adhering to this standard allows manufacturers, laboratories, and contractors to achieve consistent quality, regulatory compliance, and optimal material performance. Following safety and procedural guidelines as detailed in ASTM D4-86(2018) contributes to reliable results and effective quality management across projects involving bituminous materials.

Keywords: ASTM D4-86, bitumen content, standard test method, bituminous materials, roofing, paving, construction, asphalt testing, laboratory analysis, quality control.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4 − 86 (Reapproved 2018)
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 U.S. 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.
1. Scope ASTM Test Methods
1.1 This test method covers the determination of bitumen
3. Apparatus, Reagents, and Materials
content in materials containing at least 25 % bitumen. Bitumen
3.1 Filtering Crucible, porcelain, high-form, 25- to 40-mL
content may usually be expeditiously and accurately deter-
capacity, with fine-porosity bottom, 7-µm maximum porosity.
mined by Procedure No. 1, Section 7. However, some bitumi-
nous materials containing finely divided mineral matter may
NOTE 1—Selas grade 01, size FC 30 or FC 40, or equivalent.Available
clog the filter or the mineral residue may not be easily retained,
from various laboratory supply houses.
in which cases Procedure No. 2, Section 8, shall be followed.
3.2 Celite Analytical Filter Aid (CAFA), dried to constant
1.2 The values stated in SI units are to be regarded as mass at 105°C and stored in a tightly stoppered container.
standard. No other units of measurement are included in this
NOTE 2—Use Celite 211 or Celite 505.
standard.
3.3 Beakers—One 30-mLbeaker, Griffin low-form, and one
1.3 This standard does not purport to address all of the
150-mL beaker, Griffin low-form.
safety concerns, if any, associated with its use. It is the
3.4 Carbon Disulfide, cp.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
NOTE 3—For filled asphaltic materials, trichloroethylene may be
mine the applicability and regulatory limitations prior to use. directly substituted for carbon disulfide if desired. However, carbon
disulfide shall be used in referee testing.
For specific precautionary information, see Section 4.
1.4 This international standard was developed in accor-
3.5 Filtering Flask, with crucible adapter.
dance with internationally recognized principles on standard-
3.6 Drying Oven.
ization established in the Decision on Principles for the
3.7 Bunsen Burner or Muffle Furnace.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3.8 Suction Pump.
Barriers to Trade (TBT) Committee.
3.9 Analytical Balance.
2. Referenced Documents
3.10 Desiccator.
2.1 ASTM Standards: 3.11 Evaporating Dish.
D370/D370M Practice for Dehydration of Oil-Type Preser-
3.12 Watch Glasses.
vatives
E177 Practice for Use of the Terms Precision and Bias in
4. Safety Precautions
4.1 Carbondisulfideisextremelyflammable.Thevaporwill
1 oftenignitespontaneouslyoncontactwithahotsurfacesuchas
This test method is under the jurisdiction ofASTM Committee D08 on Roofing
and Waterproofing and is the direct responsibility of Subcommittee D08.03 on
a hot plate, oven, or radiator. When using this solvent, be sure
Surfacing and Bituminous Materials for Membrane Waterproofing and Built-up
that the filtration is conducted under a hood and well away
Roofing.
fromflameorothersourcesofheat.Beforeplacingcruciblesor
Current edition approved May 1, 2018. Published June 2018. Originally
other containers in the oven, all traces of carbon disulfide
approved in 1911. Last previous edition approved in 2010 as D4 – 86 (2010). DOI:
10.1520/D0004-86R18.
should be removed (as indicated by the disappearance of all
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
odor). Otherwise, the vapors will ignite. Carbon disulfide is
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
also very irritating to the skin and direct contact should be
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. avoided.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4 − 86 (2018)
5. Preparation of Sample carbonate solution and let it digest for1hat room temperature
in a covered beaker; then dry in an oven at 105 to 110°C to
5.1 The sample shall be representative, and if it contains
constant mass (Note 4). Add the corrections described in 7.4
more than 2 % of water it shall be dehydrated in accordance
and,ifneeded,7.6tothemassofmineralmatterinthecrucible.
with Test Method D370/D370M. If the material is hard and
brittle, it may be ground and dried at a temperature below the
NOTE 4—In the event that water-soluble salts insoluble in carbon
disulfide are present, the amount of these salts may be determined in
temperature of volatilization of the material.
accordancewiththeproceduredescribedinthe1937ReportofCommittee
D04 on Road and Paving Materials.
6. Crucible Preparation
7.6 If there is any question involving the amount of mineral
6.1 If the crucible, after thorough cleaning (see 6.2), has
matterthatmayhavepassedthroughthefilter,acorrectionmay
been used for less than six determinations, clean it as follows:
be determined as described in 8.5.
Remove the CAFA mat completely, wash the crucible with
distilled water, dry, and ignite in a muffle furnace for1hat
8. Procedure No. 2
about 800°C. Cool the crucible slowly by placing it in a drying
8.1 Weigh approximately2gofthe sample into a tared
ovenfor1hafterremovalfromthefurnacetopreventcracking
50-mL beaker. Add to the beaker about 0.5 g, weighed to the
and place it in a desiccator while still warm.
nearest 0.001 g, of freshly dried CAFA. Cover with about 25
6.2 After the crucible has been used for six determinations,
mLof carbon disulfide and stir the filter aid into the liquid. Let
remove any residual ash from pores in the filtering area by
stand, covered with a watch glass, at least 1 h, stirring
boiling in 1 + 1 hydrochloric acid. Then boil the crucible in
occasionally in order to dissolve the sample completely.
distilled water, thoroughly back wash with distilled water, dry,
8.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,
and ignite as in 6.1.
filtering crucible. Distribute the Celite evenly over the bottom.
ImmediatelyweighandrecordthemassofcrucibleplusCelite.
7. Procedure No. 1
8.3 Immediately before starting the filtering process, stir the
7.1 Weigh approximately2gofthe sample (size sample to
filter aid into the liquid.Wet the CAFAmat in the crucible with
obtain 0.1 to 0.3 g of insoluble matter) into a tared 150-mL
carbon disulfide. Pour the solution from the beaker onto the
beaker and add 100 mL of carbon disulfide to the beaker in
pad, filling the crucible to the top. Apply light suction and, as
small portions, with continuous agitation, until all lumps
the liquid filters through, pour the remaining con
...