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): Standard Test Method for Bitumen Content is an international standard developed by ASTM International. This test method outlines procedures for the determination of bitumen content in materials that contain at least 25% bitumen. Widely used in industries that handle bituminous materials, such as construction, roofing, and paving, the ASTM D4 standard ensures reliable results through detailed test procedures. This document is recognized in accordance with international principles on standardization as established by the World Trade Organization (WTO) Technical Barriers to Trade (TBT) Committee.

Key Topics

• Sample Preparation: The sample must be representative. If the sample contains more than 2% water, dehydration is required in accordance with ASTM D370/D370M.
• Test Procedures: Two main procedures are specified:
  • Procedure No. 1 - For most materials where filtration is straightforward, allows for rapid and accurate bitumen content determination.
  • Procedure No. 2 - Intended for samples with finely divided mineral matter that may clog filters or are difficult to retain. This method ensures accurate results even in challenging material compositions.
• Safety Requirements: The test involves hazardous substances such as carbon disulfide, which is extremely flammable and toxic. The standard emphasizes adherence to strict safety, health, and environmental practices.
• Results Calculation: The standard provides a method for calculating bitumen content and advises reporting to the nearest 0.1%. Corrections are applied for residue and filter aid materials.
• Precision and Bias: Guidance is provided for evaluating the precision of the results within and between laboratories, enhancing the reliability of inter-laboratory comparisons.
• Use of SI Units: All measurements are specified in SI units as standard.

Applications

• Quality Control: The ASTM D4-86(2018) bitumen content test is critical for quality assurance in the manufacture of roofing, waterproofing membranes, and paving materials.
• Construction Materials Testing: Helps verify compliance of bituminous materials with product specifications, ensuring suitable material properties for roads, roofs, and related structures.
• Research and Development: Facilitates the comparison of new formulations or sources of bituminous materials for improved performance or sustainability.
• Regulatory Compliance: Used by government and industry bodies to ensure materials meet required performance and safety standards.
• Defense and Infrastructure Projects: Approved for use by U.S. Department of Defense agencies, highlighting its acceptance for critical infrastructure projects.

Related Standards

• ASTM D370/D370M: Practice for Dehydration of Oil-Type Preservatives, required for preparing wet samples.
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods, referenced for statistical analysis of test results.
• ASTM D2042: Test Method for Solubility of Asphalt Materials in Trichloroethylene, currently used in place of Procedure No. 1 for many applications.
• WTO TBT Principles: The standard aligns with the World Trade Organization's Technical Barriers to Trade principles for international standards development.

Practical Value

By following ASTM D4-86(2018), laboratories and quality control professionals can ensure the accurate and repeatable determination of bitumen content in various materials. This not only enhances the durability and performance of bituminous products but also supports regulatory compliance and international trade, making it an essential reference for those involved with asphalt, coal tar, and related bituminous mixtures.

Keywords: ASTM D4, bitumen content, bituminous materials, construction materials testing, quality control, roofing, paving, carbon disulfide, sample preparation, international standard, laboratory testing.

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
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