ASTM D6703-14

Standard Test Method for Automated Heithaus Titrimetry

SIGNIFICANCE AND USE
5.1 This test method is intended primarily as a laboratory diagnostic tool for estimating the colloidal stability of bitumen asphalt, asphalt cross blends, aged asphalt, and heavy oil residuum. Historically, bituminous asphalt and heavy oil residua have been modeled as colloidal suspensions in which a polar associated asphaltene moiety (the dispersed phase) is suspended in a maltene solvent moiety (the dispersing medium) (refer to Test Methods D3279, D4124, and D5546 for further definition of asphalt fraction materials). The extent to which these two moieties remain in state of peptization is a measure of the compatibility (colloidal stability) of the suspension. Compatibility influences the physical properties of these materials, including rheological properties, for example, phase angle and viscosity. This test method and other similar test methods, along with the classical Heithaus test, measures the overall compatibility of a colloidal system by determining a parameter referred to as the state of peptization, P. The value of P commonly varies between 2.5 to 10 for unmodified or neat asphalts. Materials calculated to have low values of P are designated incompatible. Materials calculated to have high P values are designated compatible. Values in P are calculated as a function of two parameters that relate to the peptizability of the asphaltene moiety (the asphaltene peptizability parameter, pa) and the solvent power of the maltene moiety (the maltene peptizing power parameter, po). Values of pa and po are calculated as functions of the quantities Cmin and FRmax. Values of Cmin and FRmax are determined from experimental variables, the weight of asphalt (Wa), the volume of solvent (VS) to dissolve the weight of asphalt, and the volume of titrant (VT) added to initiate flocculation.
SCOPE
1.1 This test method describes a procedure for quantifying three Heithaus compatibility parameters that quantify the colloidal stability of asphalts and asphalt cross blends and aged asphalts.  
1.2 Units—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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-May-2014
• ICS: 17.060 - Measurement of volume, mass, density, viscosity
• Technical Committee: D04 - Road and Paving Materials
• Drafting Committee: D04.47 - Miscellaneous Asphalt Tests

Relations

• Replaces: ASTM D6703-13 - Standard Test Method for Automated Heithaus Titrimetry
• Effective Date: 01-Jun-2014
• Replaced By: ASTM D6703-19 - Standard Test Method for Automated Heithaus Titrimetry
• Effective Date: 15-Dec-2019

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:D6703 −14
Standard Test Method for
1
Automated Heithaus Titrimetry
This standard is issued under the fixed designation D6703; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 asphaltene peptizability, n—the tendency of as-
phaltenes to exist as a stable dispersion in a maltene solvent,
1.1 This test method describes a procedure for quantifying
measured by the Heithaus parameter p .
a
three Heithaus compatibility parameters that quantify the
3.1.2 asphalt state of peptization, n—a measure of the
colloidalstabilityofasphaltsandasphaltcrossblendsandaged
ability of the combination of a maltene solvent and dispersed
asphalts.
asphaltenes to form a stable dispersed system.
1.2 Units—The values stated in SI units are to be regarded
3.1.3 colloidal suspension, n—an intimate mixture of two
as standard. No other units of measurement are included in this
substances, one of which, called the dispersed phase (or
standard.
colloid), is uniformly distributed in a finely divided state
1.3 This standard does not purport to address all of the
throughthesecondsubstance,calledthedispersionmedium(or
safety concerns, if any, associated with its use. It is the
dispersing medium).
responsibility of the user of this standard to establish appro-
3.1.4 compatibility, n—the state of peptization of an asphalt,
priate safety and health practices and determine the applica-
which is measured quantitatively by the Heithaus parameter P.
bility of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
3.1.5 dispersed phase, n—one phase of a dispersion consist-
dance with internationally recognized principles on standard-
ingofparticlesordropletsofonesubstancedistributedthrough
ization established in the Decision on Principles for the
a second phase.
Development of International Standards, Guides and Recom-
3.1.6 dispersing medium, n—one phase of a dispersion that
mendations issued by the World Trade Organization Technical
distributes particles or droplets of another substance, the
Barriers to Trade (TBT) Committee.
disperse phase.
3.1.7 flocculation, n—theprocessofaggregationandcoales-
2. Referenced Documents
2 cence into a flocculent mass.
2.1 ASTM Standards:
3.1.8 Heithaus compatibility parameters, n—three param-
D8 Terminology Relating to Materials for Roads and Pave-
eters: asphaltene peptizability (p ), maltene peptizing power
ments
a
(p ), and asphalt state of peptization (P), measured using
D3279 Test Method forn-Heptane Insolubles o
Heithaus titration methods.
D4124 Test Method for Separation of Asphalt into Four
Fractions
3.1.9 maltene peptizing power, n—the ability of a maltene
D5546 Test Method for Solubility of Asphalt Binders in
solvent to disperse asphaltenes, measured by the Heithaus
Toluene by Centrifuge
parameter p .
o
E169 PracticesforGeneralTechniquesofUltraviolet-Visible
4. Summary of Test Method
Quantitative Analysis
4.1 Three 40 mL reaction vials are tared (Fig. 1). Three
3. Terminology
samples of asphalt of weights 0.400 g, 0.600 g and 0.800 g are
3.1 Definitions of Terms Specific to This Standard: transferred to each of three reaction vials. Toluene (3.000 mL)
is added to each reaction vial to dissolve the asphalt constitut-
ingthreesolutionswhichdifferbyconcentration.Eachsolution
1
This test method is under the jurisdiction of ASTM Committee D04 on Road
is titrated with isooctane (2,2,4-trimethyl pentane) to promote
and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
Miscellaneous Asphalt Tests.
onset of flocculation of the solution.
CurrenteditionapprovedJune1,2014.PublishedJuly2014.Originallyapproved
4.2 Titrations are performed by placing reaction vials sepa-
in 2001. Last previous edition approved in 2013 as D6703 – 13. DOI: 10.1520/
D6703-14.
rately in the apparatus illustrated in Fig. 2. Each reaction vial
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is separately placed into a 250 mL water-jacketed reaction
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
vessel. A sample circulation loop is made by pumping the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. solution through a short path length quartz flow cell housed in
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6703−14
FIG. 1Reaction Vial (40 mL) with TFE-fluorocarbon Cover and Temperature Probe
an ultraviolet-visible spectrophotomet
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6703 − 13 D6703 − 14
Standard Test Method for
1
Automated Heithaus Titrimetry
This standard is issued under the fixed designation D6703; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method describes a procedure for quantifying three Heithaus compatibility parameters that quantify the colloidal
stability of asphalts and asphalt cross blends and aged asphalts.
1.2 Units—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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D8 Terminology Relating to Materials for Roads and Pavements
D3279 Test Method forn-Heptane Insolubles
D4124 Test Method for Separation of Asphalt into Four Fractions
D5546 Test Method for Solubility of Asphalt Binders in Toluene by Centrifuge
E169 Practices for General Techniques of Ultraviolet-Visible Quantitative Analysis
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 asphalt binder, n—asphalt which may or may not contain an asphalt modifier (see asphalt modifier).
1
This test method is under the jurisdiction of ASTM Committee D04 on Road and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
Miscellaneous Asphalt Tests.
Current edition approved Dec. 1, 2013June 1, 2014. Published February 2014July 2014. Originally approved in 2001. Last previous edition approved in 20072013 as
D6703 – 07.D6703 – 13. DOI: 10.1520/D6703-13.10.1520/D6703-14.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3.1.1.1 Discussion—
This term is often used in the Performance Graded Binder system.
3.1.2 asphalt cross-blend, n—any mixture of two or more asphalts blended together to form a consistent material.
3.1.1 asphaltene peptizability, n—the tendency of asphaltenes to exist as a stable dispersion in a maltene solvent, measured by
the Heithaus parameter p .
a
3.1.4 asphaltene, n—insoluble fractions of asphalt that are precipitated by use of selected solvents, such as n-heptane.
3.1.2 asphalt state of peptization, n—a measure of the ability of the combination of a maltene solvent and dispersed asphaltenes
to form a stable dispersed system.
3.1.3 colloidal suspension, n—an intimate mixture of two substances, one of which, called the dispersed phase (or colloid), is
uniformly distributed in a finely divided state through the second substance, called the dispersion medium (or dispersing medium).
3.1.4 compatibility, n—the state of peptization of an asphalt, which is measured quantitatively by the Heithaus parameter P.
3.1.5 dispersed phase, n—one phase of a dispersion consisting of particles or droplets of one substance distributed through a
second phase.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6703 − 14
3.1.6 dispersing medium, n—one phase of a dispersion that distributes particles or droplets of another substance, the disperse
phase.
3.1.7 flocculation, n—the process of aggregation and coalescence into a flocculent mass.
3.1.8 Heithaus compatibility parameters, n—three parameters: asphaltene peptizability (p ), maltene peptizing power (p ), and
a o
asphalt state of peptization (P), measured using Heithaus titration methods.
3.1.12 maltene, n—soluble fractions of asphalt that are recovered from an eluate by use of selected solvents, such as n-heptane.
3.1.9 maltene peptizing power, n—the ability of a maltene solvent to disperse asphaltenes, measured by the Heithaus parameter
p .
o
4. Summary of Test Method
4.1 Three 40 mL reaction vials are tared. tared (Fig. 1). Three samples of asphalt of weights 0.400 g, 0.600 g and 0.800 g are
transferred to each of three reaction vials. Toluene (3.000 mL) is added to each reaction vial to d
...