ASTM D6703-13
(Test Method)Standard Test Method for Automated Heithaus Titrimetry
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.
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Designation: D6703 − 13
StandardTest 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 3.1.3 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
colloidalstabilityofasphaltsandasphaltcrossblendsandaged
3.1.4 asphaltene, n—insoluble fractions of asphalt that are
asphalts. precipitated by use of selected solvents, such as n-heptane.
1.2 Units—The values stated in SI units are to be regarded
3.1.5 asphalt state of peptization, n—a measure of the
as standard. No other units of measurement are included in this
ability of the combination of a maltene solvent and dispersed
standard.
asphaltenes to form a stable dispersed system.
1.3 This standard does not purport to address all of the
3.1.6 colloidal suspension, n—an intimate mixture of two
safety concerns, if any, associated with its use. It is the
substances, one of which, called the dispersed phase (or
responsibility of the user of this standard to establish appro-
colloid), is uniformly distributed in a finely divided state
priate safety and health practices and determine the applica-
throughthesecondsubstance,calledthedispersionmedium(or
bility of regulatory limitations prior to use.
dispersing medium).
3.1.7 compatibility, n—the state of peptization of an asphalt,
2. Referenced Documents
which is measured quantitatively by the Heithaus parameter P.
2
2.1 ASTM Standards:
3.1.8 dispersed phase, n—one phase of a dispersion consist-
D3279 Test Method forn-Heptane Insolubles
ingofparticlesordropletsofonesubstancedistributedthrough
D4124 Test Method for Separation of Asphalt into Four
a second phase.
Fractions
D5546 Test Method for Solubility of Asphalt Binders in 3.1.9 dispersing medium, n—one phase of a dispersion that
distributes particles or droplets of another substance, the
Toluene by Centrifuge
E169 PracticesforGeneralTechniquesofUltraviolet-Visible disperse phase.
Quantitative Analysis
3.1.10 flocculation, n—the process of aggregation and co-
alescence into a flocculent mass.
3. Terminology
3.1.11 Heithaus compatibility parameters, n—three param-
3.1 Definitions of Terms Specific to This Standard:
eters: asphaltene peptizability (p ), maltene peptizing power
a
3.1.1 asphalt binder, n—asphalt which may or may not
(p ), and asphalt state of peptization (P), measured using
o
contain an asphalt modifier (see asphalt modifier).
Heithaus titration methods.
3.1.1.1 Discussion—This term is often used in the Perfor-
3.1.12 maltene, n—soluble fractions of asphalt that are
mance Graded Binder system.
recovered from an eluate by use of selected solvents, such as
3.1.2 asphalt cross-blend, n—any mixture of two or more
n-heptane.
asphalts blended together to form a consistent material.
3.1.13 maltene peptizing power, n—the ability of a maltene
solvent to disperse asphaltenes, measured by the Heithaus
parameter p .
o
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. 4. Summary of Test Method
Current edition approved Dec. 1, 2013. Published February 2014. Originally
4.1 Three 40 mL reaction vials are tared. Three samples of
approved in 2001. Last previous edition approved in 2007 as D6703 – 07. DOI:
10.1520/D6703-13.
asphalt of weights 0.400 g, 0.600 g and 0.800 g are transferred
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
to each of three reaction vials. Toluene (3.000 mL) is added to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
each reaction vial to dissolve the asphalt constituting three
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. solutions which differ by concentration. Each solution is
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6703 − 13
titrated with isooctane (2,2,4-trimethyl pentane) to promote referred to as the dilution concentration and FR referred to as
onset of flocculation of the solution. theflocculationratioarecalculatedas C= W /(V + V )and FR
a S T
= V /(V + V ). Values of C plotted along an x-axis versus FR
S S T
4.2 Titrations are performed by placing reactio
...
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 − 07 D6703 − 13
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 (1,2)that estimatequantify
the colloidal stability of asphalts and asphalt cross blends (1,2), aged asphalts (3),and pyrolyzed heavy oil residua and asphalt aged
asphalts.(4) using automated Heithaus titrimetry as a stability diagnostic tool.
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:
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,5), n—a dark brown to black cementitious material, solid or semisolid in consistency, in which the
predominating constituents are bitumen, which occur in nature as such or are obtained as residue by the refiningasphalt which may
or may not contain an asphalt modifier (see of petroleum.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, 2007Dec. 1, 2013. Published January 2008February 2014. Originally approved in 2001. Last previous edition approved in 20012007 as
D6703 – 01.D6703 – 07. DOI: 10.1520/D6703-07.10.1520/D6703-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. 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.
3.1.3 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 asphaltenes,asphaltene, n—the high molecular weight hydrocarbon fraction precipitated from asphalt by a designated
paraffinic naphtha solvent at a specified solvent-asphalt ratio.insoluble fractions of asphalt that are precipitated by use of selected
solvents, such as n-heptane.
3.1.4.1 Discussion—
The asphaltene fraction should be identified by the solvent and solvent-asphalt ratio used.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6703 − 13
3.1.5 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. Equivalent to compatibility of the system.
3.1.6 bitumen, n—a class of black or dark-colored (solid, semisolid, or viscous) cementitious substances, natural or
manufactured, composed principally of high-molecular weight hydrocarbons, of which asphalts, tars, pitches, and asphaltites are
typical.
3.1.7 coke, n—the solid product resulting from the destructive distillation of coal, petroleum residuum, or bitumen in an oven
or closed chamber, or from imperfect combustion of these materials, consisting principally of carbon.
3.1.6 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).
3.1.7 compatibility, n—the state of peptization of an asphalt, which is measured quantitative
...
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