ASTM D7403-19

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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: D7403 − 09 (Reapproved 2017) D7403 − 19
Standard Test Method for
Determination of Residue of Emulsified Asphalt by Low-
Temperature Low Temperature Vacuum Distillation
This standard is issued under the fixed designation D7403; 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 method covers the quantitative determination of residue in emulsified asphalts composed principally of a semisolid or
liquid asphaltic base, water, and an emulsifying agent. The emulsified asphalts will generally contain polymeric materials. It is
especially suitable for emulsified asphalt residue properties that may be altered at the high-temperature 260 °C (500 °F) distillation.
Since there is currently not a precision statement for this procedure, it is recommended to the user that this procedure not be used
for buy/sell purposes at the present time.
1.2 Units—The values stated in SI units are to be regarded as the standard. Values standard. The values given in parentheses
in inch-poundafter SI units are provided for informational purposes only.information only and are not considered standard.
1.3 The text of this standard reference notes and footnotes which provide explanatory material. These notes and footnotes
(excluding those in tables and figures) shall not be considered as requirements of the standard.
1.4 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 of
regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D3666 Specification for Minimum Requirements for Agencies Testing and Inspecting Road and Paving Materials
D6997 Test Method for Distillation of Emulsified Asphalt
E1 Specification for ASTM Liquid-in-Glass Thermometers
3. Significance and Use
3.1 This test method can be used for quantitative determination of residue in emulsified asphalts at a temperature of 135 °C
(275 °F) with a 60-min distillation test using current distillation apparatus. This method is suitable to obtain residues for service
evaluation, quality control, and research. This distillation method is not intended to produce residues equivalent to the Test Method
D6997 260 °C (500 °F) distillation procedure.
NOTE 1—The quality of the results produced by this standard are dependent on the competence of the personnel performing the procedure and the
capability, calibration, and maintenance of the equipment used. Agencies that meet the criteria of Specification D3666 are generally considered capable
of competent and objective testing, sampling, inspection, etc. Users of this standard are cautioned that compliance with Specification D3666 alone does
not completely ensure reliable results. Reliable results depend on many factors; following the suggestions of Specification D3666 or some similar
acceptable guideline provides a means of evaluating and controlling some of those factors.
This test method is under the jurisdiction of ASTM Committee D04 on Road and Paving Materials and is the direct responsibility of Subcommittee D04.42 on Emulsified
Asphalt Test.
Current edition approved Oct. 1, 2017July 15, 2019. Published October 2017August 2019. Originally approved in 2009. Last previous edition approved in 20092017 as
D7403 – 09.D7403 – 09 (2017). DOI: 10.1520/D7403-09R17.10.1520/D7403-19.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7403 − 19
4. Apparatus
PROCEDURE A
4.1 Aluminum Alloy Still, conforming to Test Method D6997 except that a 13-mm ( ⁄2-in.) diameter hole is drilled between the
two existing 13-mm ( ⁄2-in.) thermometer holes for the connection of a vacuum gauge (see Fig. 1). The joint between the still and
lid shall be airtight with the gasket in place. Other heating devices may be used, provided they employ the intended control of
temperature during the distillation procedure.
4.2 Connection Apparatus, Test Method D6997, with modifications as shown in Fig. 2. Connection tubing may be of suitable
materials provided the intended vacuum, temperature, and method are maintained. Other forms of condensers may be used,
provided they have an equivalent or greater interior surface area for condensation of distillate.
NOTE 2—Silicone rubber stoppers are recommended.
NOTE 1—Silicone rubber stoppers are recommended.
4.3 Thermometric Device, Thermometer—One of the following: (1) ASTM 7C (7F) thermometers,thermometer, or thermo-
couple(2 devices) thermocouple(s) calibrated at 135 °C (275 °F). The thermocouple probe, Type T with exposed junction, should
be of sufficient length (approximately 300 mm (12 in.)) to be positioned approximately 6 mm (0.25 in.) off the bottom of the
assembled still. Use of equivalent thermometric devices is permitted.
4.4 Balance, capable of weighing 3500 g to 60.1 g.
4.5 Vacuum Pump, rotary vane type, capable of maintaining a vacuum of 88 kPa below gauge pressure or greater.
NOTE 3—88 kPa below gauge pressure is equal to 26 in. Hg (660 mm) below atmospheric pressure.
4.6 Gasket, of silicone rubber, 3 mm ( ⁄8 in.) thick, cut to fit flanged opening on still. Other gasket materials may be used,
provided they withstand the maximum temperature reached during distillation and are able to maintain the specified vacuum within
the still.
4.7 Vacuum Gauges, dial type or other suitable type connected to vacuum tubing and/or fittings tubing, fittings, or both, to allow
attachment to both vacuum pump and to still apparatus and capable of reading a minimum vacuum of 88 kPa below gauge pressure
(660 mm or 26 in. Hg below atmospheric pressure).
4.8 Freezer, maintained at approximately –10 °C.–10 °C (14 °F).
4.9 Disposable Plastic Drink Cups, of convenient size and make to serve as a container during freezing of emulsified asphalt.
4.10 Oven, maintained at 150 6 5 °C (302 6 9 °F).
PROCEDURE B
4.11 Rotary Evaporator, with an oil bath capable of maintaining a temperature of at least 165 °C (329 °F), maintaining a vacuum
as stipulated in 4.5 and being able to rotate the distillation flask at 25 6 5 rpm.
FIG. 1 Aluminum Alloy Still Lid Showing Location of the Hole for Vacuum Gauge Connection
D7403 − 19
FIG. 2 Connection Apparatus Schematic
NOTE 4—The recommended flask for this test is a 2-L Morton flask, also referred to as a modified German rolling flask; see Fig. 3. The 2-L Morton
flask is recommended because there is a fair amount of foaming when the emulsified asphalt is above 100 °C and under vacuum. As can be seen in Fig.
3, the Morton flask has indentations arranged at 90° intervals around the flask perimeter. These indentations facilitate agitation of the emulsified asphalt
during the vacuum distillation procedure. A standard pear-shaped rotary evaporator flask would not provide the same level of agitation and is therefore
not recommended. The bath must be of sufficient volume and depth such that the Morton flask can be submerged in the bath liquid so that the full volume
of emulsified asphalt when fluid is below the surface of the bath oil when the flask is not being rotated. A food-grade mineral oil with a nominal viscosity
of 350 cs at 60 °C (140 °F) has been found acceptable as a bath fluid. The rotary evaporator bath manufacturer for the specific conditions of this test may
recommend other bath fluids. The rotary evaporator condenser can be cooled by tap water or by using a closed-system circulating chiller to ensure
condensation of water vapor from the vacuum distillation procedure.
FIG. 3 Two-Liter Morton Flask on Cork Ring
It is known that the OA-SYS bath available from Organomation Associates, Inc. (Fig. 5) will accommodate the 2-L Morton flask, although any bath capable of
submerging the flask as described and maintaining the temperature as required is acceptable.
D7403 − 19
FIG. 4 Emulsified Asphalt Sample in Rotary Evaporator
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