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: D6997 − 12 (Reapproved 2020)

Standard Test Method for

Distillation of Emulsified Asphalt1
This standard is issued under the fixed designation D6997; 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 distillate and water obtained are measured. The residue from
1.1 This test method covers the quantitative determination the distillation, and also any oil portion of the distillate, may be
of residue and oil distillate in emulsified asphalts composed tested as required.
principally of a semisolid or liquid asphaltic base, water, and 4. Significance and Use
an emulsifying agent.
4.1 This test method can be used for quantitative determi-
1.2 The values stated in SI units are to be regarded as the nation of residue and oil distillates in emulsified asphalts for
standard. No other units of measurement are included in this specification acceptance, service evaluation, control, and re-
standard. search. This test method can also be used to obtain residue and
1.3 This standard does not purport to address all of the oil distillate for further testing. This method may not be
safety concerns, if any, associated with its use. It is the appropriate for emulsified asphalts containing latex or poly-
responsibility of the user of this standard to establish appro- mer; however, some specifying agencies may utilize this
priate safety, health, and environmental practices and deter- method and stipulate a lowered distillation temperature. By
mine the applicability of regulatory limitations prior to use. stipulating a lowered distillation temperature, the precision and
1.4 This international standard was developed in accor- bias statement may not be considered valid. Low-temperature
dance with internationally recognized principles on standard- methods such as Test Method D7403 and Practice D7497 are
ization established in the Decision on Principles for the options for obtaining residue for latex or polymer modified
Development of International Standards, Guides and Recom- emulsified asphalts.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 5. Apparatus
5.1 Aluminum-Alloy Still—Approximately 241 mm in
2. Referenced Documents height by 95 mm inside diameter with cover and clamp as
2.1 ASTM Standards:2 shown in Fig. 1. The dimensions as noted in Fig. 1 are provided
D7403 Test Method for Determination of Residue of Emul- as reference for the ease of the user and are considered
sified Asphalt by Low Temperature Vacuum Distillation noncritical dimensions.
D7497 Practice for Recovering Residue from Emulsified NOTE 1—Residue by distillation results obtained with iron stills are
Asphalt Using Low Temperature Evaporative Technique acceptable.
E1 Specification for ASTM Liquid-in-Glass Thermometers 5.2 Gasket—A variety of gasket materials may be used to
E11 Specification for Woven Wire Test Sieve Cloth and Test seal the still providing they withstand the maximum tempera-
Sieves ture reached during distillation.
3. Summary of Method NOTE 2—Use of a gasket is optional if the joint can be ground to a tight
fit or only residue recovery is required and further analysis on the water
3.1 A sample of emulsified asphalt is heated in an or oil distillate is not needed.
aluminum-alloy still to 260 6 5 °C and the volumes of 5.3 Heat Sources—Having holes on the inner periphery and
having three spacers, to ensure centering of burner around the
1
still (see Fig. 2). The dimensions as noted in Fig. 2 are provided
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 for reference for the ease of the user and are considered
Emulsified Asphalt Test. noncritical dimensions.
Current edition approved Oct. 15, 2020. Published October 2020. Originally
approved in 2004. Last previous edition approved in 2012 as D6997 – 12. DOI: NOTE 3—Optional use of a bunsen burner (equipped with optional wing
10.1520/D6997-12R20. tip) as shown in Fig. 3.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
5.4 Connection Apparatus—Consisting of approximately
Standards volume information, refer to the standard’s Document Summary page on 12 mm glass or metal connecting tube, tin shield (as detailed in
the ASTM website. Fig. 3), and a water-cooled glass condenser tube with a metal

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
 D6997 − 12 (2020)
NOTE 4—For details of the assembly of apparatus for the distillation
test, see Fig. 3.

6. Sample Conditioning for Testing

6.1 All emulsified asphalts shall be properly stirred to
achieve homogeneity before testing.
6.2 All emulsified asphalts with viscosity testing require-
ments of 50 °C shall be heated to 50 6 3 °C in the original
sample container in a water bath or oven. The container should
be vented to relieve pressure. After the sample reaches 50 6
3 °C, stir the sample to achieve homogeneity.
6.3 Emulsified asphalts with viscosity testing requirements
of 25 °C shall be conditioned to 25 6 3 °C in the original
sample container to achieve homogeneity. After the sample
reaches 25 6 3 °C, stir the sample to achieve homogeneity.
NOTE 5—Emulsified asphalts with viscosity testing requirements of
25 °C may be heated and stirred as specified in 6.2, if necessary.
6.4 Emulsified asphalts presented for testing from a storage
tank may be tested at the storage tank temperature. Condition-
ing as in 6.2 and 6.3 is not required.
7. Procedure
7.1 Determine the mass of the aluminum-alloy still. Include
in this determination the still, cover, clamp, temperature
measuring device(s), small stopper (if used), and gasket (if
used).
7.2 Add 200 6 1.0 g of a representative sample of the
emulsified asphalt. Record this mass.
NOTE 6—If additional residue is needed for further testing, the sample
size may be increased. A total sample mass between 200 to 300 g will be
considered acceptable. This mass must be recorded and used in calcula-
tions 8.1 and 8.2. The precision data of this method was developed using
FIG. 1 Aluminum-Alloy Still 200 g samples and may not apply to other sample sizes.
7.3 Securely clamp the cover on the still. If a gasket is used,
insert between the still and the cover prior to clamping.
or borosilicate glass jacket. The metal connecting tube may be 7.4 Insert the temperature measuring device first through a
secured to the lid by a threaded compressing fitting. Glass cork or silicone stopper, and then in one of the small holes
connecting tube may be secured to the lid by means of a cork provided in the cover. Seal the other hole with a cork or
or silicone stopper. Other condensers of approximately 12 mm silicone stopper. Adjust the temperature measuring device so
glass or metal tubing may be used, providing that the wetted that the end of the probe or bulb is approximately 6 mm from
length is 400 to 550 mm. The dimensions as noted in Fig. 3 are the bottom of the still.
provided for reference for the ease of the user and are
considered noncritical dimensions. NOTE 7—A second temperature measuring device may be used in the
second small hole, with the probe or bulb placed approximately 165 mm
5.5 Graduated Cylinder—100 mL, with graduation intervals from the bottom of the still. A sudden change in temperature reading of
of 1.0 mL. upper temperature measuring device indicates foaming. Remove heat until
foaming ceases.
5.6 Thermometer—ASTM 7C thermometer, as prescribed in
Specification E1, or any other thermometric device of equal 7.5 Place the ring burner around the still approximately
accuracy. 150 mm from the bottom of the still. Apply heat by lighting this
burner and adjusting to low flame. Also apply just enough heat
5.7 Balance—Capable of weighing 3500 g to within 60.1 g. from bunsen burner to the connecting tube to prevent conden-
5.8 Stoppers—Cork (wrapped in foil) or silicone stoppers to sation of water in this tube.
seal holes in still cover, maintain temperature measuring device NOTE 8—Use of the bunsen burner is optional.
position, and secure connecting tube to still cover.
7.6 When the temperature reaches approximately 215 °C,
5.9 Rubber Tubing—Heat-resistant tubing of adequate size move the ring burner approximately level with the bottom of
to secure glass to glass joint of connecting tube and condenser. the still. Increase the temperature to 260 6 5 °C, maintaining
5.10 Sieve—300 µm sieve to capture foreign materials when it at this temperature for 15 min. Complete the total distillation
suspected. in 60 6 15 min from the first application of heat.

2
 D6997 − 12 (2020)

FIG. 2 Ring Burner with 125-mm Inside Diameter

FIG. 3 Apparatus Assembly for Distillation Test of Emulsified Asphalts

NOTE 9—The ring burner may be raised to decrease chance of 7.8 Stir the still contents by gently agitating the residue.
foam-over or lowered to the middle of still for emulsified asphalts This may be done using a swirling motion or stirring with a
containing no solvent. The ring burner may be gradually lowered as the
distillation proceeds to ensure that the time requirements of this test long glass or steel rod to obtain consistent material prior to
method are satisfied. It is also acceptable to incorporate two ring burners pouring. Remove the cover from the still and immediately pour
rather than moving a single ring burner. If a secondary ring burner is used, suitable portions of the residue into a container or molds
only one ring burner is to be operational at any given point during the required for residue testing. If there is foreign matter suspected
distillation.
in the residue, pour the material through a sieve prior to
7.7 Immediately at the expiration of the heating period, turn pouring into the test molds and container(s).
off the flame and again weigh the still and accessories as
described in 7.1. The aluminum-alloy still at ambient tempera- 8. Calculation
ture (7.1) weighs 1.5 g more than at 260 °C. Correct for this
error by adding 1.5 g to gross weight obtained prior to 8.1 Calculate the percentage of residue in the sample as
calculating the percentage of residue by distillation. Calculate follows:
per 8.1 and report the percentage residue by distillation. Record Sample residue, % 5 ~~ B 2 A ! /C ! 3 100 (1)
the volume of oil distillate to the nearest 0.5 mL. Calculate per
8.2 and report the oil distillate as a volume percentage of the where:
total emulsified asphalt based upon the sample weight as A = mass of empty still (7.1) assembly before test, g,
recorded in 7.2.

3
 D6997 − 12 (2020)

B = mass of still assembly (7.7) after test (with added 1.5 g), 10.1.1 Duplicate results by the same operator should not be
g, and considered suspect unless they differ by more than the follow-
C = mass of emulsified asphalt added to still, g. ing amount:
Residue by Distillation, mass % Repeatability, mass %
8.2 Calculate the % oil distillate as follows: 50 to 70 1.0
Oil Distillate, % = (Volume of oil recorded to the nearest 0.5 10.1.2 The results submitted by each of two laboratories
ml / sample weight) × 100. Record the % Oil Distillate to the should not be considered suspect unless they differ by more
nearest 0.1 % than the following amount:
Residue by Distillation, mass % Repeatability, mass %
9. Report 50 to 70 2.0

9.1 Report the percentage of residue in the sample and the 10.2 The bias of this test method cannot be determined
percentage of oil distillate. because no material having an accepted reference value is
available.
10. Precision and Bias 11. Keywords
10.1 The following criteria should be used for judging the 11.1 asphalt emulsion; cationic emulsified asphalt; distilla-
acceptability of results (95 % probability): tion; emulsified asphalt; residue

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