Density of Semi-Solid Asphalt Binder (Pycnometer Method) : Standard Test Method For

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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: D70 − 18

Standard Test Method for


Density of Semi-Solid Asphalt Binder (Pycnometer Method)1
This standard is issued under the fixed designation D70; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 1.6 This international standard was developed in accor-


1.1 This test method covers the determination of the relative dance with internationally recognized principles on standard-
density and density of semi-solid asphalt binder and soft tar ization established in the Decision on Principles for the
pitches by use of a pycnometer. Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
NOTE 1—An alternate method for determining the density of asphalt Barriers to Trade (TBT) Committee.
binder is Test Method D3289. For materials which are too fluid for use of
this test method, use Test Method D3142/D3142M. 2. Referenced Documents
1.2 The values stated in either SI units or inch-pound units 2.1 ASTM Standards:2
are to be regarded separately as standard. The values stated in C670 Practice for Preparing Precision and Bias Statements
each system may not be exact equivalents; therefore, each for Test Methods for Construction Materials
system shall be used independently of the other. Combining D140/D140M Practice for Sampling Asphalt Materials
values from the two systems may result in nonconformance D3142/D3142M Test Method for Specific Gravity, API
with the standard. Gravity, or Density of Cutback Asphalts by Hydrometer
1.3 Warning—Mercury has been designated by the United Method
States Environmental Protection Agency (EPA) and many state D3289 Test Method for Density of Semi-Solid and Solid
agencies as a hazardous material that can cause central nervous Asphalt Materials (Nickel Crucible Method)
system, kidney, and liver damage. Mercury, or its vapor, may D3666 Specification for Minimum Requirements for Agen-
be hazardous to health and corrosive to materials. Caution cies Testing and Inspecting Road and Paving Materials
should be taken when handling mercury and mercury- D4311/D4311M Practice for Determining Asphalt Volume
containing products. See the applicable product Material Correction to a Base Temperature
Safety Data Sheet (MSDS) or Safety Data Sheet (SDS) for E1 Specification for ASTM Liquid-in-Glass Thermometers
details and the EPA’s website (www.epa.gov/mercury/faq.htm) E77 Test Method for Inspection and Verification of Ther-
for additional information. Users should be aware that selling mometers
mercury, mercury-containing products, or both, in your state E563 Practice for Preparation and Use of an Ice-Point Bath
may be prohibited by state law. as a Reference Temperature
1.4 The text of this standard references notes and footnotes E644 Test Methods for Testing Industrial Resistance Ther-
which provide explanatory material. These notes and footnotes mometers
(excluding those in tables and figures) shall not be considered E879 Specification for Thermistor Sensors for General Pur-
as requirements of the standard. pose and Laboratory Temperature Measurements
E1137/E1137M Specification for Industrial Platinum Resis-
1.5 This standard does not purport to address all of the tance Thermometers
safety concerns, if any, associated with its use. It is the 2.2 Other:
responsibility of the user of this standard to establish appro- CRC Handbook of Chemistry and Physics
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 density—the mass per unit volume of a material.
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
2
Miscellaneous Asphalt Tests. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2018. Published April 2018. Originally contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
approved in 1920. Last previous edition approved in 2017 as D70 – 17. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D0070-18. the ASTM website.

*A Summary of Changes section appears at the end of this standard


Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
D70 − 18
3.1.2 relative density—the ratio of the mass of a given [0.95 to 1.18 in.] and shall weigh not more than 40 g [1.4 oz].
volume of a material to the mass of the same volume of water Suitable pycnometers are illustrated in Fig. 1.
at the same temperature (see Note 2). 6.2 Water Bath, constant-temperature, capable of maintain-
NOTE 2—Relative density is also described as specific gravity. ing the temperature within 0.1 °C [0.2 °F] of the test tempera-
ture. The water bath shall be equipped with a thermometer as
4. Summary of Test Method described in 6.3.
4.1 The sample is placed in a standardized pycnometer. The 6.3 Thermometer—The thermometer shall be one of the
pycnometer and sample are weighed, then the remaining following:
volume is filled with water. The filled pycnometer is brought to 6.3.1 A liquid-in-glass partial immersion thermometer of
the test temperature and weighed. The density of the sample is suitable range with subdivisions and maximum scale error of
calculated from its mass and the mass of water displaced by the 0.1 °C [0.2 °F] which conforms to the requirements of Speci-
sample in the filled pycnometer. fication E1. Calibrate the thermometer in accordance with one
of the methods in Test Method E77 or verify its original
5. Significance and Use
calibration at the ice point (Notes 3 and 4). A thermometer
5.1 Values of density are used for converting volumes to commonly used is an ASTM 63C.
units of mass, and for correcting measured volumes from the
temperature of measurement to a standard temperature using NOTE 3—Practice E563 provides instructions on the preparation and use
of an ice-point bath as a reference temperature.
Practice D4311/D4311M.
NOTE 4—If the thermometer does not read 0.0 6 0.1 °C [32.0 6 0.2 °F]
5.2 The quality of the results produced by this standard are at the ice point, then the thermometer should be recalibrated.
dependent on the competence of the personnel performing the 6.3.2 A platinum resistance thermometer (PRT) with sensor
procedure and the capability, calibration, and maintenance of which conforms to the requirements of Specification E1137/
the equipment used. Agencies that meet the criteria of Speci- E1137M. The thermometer shall be calibrated annually as a
fication D3666 are generally considered capable of competent single unit and have a 3- or 4-wire connection configuration.
and objective testing, sampling, inspection, etc. Users of this The sensing element shall be immersed to the depth specified
standard are cautioned that compliance with Specification by the manufacturer. Calibrate the PRT system (sensor and
D3666 alone does not completely ensure reliable results. readout) in accordance with Test Methods E644 or verify its
Reliable results depend on many factors; following the sug- original calibration at the ice point (Notes 3 and 4). Corrections
gestions of Specification D3666 or some similar acceptable shall be applied to ensure accurate measurements within 0.1 °C
guideline provides a means of evaluation and controlling some [0.2 °F].
of these factors. 6.3.3 A thermistor thermometer with sensor which con-
forms to the requirements of Specification E879, calibrated
6. Apparatus
annually as a single unit. The sensing element of the thermistor
6.1 Pycnometer, glass, consisting of a cylindrical or conical shall be completely immersed. Calibrate the thermistor ther-
vessel carefully ground to receive an accurately fitting glass mometer system (sensor and readout) in accordance with Test
stopper 22 to 26 mm [0.9 to 1.0 in.] in diameter. The stopper Methods E644 or verify its original calibration at the ice point
shall be provided with a hole 1.0 to 2.0 mm [0.04 to 0.08 in.] (Notes 3 and 4). Corrections shall be applied to ensure accurate
in diameter, centrally located in reference to the vertical axis. measurements within 0.1 °C [0.2 °F].
The top surface of the stopper shall be substantially plane and
have no chips, and the lower surface shall be concave to allow 6.4 Balance, capable of making the required measurements
all air to escape through the bore. The height of the concave to an accuracy of at least 0.001 g [0.00001 oz].
section shall be 4.0 to 18.0 mm [0.16 to 0.71 in.] at the center. 6.5 Beaker, 600-mL [20-fluid oz] or larger Griffin low-form
The stoppered pycnometer shall have a capacity of 24 to 30 mL beaker.

FIG. 1 Suitable Pycnometers and Stopper

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D70 − 18
6.6 Tongs or Clean Nitrile (or Similar) Gloves, for placing removing the pycnometer from the water, the proper mass of the contents
and removing the pycnometer from the beaker. at the test temperature will be recorded. If moisture condenses on the
pycnometer during weighing, quickly re-dry the outside of the pycnometer
(excluding the top) before recording the mass.
7. Materials
7.1 Water—Boiled and cooled distilled or deionized water, 11. Procedure
free of visual contaminants. Water greater than three days post 11.1 Perform each of the following steps, handling the
boiling and cooling shall not be used (Note 6). pycnometer only with tongs or gloves as described in 6.6:
NOTE 5—Water should be discarded or re-boiled if bubbles are seen in 11.1.1 Preparation of Sample—Heat the sample with care,
the pycnometer during testing. stirring to prevent local overheating, until the sample has
NOTE 6—As an alternative to using heat, a vacuum source to pull a become sufficiently fluid to pour. In no case should the
negative pressure until the water boils without heat may be used. In this temperature be raised to more than 55 °C [131 °F] above the
case, the water does not have to be cooled before use.
expected softening point for tar, or to more than 110 °C
8. Sampling [230 °F] above the expected softening point for asphalt. Do not
heat for more than 120 min, and avoid incorporating air
8.1 Take samples in accordance with Practice D140/ bubbles into the sample.
D140M. The sample shall be free of foreign substances. 11.1.2 Pour enough sample into the clean, dry, warmed
8.2 Thoroughly mix the sample before removing a repre- pycnometer to fill it about three-fourths of its capacity. Take
sentative portion for testing. precautions to keep the material from touching the sides of the
pycnometer above the final level and prevent the inclusion of
9. Preparation of Apparatus air bubbles (Note 9). Allow the pycnometer and its contents to
9.1 Partially fill a 600-mL [20-fluid oz] or larger Griffin cool to ambient temperature for a period of not less than 40 min
low-form beaker with freshly boiled and cooled distilled or and weigh with the stopper to the nearest 0.001 g [0.00001 oz].
deionized water to a level that will allow the top of the Designate the mass of the pycnometer plus sample as C. The
pycnometer to be immersed to a depth of not less than 40 mm pycnometer shall be handled with only tongs or gloves during
[1.6 in.]. this entire process.
9.2 Partially immerse the beaker in the water bath to a depth NOTE 9—If any air bubbles are inadvertently entrained, remove by
sufficient to allow the bottom of the beaker to be immersed to brushing the surface of the asphalt in the pycnometer with a high “soft”
a depth of not less than 100 mm [3.9 in.], while the top of the flame of a Bunsen burner or torch. To avoid overheating, do not allow the
flame to remain in contact with the asphalt more than a few seconds at any
beaker is above the water level of the bath. Utilize some one time.
method to ensure that the beaker does not tip over, while
11.1.3 Remove the beaker from the water bath, if necessary.
making sure that circulation of the water in the conditioning
Fill the pycnometer containing the sample with freshly boiled
bath around the beaker is not restricted.
distilled or deionized water, placing the stopper loosely in the
9.3 Maintain the temperature of the water bath within 0.1 °C pycnometer. Do not allow any air bubbles to remain in the
[0.2 °F] of the test temperature as determined by the thermom- pycnometer. Place the pycnometer in the beaker and press the
eter described in 6.3. stopper firmly in place. Return the beaker to the water bath if
previously removed.
10. Standardization of Pycnometer 11.1.4 Allow the pycnometer to remain in the water bath for
10.1 Perform each of the following steps, handling the a period of not less than 30 min. Remove the pycnometer from
pycnometer only with tongs or gloves as described in 6.6: the bath. Dry and weigh using the same technique and timing
10.1.1 Thoroughly clean, dry, and weigh the pycnometer to as that employed in 10.1.3. Designate this mass of pycnometer
the nearest 0.001 g [0.00001 oz]. Designate this mass as A. plus sample plus water as D.
10.1.2 Remove the beaker from the water bath, if necessary.
Fill the pycnometer with freshly boiled distilled or deionized 12. Calculation
water, placing the stopper loosely in the pycnometer. Place the 12.1 Calculate the relative density to the nearest 0.001 as
pycnometer in the beaker and press the stopper firmly in place. follows:
Return the beaker to the water bath if previously removed. relative density 5 ~ C 2 A ! / @ ~ B 2 A ! 2 ~ D 2 C ! # (1)
NOTE 7—Standardization must be done at the test temperature. A
pycnometer standardized at one temperature cannot be used at a different
where:
temperature without restandardization at that temperature. A = mass of pycnometer (plus stopper),
10.1.3 Allow the pycnometer to remain in the water for a B = mass of pycnometer filled with water,
C = mass of pycnometer partially filled with asphalt, and
period of not less than 30 min. Remove the pycnometer and
D = mass of pycnometer plus asphalt plus water.
immediately dry the top of the stopper with one stroke of a dry
towel (Note 8), then quickly dry the remaining outside area of 12.2 Calculate density to the nearest 0.001 as follows:
the pycnometer and weigh to the nearest 0.001 g [0.00001 oz]. Density 5 relative density 3 W T (2)
Designate the mass of the pycnometer plus water as B.
where:
NOTE 8—Do not re-dry the top of the stopper even if a small droplet of
water forms as a result of expansion. If the top is dried at the instant of
WT = density of water at the test temperature (Note 10).

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D70 − 18
NOTE 10—Density of water from CRC Handbook of Chemistry and 14.2 Multilaboratory Precision—The multilaboratory
Physics: pooled standard deviation for the relative density (specific
Temperature Density of Water [Density of Water gravity) of semi-solid bituminous materials has been found to
°C [°F] kg/m3 (kg/L) lb/ft3 (lb/gal)]
15.6 [60.1] 999.0 (0.9990) [62.37 (8.337)] be 0.0024 at 15.6 °C and 0.0019 at 25.0 °C (see Table 1).
25.0 [77] 997.0 (0.9970) [62.24 (8.321)] Therefore, results of two properly conducted tests by two
13. Report laboratories on samples of the same material should not differ
by more than the following values (see Note 11):
13.1 Report density to the nearest 1 kg/m3 (0.001 kg/L)
Test Temperature, °C [°F] Density, kg/m3 (kg/L)
[0.05 lb ⁄ft3 (0.001 lb ⁄gal)] and the test temperature. 15.6 [60.1] 6.8 (0.0068)
25.0 [77] 5.4 (0.0054)
14. Precision and Bias
14.1 Single-Operator Precision—The single-operator NOTE 11—These number represent, respectively, the (1S) and (D2S)
pooled standard deviation for the relative density (specific limits as described in Practice C670.
gravity) of semi-solid bituminous materials has been found to 14.3 Bias—No information can be presented on the bias of
be 0.0013 at 15.6 °C and 0.00082 at 25.0 °C (see Table 1). the procedure in this test method for measuring density because
Therefore, results of two properly conducted tests by the same no material having an accepted reference value is available.
operator on the same material should not differ by more than
the following values (see Note 11): 15. Keywords
Test Temperature, °C [°F] Density, kg/m3 (kg/L)
15.6 [60.1] 3.7 (0.0037) 15.1 density; pycnometer; relative density; specific gravity
25.0 [77] 2.3 (0.0023)

SUMMARY OF CHANGES

Committee D04 has identified the location of selected changes to this standard since the last issue (D70 – 17)
that may impact the use of this standard. (Approved Apr. 1, 2018.)

(1) Term ‘bituminous materials’ changed to ‘asphalt binder’ in (4) Added new subsections 1.4 and 5.2.
Section 1. (5) Thermometer requirements updated in 6.3.2 and 6.3.3.
(2) SI units changed to combined SI/inch-pound units through- (6) Wording updated throughout to specify that the pycnometer
out. is to be handled with tongs or gloves at all times.
(3) Specifications D3666 and E879 added to Section 2.

Committee D04 has identified the location of selected changes to this standard since the last issue (D70 – 09)
that may impact the use of this standard. (Approved Dec. 15, 2017.)

(1) Term ‘asphalt cement’ changed to ‘asphalt’ in 1.1. (8) Rubber-covered tongs added to the apparatus in 6.6.
(2) Units changed to SI only in 1.2. (9) Maximum preheat time changed from 60 min to 120 min in
(3) Mercury caveat moved to Section 1. 11.1.
(4) Term ‘calibrate’ changed to ‘standardize’ throughout. (10) ASTM standards E77, E563, E644, and E1137/E1137M
(5) Thermometer wording changed to be more specific in 6.3. added to Section 2.
(6) Requirements for water updated in 7.1.
(7) Note 6 added to indicate that water can be boiled by
applying negative pressure until it boils.

TABLE 1 Precision of Relative Density Data for Semi-Solid Bituminous Materials


Single-Operator Multilaboratory
Temperature
°C [°F] Degrees of Degrees of
(1S) (D2S) (1S) (D2S)
Freedom Freedom
Asphalt 15.6 [60.1] 54 0.0011 0.0032 24 0.0018 0.0051
25.0 [77] 54 0.00080 0.0023 24 0.0024 0.0068

Soft tar pitch 15.6 [60.1] 72 0.0013 0.0038 27 0.0029 0.0083


25.0 [77] 72 0.00083 0.0023 27 0.0017 0.0048

Pooled values 15.6 [60.1] 114 0.0013 0.0037 51 0.0024 0.0068


25.0 [77] 114 0.00082 0.0023 51 0.0019 0.0053

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D70 − 18
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