Standard Test Method for Softening Point of Pitches (Cube-in-Water Method)

SIGNIFICANCE AND USE
5.1 Pitch does not go through a solid-liquid phase change when heated, and therefore it does not have a true melting point. As the temperature rises, pitch softens and becomes less viscous. The softening point is arbitrarily defined and shall be established by a closely controlled method which shall be carefully followed if test results are to be reproducible.  
5.2 This test is useful in determining the consistency of pitch as one element in establishing the uniformity of shipments or sources of supply.
SCOPE
1.1 This test method covers the determination of the softening point of pitches below 176 °F (80 °C). Pitches of higher softening point should be tested by Test Method D2319 or Test Method D3104.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

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Publication Date
30-Nov-2019
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ASTM D61-15(2019) - Standard Test Method for Softening Point of Pitches (Cube-in-Water Method)
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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: D61 − 15 (Reapproved 2019)
Standard Test Method for
Softening Point of Pitches (Cube-in-Water Method)
This standard is issued under the fixed designation D61; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope E2251 Specification for Liquid-in-Glass ASTM Thermom-
eters with Low-Hazard Precision Liquids
1.1 This test method covers the determination of the soft-
E2877 Guide for Digital Contact Thermometers
ening point of pitches below 176 °F (80 °C). Pitches of higher
softening point should be tested by Test Method D2319 or Test
3. Terminology
Method D3104.
3.1 Definitions:
1.2 The values stated in inch-pound units are to be regarded
3.1.1 Digital Contact Thermometer (DCT), n—an electronic
as standard. The values given in parentheses are mathematical
device consisting of a digital display and associated tempera-
conversions to SI units that are provided for information only
ture sensing probe.
and are not considered standard.
3.1.1.1 Discussion—This device consists of a temperature
1.3 This standard does not purport to address all of the
sensor connected to a measuring instrument; this instrument
safety concerns, if any, associated with its use. It is the
measures the temperature-dependent quantity of the sensor,
responsibility of the user of this standard to establish appro-
computes the temperature from the measured quantity, and
priate safety, health, and environmental practices and deter-
providesadigitaloutputordisplay,orboth,ofthetemperature.
mine the applicability of regulatory limitations prior to use.
The temperature sensing probe is in contact with the material
1.4 This international standard was developed in accor-
whose temperature is being measured. This device is some-
dance with internationally recognized principles on standard-
times referred to as a digital thermometer.
ization established in the Decision on Principles for the
NOTE 1—Portable electronic thermometers (PET) is an acronym some-
Development of International Standards, Guides and Recom-
times used to refer to a subset of the devices covered by this definition.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4. Summary of Test Method
4.1 Two cubes of pitch, supported on wire hooks, are heated
2. Referenced Documents
at a controlled rate in water in a glass container. The softening
2.1 ASTM Standards:
point is defined as the mean of the temperatures at which the
D140 Practice for Sampling Asphalt Materials
cubes sag downwards a distance of 25 mm.
D2319 Test Method for Softening Point of Pitch (Cube-in-
Air Method)
5. Significance and Use
D3104 Test Method for Softening Point of Pitches (Mettler
5.1 Pitch does not go through a solid-liquid phase change
Softening Point Method)
when heated, and therefore it does not have a true melting
E1 Specification for ASTM Liquid-in-Glass Thermometers
point.As the temperature rises, pitch softens and becomes less
E563 Practice for Preparation and Use of an Ice-Point Bath
viscous. The softening point is arbitrarily defined and shall be
as a Reference Temperature
established by a closely controlled method which shall be
E1137 SpecificationforIndustrialPlatinumResistanceTher-
carefully followed if test results are to be reproducible.
mometers
5.2 This test is useful in determining the consistency of
pitch as one element in establishing the uniformity of ship-
ments or sources of supply.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
6. Apparatus
Current edition approved Dec. 1, 2019. Published December 2019. Originally
6.1 Mold—A mold suitable for forming two ⁄2 in.
approved in 1919. Last previous edition approved in 2015 as D61 – 15. DOI:
10.1520/D0061-15R19.
(12.7 mm) cubes of pitch, having cylindrical core pins 12
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
gauge (2.05 mm) in diameter located in the base plate of the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
assembly to produce accurately centered suspension holes in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the cubes. (See Fig. 1.)
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D61 − 15 (2019)
FIG. 1 Apparatus for Cube-in-Water Method
6.2 Hooks—Two L-shaped hooks, made of 12 gauge glass thermometers described in 6.4.2. A DCT or calibrated
(2.05 mm) copper wire. The foot of the hook shall be 1 in. liquid-in-glass thermometer shall be used as the thermometer
(25 mm) long and at a right angle to the upright portion for
for temperature measurement independent of the instrument’s
insertion into the center hole of the pitch cube.
temperature control, and shall be located in the thermowell.
6.3 Container—A glass vessel that can be heated, not less
NOTE 2—The display device and sensor must be correctly paired.
than85 mmindiameterand105 mmdeep.(Astandard600 mL
Incorrect pairing will result in temperature measurement errors and
low-form beaker meets these requirements).
possibly irreversible damage to the electronics of the display.
6.4 Temperature Measuring Device—Use either a calibrated
DCT meeting the requirements described in 6.4.1 or liquid-in-
D61 − 15 (2019)
6.4.1 Digital Contact Thermometer Requirements: ice point by one scale division, or until five years has elapsed
since the last full calibration.
Criteria Requirements
DCT E2877 Class E, Minimum
6.5 Heat Source:
Temperature range –2 °C to 80 °C 6.5.1 Electric Heater—A hot plate or immersion heater
provided with a variable transformer or other device suitable
Display resolution 0.1 °C
for regulating the temperature of the heating element.
6.5.2 Gas Heater—A bunsen-type burner, fitted with a
Sensor type PRT, thermistor, Type E or T thermocouple
chimney.
Sensor, sheath Metal or glass
7. Sampling
Sensor length Less than 12 mm in length
7.1 Samples from shipments shall be taken in accordance
Immersion depth 76 mm
with Practice D140 and shall be free of foreign substances.
Display accuracy ±0.2 °C for combined probe and sensor
Thoroughly mix the sample before removing a representative
portion for the determination or for dehydration.
Response time Less than or equal to 30 s as defined in Specifica-
tion E1137
7.2 If the presence of water is indicated by surface foam on
heating, maintain the sample at a temperature of about 260 °F
Drift Less than 0.2 °C per year
(125 °C) in an open container until the surface is free of foam.
Calibration error Less than 0.2 °C over the range of intended use
Take care not to overheat, and remove from the heat source as
soon as the foam has subsided.
Calibration range –2 °C to 80 °C
8. Test Specimens
Calibration data 4 data points evenly distributed over the range
and included in calibration report
8.1 Coat the inner surfaces and core pins of the mold very
Calibration report From a calibration laboratory with demonstrated lightly with silicone oil or silicone grease. Form the pitch into
competency in temperature calibration which
...

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