ASTM D3104-14a(2018)
(Test Method)Standard Test Method for Softening Point of Pitches (Mettler Softening Point Method)
Standard Test Method for Softening Point of Pitches (Mettler Softening Point Method)
SIGNIFICANCE AND USE
4.1 Pitch does not go through a solid-liquid phase change when heated, and therefore does not have a true melting point. As the temperature is raised pitch gradually softens or becomes less viscous. For this reason, the determination of the softening point must be made by an arbitrary, but closely defined, method if the test values are to be reproducible.
4.2 This test method is useful in determining the consistency of pitches 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 having softening points in the range from 50 °C to 180 °C by this test method, and gives results comparable to those obtained by Test Method D2319 above 80 °C (176 °F).
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units 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.
General Information
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Standards Content (Sample)
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: D3104 − 14a (Reapproved 2018)
Standard Test Method for
Softening Point of Pitches (Mettler Softening Point Method)
This standard is issued under the fixed designation D3104; 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 a 6.35 mm hole in the bottom, flows downward a distance of
19 mm to interrupt a light beam, as the sample is heated at a
1.1 This test method covers the determination of the soft-
linear rate in air.
eningpointofpitcheshavingsofteningpointsintherangefrom
50 °C to 180 °C by this test method, and gives results
4. Significance and Use
comparable to those obtained by Test Method D2319 above
80 °C (176 °F). 4.1 Pitch does not go through a solid-liquid phase change
when heated, and therefore does not have a true melting point.
1.2 The values stated in SI units are to be regarded as
Asthetemperatureisraisedpitchgraduallysoftensorbecomes
standard. The values given in parentheses after SI units are
less viscous. For this reason, the determination of the softening
provided for information only and are not considered standard.
pointmustbemadebyanarbitrary,butcloselydefined,method
1.3 This standard does not purport to address all of the
if the test values are to be reproducible.
safety concerns, if any, associated with its use. It is the
4.2 This test method is useful in determining the consis-
responsibility of the user of this standard to establish appro-
tency of pitches as one element in establishing the uniformity
priate safety, health, and environmental practices and deter-
of shipments or sources of supply.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
5. Apparatus
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 5.1 A METTLER TOLEDO dropping point cell shall be
Development of International Standards, Guides and Recom- used to determine pitch softening points by this test method.
mendations issued by the World Trade Organization Technical These commercially available instruments consist of a control
Barriers to Trade (TBT) Committee. unit with a digital temperature indicator, with furnace built in
or attached, sample cartridges, and accessories. The control
unitautomaticallyregulatestheheatingrateofthefurnace.The
2. Referenced Documents
2 softening point is indicated on the readout, and the heating
2.1 ASTM Standards:
program stopped, when the sample flow triggers the softening
A314 Specification for Stainless Steel Billets and Bars for
point detection.Ageneral view of the contents of a METTLER
Forging
TOLEDO dropping point instrument is shown in Fig. 1 (old
D2319 Test Method for Softening Point of Pitch (Cube-in-
instrument) and Fig. 2 (new instrument).
Air Method)
5.1.1 IntegratedorSeparateControlUnit—The control unit
D4296 Practice for Sampling Pitch
shall provide a continuous, linear temperature increase from 25
°C to 250 °C at a rate of 2 °C/min. A digital readout shall
3. Summary of Test Method
indicate the temperature to 0.1 °C throughout.
3.1 In this test method, the softening point is defined as the
5.1.2 Integrated or Separate Furnace Unit—The furnace
temperatureatwhichpitch,suspendedinacylindricalcupwith
unit shall be capable of heating one or two sample cup
assemblies, as described in 5.1.3, at a linear rate of 2 °C 6
0.3 °C⁄min. It shall include a sensing system capable of
1 detecting the softening point with a precision of 0.1 °C.
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.
Current edition approved Dec. 1, 2018. Published December 2018. Originally
approved in 1972. Last previous edition approved in 2014 as D3104 – 14a. DOI: The sole source of supply of the apparatus known to the committee at this time
10.1520/D3104-14AR18. is available from Mettler-Toledo, LLC., 1900 Polaris Pkwy, Columbus, OH 43240,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or www.mt.com. If you are aware of alternative suppliers, please provide this
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
Standards volume information, refer to the standard’s Document Summary page on careful consideration at a meeting of the responsible technical committee, which
the ASTM website. you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3104 − 14a (2018)
FIG. 1 General View of the METTLER TOLEDO FP90 Control Unit with Heater FP83HT
5.1.3 Sample Cup Assembly—A cup of chromium-plated 7. Calibration of the METTLER TOLEDO Apparatus
brass, or of aluminum, or of stainless steel conforming to the
7.1 This step, required only occasionally, is designed to
requirements for Type 303 (UNS S30300) stainless steel as
establish that the temperature indicated by the instrument is in
prescribed in Specification A314, with the dimensions shown
agreement with a known standard.Aspecial cup with a bottom
in Fig. 3. It shall be placed in the assembly so that the pitch
orifice of 2.8 mm is used instead of the one prescribed for the
sample softening point will be detected when it has flowed
testing of pitch.
down a distance of 19 mm.
7.2 Reagent—Use either analytical reagent or primary stan-
dard grade benzoic acid for the calibration. As this material is
6. Reagents
hygroscopic it must be stored in a tightly sealed container, and
6.1 Xylene, industrial grade.
replaced with fresh material from a newly opened supply if
6.2 Benzoic Acid. hydration or other contamination is suspected.
D3104 − 14a (2018)
FIG. 2 General View of the METTLER TOLEDO DP70
7.3 Procedure—Old Instruments: heating cycle at 0.2 °C/min. The temperature will rise steadily
7.3.1 Filling the Sample Cup—Place the cup on a clean, flat
at the correct rate until the drop point is reached, and then
surface.Add a small amount of benzoic acid crystals and press remain steady on the readout.
down with a rod (approximately 4.5 mm in diameter). Check
7.3.3 Cleaning—Immediately remove the cartridge assem-
thatthebottomorificeiscompletelyfilled.Refillandrepeatthe
bly. Check to determine that the sample has passed through the
pressing step until the cup is filled with benzoic acid. Remove
light beam and no pre-triggering has occurred. If a malfunction
any crystals from the exterior of the cup.
is suspected, the entire procedure must be repeated. Inspect the
7.3.2 Heating—Preheat the Mettler furnace to 121 °C, and
apparatus carefully to ensure that no residue remains. Use a
maintain it at that temperature. Place the cartridge assembly
spatula shaped to the contour of the cup to remove most of the
containing the benzoic acid in position in the furnace, taking
remaining acid from the cup and from the bottom of the
care that the slits for the light beam are properly positioned.
cartridge. Wash the cup and cartridge in xylene, or other
Wait for temperature equilibration, that is, the furnace and the
suitable solvent, to remove the last traces of the residue.
sampleareinequilibriumatthepresettemperature,butnotless
than the 30 s after inserting the cartridge, start the automatic 7.4 Interpretation—See 7.6.
D3104 − 14a (2018)
benzoic acid. If the deviation exceeds 0.6 °C, the instrument
requires recalibration or repair. Consult the manufacturer’s
instruction manual.
8. Sampling
8.1 Samples from shipments shall be taken in accordance
with Practice D4296, and shall be free of foreign substances.
Thoroughly mix the sample before removing a representative
portion for the determination or for dehydration.
8.2 If a solid bulk sample contains free water, air-dry a
representative portion in a forced draft oven at 50 °C.
8.3 Ifthesampleisliquid,checkforanysurfacefoamwhich
may indicate the presence of water. If foam is found, maintain
the sample at a temperature of about 125 °C in an open
container until the surface is free of foam. Take care not to
overheat.Removefromtheheatsourceassoonasthefoamhas
subsided. Proceed as directed in 8.4.2.
8.4 Filling the Sample Cup:
FIG. 3 Sample Cup
8.4.1 Crush air-dry lumps of pitch to a size of 6 mm to
12 mm. Add the material to a container, having a height equal
to or exceeding its width, and having a volume of not less than
7.5 Procedure—New Instruments:
50 mL, until it is about half full. Place the container on a hot
7.5.1 Filling the Sample Cup—Place the cup on a clean, flat
plate, or in an oven or a bath. Do not use an open flame to melt
surface. Optionally, the sample preparation tool may be used.
pitch. After melting is complete, stir gently but thoroughly,
See Fig. 2. Add a small amount of benzoic acid crystals and
avoiding incorporation of air bubbles. The maximum tempera-
press down with a rod (approximately 4.5 mm in diameter).
ture of the molten pitch should not exceed the expected
Check that the bottom orifice is completely filled. Refill and
softening point by more than 50 °C.Any foam that forms must
repeatthepressingstepuntilthecupisfilledwithbenzoicacid.
be skimmed off.
Remove any crystals from the exterior of the cup. Place a glass
8.4.2 Prepare the sample by slightly overfilling the sample
collector below the cup and a cup cap on top, and place in the
cup, which rests on a brass plate. Optionally, the sample
sample carrier. Two cup assemblies m
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