ASTM D4-86(1998)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4–86 (Reapproved 1998)
Standard Test Method for
Bitumen Content
This standard is issued under the fixed designation D 4; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense. Although this test method was withdrawn by the
Society in June 1966 at the request of Committee D-4, the Committee on Standards has approved its reinstatement under the jurisdiction
of Committee D-8 on the basis that Procedure No. 2 still applies to their interest. Procedure No. 1 has been replaced by Method D 2042,
Test for Solubility of Asphalt Materials in Trichloroethylene.
1. Scope 3.3 Beakers—One 30-mL beaker, Griffin low-form, and one
150-mL beaker, Griffin low-form.
1.1 This test method covers the determination of bitumen
3.4 Carbon Disulfide, cp.
content in materials containing at least 25 % bitumen. Bitumen
content may usually be expeditiously and accurately deter-
NOTE 1—For filled asphaltic materials, trichloroethylene may be di-
mined by Procedure No. 1, Section 7. However, some bitumi- rectly substituted for carbon disulfide if desired. However, carbon disul-
fide shall be used in referee testing.
nous materials containing finely divided mineral matter may
clog the filter or the mineral residue may not be easily retained,
3.5 Filtering Flask, with crucible adapter.
in which cases Procedure No. 2, Section 8, shall be followed.
3.6 Drying Oven.
1.2 This standard does not purport to address all of the
3.7 Bunsen Burner or Muffle Furnace.
safety concerns, if any, associated with its use. It is the
3.8 Suction Pump.
responsibility of the user of this standard to establish appro-
3.9 Analytical Balance.
priate safety and health practices and determine the applica-
3.10 Desiccator.
bility and regulatory limitations prior to use. For specific
3.11 Evaporating Dish.
precautionary information, see Section 4.
3.12 Watch Glasses.
2. Referenced Documents
4. Safety Precautions
2.1 ASTM Standards:
4.1 Carbon disulfide is extremely flammable. The vapor will
D 370 Test Method for Dehydration of Oil-Type Preserva-
often ignite spontaneously on contact with a hot surface such as
tives
a hot plate, oven, or radiator. When using this solvent, be sure
E 177 Practice for Use of the Terms Precision and Bias in
that the filtration is conducted under a hood and well away
ASTM Test Methods
from flame or other sources of heat. Before placing crucibles or
other containers in the oven, all traces of carbon disulfide
3. Apparatus, Reagents, and Materials
should be removed (as indicated by the disappearance of all
3.1 Filtering Crucible, porcelain, high-form, 25 to 40-mL
odor). Otherwise, the vapors will ignite. Carbon disulfide is
capacity, with fine-porosity bottom, 7-μm maximum porosity.
also very irritating to the skin and direct contact should be
5 6
3.2 Celite Analytical Filter Aid (CAFA), dried to constant
avoided.
mass at 105°C and stored in a tightly stoppered container.
5. Preparation of Sample
1 5.1 The sample shall be representative, and if it contains
This test method is under the jurisdiction of ASTM Committee D08 on
Roofing, Waterproofing, and Bituminous Materialsand is the direct responsibility of more than 2 % of water it shall be dehydrated in accordance
Subcommittee D08.03 on Surfacing and Bituminous Materials for Membrane
with Test Method D 370. If the material is hard and brittle, it
Waterproofing and Builtup Roofing.
may be ground and dried at a temperature below the tempera-
Current edition approved May 30, 1986. Published July 1986. Originally
ture of volatilization of the material.
published as D4–11. Last previous edition D4–80 (1985).
Annual Book of ASTM Standards, Vol 04.09.
Annual Book of ASTM Standards, Vol 14.02. 6. Crucible Preparation
Selas grade 01, size FC 30 or FC 40, or equivalent. Available from various
6.1 If the crucible, after thorough cleaning (see 6.2), has
laboratory supply houses such as Fisher Scientific. An alternative is Royal Berlin
been used for less than six determinations, clean it as follows:
2A2 (size equivalent to FC 40) from Fish Schurman Corp., 70 Portman Road, New
Rochelle, NY 10802.
Remove the CAFA mat completely, wash the crucible with
Trademark of Manville Corp.
distilled water, dry, and ignite in a muffle furnace for1hat
Use Celite 211 Analytical Filter Aid from Fisher Scientific, Pittsburgh, PA, or
about 800°C. Cool the crucible slowly by placing it in a drying
Celite 505 from Manville Corp., Denver, CO.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4–86 (1998)
oven for 1 h after removal from the furnace to prevent cracking 8. Procedure No. 2
and place it in a desiccator while still warm.
8.1 Weigh approximately2gofthe sample into a tared
6.2 After the crucible has been used for six determinations,
50-mL beaker. Add to the beaker about 0.5 g, weighed to the
remove any residual ash from pores in the filtering area by
nearest 0.001 g, of freshly dried CAFA. Cover with about 25
boiling in 1 + 1 hydrochloric acid. Then boil the crucible in
mL of carbon disulfide and stir the filter aid into the liquid. Let
distilled water, thoroughly back wash with distilled water, dry,
stand, covered with a watch glass, at least 1 h, stirring
and ignite as in 6.1.
occasionally in order to dissolve the sample completely.
7. Procedure No. 1
8.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,
7.1 Weigh approximately2gofthe sample (size sample to
filtering crucible. Distribute the Celite evenly over the bottom.
obtain 0.1 to 0.3 g of insoluble matter) into a tared 150-mL
Immediately weigh and record the mass of crucible plus Celite.
beaker and add 100 mL of carbon disulfide to the beaker in
8.3 Immediately before starting the filtering process, stir the
small portions, with continuous agitation, until all lumps
filter aid into the liquid. Wet the CAFA mat in the crucible with
disappear and nothing adheres to the beaker. Cover the beaker
carbon disulfide. Pour the solution from the beaker onto the
with a watch glass and set it aside for 15 min.
pad, filling the crucible to the top. Apply light suction and, as
7.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,
the liquid filters through, pour the remaining contents of the
filtering crucible. Distribute the Celite evenly over the bottom.
50-mL beaker into the crucible. Wash the beaker with a small
Immediately weigh and record the weight of crucible plus
amount of carbon disulfide and transfer all sediment from the
Celite.
beaker to the mat. Do not allow the CAFA mat to dry out until
7.3 Decant the carbon disulfide solution carefully through
filtration is complete. Wash with carbon disulfide until the
the CAFA mat (previously wetted with carbon disulfide) in the
filtrate is substantially colorless, then apply strong suction to
prepared crucible, with or without light suction as may be
remove the remaining carbon disulfide. Rem
...