ASTM D3971-89(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 3971 – 89 (Reapproved 1999)
Standard Test Method for
Dichloromethane-Soluble Matter in Cellulose
This standard is issued under the fixed designation D 3971; 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.
1. Scope 5.1.4 Allihn Standard Taper, 45/50 or
5.1.5 Friedrichs Standard Taper, 45/50 type condenser.
1.1 This test method covers the determination of
5.2 Extraction Thimble, either (1) standard thickness paper,
dichloromethane-soluble matter in cellulose and is applicable
43 by 123 mm, (2) aluminum oxide, 34 by 100 mm, medium
to dissolving-type cellulose pulps prepared from cotton or
porosity, or (3) glass with coarse-porosity fritted-glass disk, 45
wood.
by 130 mm.
1.2 This standard does not purport to address all of the
5.3 Heating Device—Steam bath or heating mantle.
safety concerns, if any, associated with its use. It is the
5.4 Oven, maintained at 105 6 3°C.
responsibility of the user of this standard to establish appro-
5.5 Dish, evaporating, disposable, light aluminum, 63 mm
priate safety and health practices and determine the applica-
in diameter by 17.5 mm deep.
bility of regulatory limitations prior to use.
5.6 Desiccator with efficient desiccant.
2. Referenced Documents
6. Reagent
2.1 ASTM Standards:
6.1 Dichloromethane, ACS, 99 % CH Cl , having a residue
2 2
D 1348 Test Methods for Moisture in Cellulose
after evaporation of less than 0.002 %.
3. Summary of Test Method
7. Procedure
3.1 A sample is extracted with dichloromethane in a Soxhlet
7.1 Weigh 8 to 12 g of loose pulp, to the nearest 0.01 g, into
apparatus as a measure of the waxes, fats, resins, and oils
an extractor thimble that has previously been extracted with
present.
dichloromethane. For sheet pulp, cut a sample into strips about
4. Significance and Use
10 mm wide and 70 mm long, and weigh about 20 g into a
thimble. Weigh a separate portion for a moisture determination
4.1 Dichloromethane-soluble materials are typically re-
in accordance with Test Methods D 1348.
ferred to as extractives. These extractives are comprised of
7.2 Place the extraction thimble with sample in the extractor
organic materials that originated in the wood or cotton. The
and connect the flask. Pour 250 mL of the dichloromethane into
measure is an indication of the efficiency of removal of these
the body of the extractor. Connect the assembled extractor to
substances during pulping and bleaching. The extractive level
the condenser and place the flask in the heating device. Turn on
is of concern to dissolving pulp users since the presence of
the cooling water to the condenser and adjust the heating rate
large amounts of extractives could inhibit the processing of
to cause siphoning 6 to 8 times per hour. Continue the
cellulose into the desired derivative.
extraction for 5 h.
5. Apparatus
7.3 Heat the evaporating dish in the oven at 105°C for 30
min, cool in a desiccator, and weigh to the nearest 0.1 mg.
5.1 Extraction Apparatus:
7.4 When the extraction is complete, disconnect the flask at
5.1.1 Soxhlet.
a time when most of the solvent has collected in the extractor.
5.1.2 Flask, 250-mL.
Partially evaporate the solvent in the extraction flask to a
5.1.3 Extractor Tube, with standard taper 4
...