ASTM D3971-89(2004)

Standard Test Method for Dichloromethane-Soluble Matter in Cellulose

SIGNIFICANCE AND USE
Dichloromethane-soluble materials are typically referred to as extractives. These extractives are comprised of organic materials that originated in the wood or cotton. The measure is an indication of the efficiency of removal of these substances during pulping and bleaching. The extractive level is of concern to dissolving pulp users since the presence of large amounts of extractives could inhibit the processing of cellulose into the desired derivative.
SCOPE
1.1 This test method covers the determination of dichloromethane-soluble matter in cellulose and is applicable to dissolving-type cellulose pulps prepared from cotton or wood.
1.2 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-May-2004
• ICS: 85.040 - Pulps
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaces: ASTM D3971-89(1999) - Standard Test Method for Dichloromethane-Soluble Matter in Cellulose
• Effective Date: 01-Jun-2004
• Replaced By: ASTM D3971-89(2010) - Standard Test Method for Dichloromethane-Soluble Matter in Cellulose
• Effective Date: 01-Jun-2010

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3971 – 89 (Reapproved 2004)
Standard Test Method for
Dichloromethane-Soluble Matter in Cellulose
This standard is issued under the fixed designation D3971; 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 5.1.3 Extractor Tube, with standard taper 45/50 top joint.
5.1.4 Allihn Standard Taper, 45/50 or
1.1 This test method covers the determination of
5.1.5 Friedrichs Standard Taper, 45/50 type condenser.
dichloromethane-soluble matter in cellulose and is applicable
5.2 Extraction Thimble, either (1) standard thickness paper,
to dissolving-type cellulose pulps prepared from cotton or
43 by 123 mm, (2) aluminum oxide, 34 by 100 mm, medium
wood.
porosity, or (3) glass with coarse-porosity fritted-glass disk, 45
1.2 This standard does not purport to address all of the
by 130 mm.
safety concerns, if any, associated with its use. It is the
5.3 Heating Device—Steam bath or heating mantle.
responsibility of the user of this standard to establish appro-
5.4 Oven, maintained at 105 6 3°C.
priate safety and health practices and determine the applica-
5.5 Dish, evaporating, disposable, light aluminum, 63 mm
bility of regulatory limitations prior to use.
in diameter by 17.5 mm deep.
2. Referenced Documents 5.6 Desiccator with efficient desiccant.
2.1 ASTM Standards:
6. Reagent
D1348 Test Methods for Moisture in Cellulose
6.1 Dichloromethane,ACS, 99 % CH Cl , having a residue
2 2
3. Summary of Test Method
after evaporation of less than 0.002 %.
3.1 Asample is extracted with dichloromethane in a Soxhlet
7. Procedure
apparatus as a measure of the waxes, fats, resins, and oils
7.1 Weigh 8 to 12 g of loose pulp, to the nearest 0.01 g, into
present.
an extractor thimble that has previously been extracted with
4. Significance and Use
dichloromethane. For sheet pulp, cut a sample into strips about
10 mm wide and 70 mm long, and weigh about 20 g into a
4.1 Dichloromethane-soluble materials are typically re-
thimble. Weigh a separate portion for a moisture determination
ferred to as extractives. These extractives are comprised of
in accordance with Test Methods D1348.
organic materials that originated in the wood or cotton. The
7.2 Place the extraction thimble with sample in the extractor
measure is an indication of the efficiency of removal of these
andconnecttheflask.Pour250mLofthedichloromethaneinto
substances during pulping and bleaching. The extractive level
the body of the extractor. Connect the assembled extractor to
is of concern to dissolving pulp users since the presence of
the condenser and place the flask in the heating device.Turn on
large amounts of extractives could inhibit the processing of
the cooling water to the condenser and adjust the heating rate
cellulose into the desired derivative.
to cause siphoning 6 to 8 times per hour. Continue the
5. Apparatus
extraction for 5 h.
7.3 Heat the evaporating dish in the oven at 105°C for 30
5.1 Extraction Apparatus:
min, cool in a desiccator, and weigh to the nearest 0.1 mg.
5.1.1 Soxhlet.
7.4 When the extraction is complete, disconnect the flask at
5.1.2 Flask, 250-mL.
a time when most of the solvent has collected in the extractor.
Partially evaporate the solvent in the extraction flask to a
This test method is under the jurisdiction of ASTM Committee D01 on Paint
volume of 15 to 20 mL. T
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