ASTM D3971-89(2010)
(Test Method)Standard Test Method for Dichloromethane-Soluble Matter in Cellulose
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3971 − 89 (Reapproved 2010)
Standard Test Method for
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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. Apparatus
1.1 This test method covers the determination of 5.1 Extraction Apparatus:
dichloromethane-soluble matter in cellulose and is applicable
5.1.1 Soxhlet.
to dissolving-type cellulose pulps prepared from cotton or
5.1.2 Flask, 250-mL.
wood.
5.1.3 Extractor Tube, with standard taper 45/50 top joint.
5.1.4 Allihn Standard Taper, 45/50 or
1.2 The values stated in SI units are to be regarded as
5.1.5 Friedrichs Standard Taper, 45/50 type condenser.
standard. No other units of measurement are included in this
standard.
5.2 Extraction Thimble, either (1) standard thickness paper,
43 by 123 mm, (2) aluminum oxide, 34 by 100 mm, medium
1.3 This standard does not purport to address all of the
porosity, or (3) glass with coarse-porosity fritted-glass disk, 45
safety concerns, if any, associated with its use. It is the
by 130 mm.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.3 Heating Device—Steam bath or heating mantle.
bility of regulatory limitations prior to use.
5.4 Oven, maintained at 105 6 3°C.
2. Referenced Documents 5.5 Dish, evaporating, disposable, light aluminum, 63 mm
2
in diameter by 17.5 mm deep.
2.1 ASTM Standards:
D1348 Test Methods for Moisture in Cellulose 5.6 Desiccator with efficient desiccant.
3. Summary of Test Method
6. Reagent
3.1 Asample is extracted with dichloromethane in a Soxhlet
6.1 Dichloromethane, ACS, 99 % CH Cl , having a residue
2 2
apparatus as a measure of the waxes, fats, resins, and oils
after evaporation of less than 0.002 %.
present.
7. Procedure
4. Significance and Use
7.1 Weigh 8 to 12 g of loose pulp, to the nearest 0.01 g, into
4.1 Dichloromethane-soluble materials are typically re-
an extractor thimble that has previously been extracted with
ferred to as extractives. These extractives are comprised of
dichloromethane. For sheet pulp, cut a sample into strips about
organic materials that originated in the wood or cotton. The
10 mm wide and 70 mm long, and weigh about 20 g into a
measure is an indication of the efficiency of removal of these
thimble. Weigh a separate portion for a moisture determination
substances during pulping and bleaching. The extractive level
in accordance with Test Methods D1348.
is of concern to dissolving pulp users since the presence of
7.2 Place the extraction thimble with sample in the extractor
large amounts of extractives could inhibit the processing of
andconnecttheflask.Pour250mLofthedichloromethaneinto
cellulose into the desired derivative.
the body of the extractor. Connect the assembled extractor to
the condenser and place the flask in the heating device.Turn on
the cooling water to the condenser and adjust the heating rate
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This test method is under the jurisdiction of ASTM Committee D01 on Paint
to cause siphoning 6 to 8 times per hour. Continue the
and Related Coatings, Materials, andApplications and is the direct responsibility of
extraction for 5 h.
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
CurrenteditionapprovedJune1,2010.PublishedJuly2010.Originallyapproved
7.3 Heat the evaporating dish in the oven at 105°C for 30
in 1980. Last previous edition approved in 2004 as D3971 – 89 (2004). DOI:
min, cool in a desiccator, and weigh to the nearest 0.1 mg.
10.1520/D3971-89R10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
7.4 When the extraction is complete, disconnect the flask at
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
a time when most of the solvent has collected in the extractor.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Partially evaporate the solvent in the extraction flask to a
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D3971 − 89 (2010)
volume of 15 to 20 mL. Transfer the extract to the tared where:
weighing dish by washing with three 5-mL portions of fresh
W = oven-dry weight of extract, g,
e
solvent.
W = oven-dry weight of solvent blank determined in 7.6,g,
b
W = weight of sample, g, and
s
7.5 Place the dish on a steam hot plate and evaporate just to
M = moisture in sample, % (Test Methods D1348).
dryness. Then place the dish in the oven at 105°C fo
...
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