ASTM D1106-96(2001)
(Test Method)Standard Test Method for Acid-Insoluble Lignin in Wood
Standard Test Method for Acid-Insoluble Lignin in Wood
SCOPE
1.1 This test method covers the determination of the acid-insoluble lignin content of 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. Specific precautionary statements are given in 6.1.
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Technical Association of Pulp and Paper Industry
Designation:D1106–96 (Reapproved 2001) Standard Method T 222-om-83
Standard Test Method for
Acid-Insoluble Lignin in Wood
This standard is issued under the fixed designation D 1106; 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 birch, beech, and maple. It is recommended that for these
woods the alcohol extraction be omitted unless it is desirable
1.1 This test method covers the determination of the
for a special purpose. In analysis of woods not listed, the
acid-insoluble lignin content of wood.
desirabilty of the alcohol extraction depends upon the purpose
1.2 This standard does not purport to address all of the
of the analysis and the report should state whether or not
safety concerns, if any, associated with its use. It is the
alcohol extraction was used.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use. Specific precau-
4.1 Wood contains approximately 20 to 30 % lignin. Re-
tionary statements are given in 6.1.
moval of the lignin is the primary objective of pulping and
2. Referenced Documents bleaching procedures. Determination of the lignin content
provides information for the evaluation and application of
2.1 ASTM Standards:
these processes.
D 1107 Test Method for Ethanol-Toluene Solubility of
Wood
5. Apparatus
3. Principle of Method 5.1 Extraction Apparatus—A compact form of Soxhlet
extraction apparatus, with ground-glass joints, is preferable.
3.1 When wood is treated with strong acids the carbohy-
The apparatus shall consist of the following items:
drates are hydrolyzed, leaving an insoluble residue which is
5.1.1 Soxhlet Extraction Flask, having a capacity of 250
determined as lignin. Since some of the wood extractives (oils,
mL.
resins, fats, waxes, tannins, gums, and starch) would remain
5.1.2 Soxhlet Extraction Tube, 45 to 50 mm in inside
insoluble with the lignin, these are first removed by proper
diameter, having a capacity to the top of the siphon of
solvents.The72 %sulfuricacidmethodforlignincontainstwo
approximately 100 mL and a siphon tube approximately 55
and sometimes three preliminary extractive treatments,
mm in height. Extraction tubes of these dimensions siphon
namely: (1) with alcohol, to remove the catechol tannins; (2)
more rapidly than extractors with higher siphon tubes.
with alcohol-benzene solution, to remove the resins, oils, fats
5.1.3 Condenser, of the Hopkins inner-cooled type.
and waxes; and (3) with hot water, to remove the remaining
5.1.4 Extraction Crucibles, of Alundum or fritted glass and
water-soluble materials.
of medium or fine porosity.
3.2 The alcohol extraction is necessary in analysis of woods
5.2 Filtering Crucibles—Alundum, porous porcelain, or
high in tannin; that is, oak, chestnut, redwood, etc. It has not
fritted-glass crucibles (all of fine porosity), or Gooch crucibles
been shown necessary in the more common pulpwoods, such
with a glass-fiber mat, are recommended for filtering the
as the various species of spruce, pine, fir, hemlock, poplar,
separated lignin. Glass crucibles cannot be used if the lignin is
to be ashed.
This test method is under the jurisdiction of ASTM Committee D7 on Wood
and is the direct responsibility of Subcommittee D07.01 on Fundamental Test 6. Reagents
Methods and Properties.
6.1 Ethylene-Toluene Solution—Mix 1.0 L absolute ethanol
Current edition approved April 10, 1996. Published June 1996. Originally
and 427 mL toluene. (Warning—Avoid inhalation of vapors
published as D 1106 – 50. Last previous edition D 1106 – 84 (1990).
For further information on this test method the following references may be
and contact with skin.)
consulted:
6.2 Sulfuric Acid (72 %)—Carefully pour 665 mL of
Bray, M. W., “Methods Used at the Forest Products Laboratory for the Chemical
H SO (sp gr 1.84) into about 300 mLof water, with vigorous
Analysis of Pulps and Pulpwoods,”PaperTradeJournal,Vol 87, No. 25, December 2 4
20, 1928, p. 29. stirring, and after cooling, dilute to 1 L. Standardize against
Ritter, G. J., Seborg, R. M., Mitchell, R. L., Industrial and Engineering
standard NaOH solution, using methyl orange indicator.Adjust
Chemistry, Analytical Edition, Vol 4, 1932, p. 202.
the H SO to a strength of 72 6 0.1 % by addition of water or
2 4
Ritter, G. J., and Barbour, J. H., Industrial and Engineering Chemistry,
H SO (sp gr 1.84) as may be found necessary. If desired, the
Analytical Edition, Vol 7, 1935, p. 238. 2 4
Annual Book of ASTM Standards, Vol 04.10.
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D1106
solution may be standardized b
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