ASTM D1106-96

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.

General Information

• Status: Historical
• Publication Date: 09-Apr-1996
• Technical Committee: D07 - Wood
• Drafting Committee: D07.01 - Fundamental Test Methods and Properties

Relations

• Replaced By: ASTM D1106-96(2001) - Standard Test Method for Acid-Insoluble Lignin in Wood
• Effective Date: 10-Sep-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 1106 – 96 Technical Association of Pulp and Paper Industry
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 woods the alcohol extraction be omitted unless it is desirable
for a special purpose. In analysis of woods not listed, the
1.1 This test method covers the determination of the
desirabilty of the alcohol extraction depends upon the purpose
acid-insoluble lignin content of wood.
of the analysis and the report should state whether or not
1.2 This standard does not purport to address all of the
alcohol extraction was used.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 Wood contains approximately 20 to 30 % lignin. Re-
bility of regulatory limitations prior to use. Specific precau-
moval of the lignin is the primary objective of pulping and
tionary statements are given in 6.1.1.
bleaching procedures. Determination of the lignin content
2. Referenced Documents provides information for the evaluation and application of
these processes.
2.1 ASTM Standards:
D 1107 Test Method for Alcohol-Benzene Solubility of
5. Apparatus
Wood
5.1 Extraction Apparatus—A compact form of Soxhlet
3. Principle of Method extraction apparatus, with ground-glass joints, is preferable.
The apparatus shall consist of the following items:
3.1 When wood is treated with strong acids the carbohy-
5.1.1 Soxhlet Extraction Flask, having a capacity of 250
drates are hydrolyzed, leaving an insoluble residue which is
mL.
determined as lignin. Since some of the wood extractives (oils,
5.1.2 Soxhlet Extraction Tube, 45 to 50 mm in inside
resins, fats, waxes, tannins, gums, and starch) would remain
diameter, having a capacity to the top of the siphon of
insoluble with the lignin, these are first removed by proper
approximately 100 mL and a siphon tube approximately 55
solvents. The 72 % sulfuric acid method for lignin contains two
mm in height. Extraction tubes of these dimensions siphon
and sometimes three preliminary extractive treatments,
more rapidly than extractors with higher siphon tubes.
namely: (1) with alcohol, to remove the catechol tannins; (2)
5.1.3 Condenser, of the Hopkins inner-cooled type.
with alcohol-benzene solution, to remove the resins, oils, fats
5.1.4 Extraction Crucibles, of Alundum or fritted glass and
and waxes; and (3) with hot water, to remove the remaining
of medium or fine porosity.
water-soluble materials.
5.2 Filtering Crucibles—Alundum, porous porcelain, or
3.2 The alcohol extraction is necessary in analysis of woods
fritted-glass crucibles (all of fine porosity), or Gooch crucibles
high in tannin; that is, oak, chestnut, redwood, etc. It has not
with a glass-fiber mat, are recommended for filtering the
been shown necessary in the more common pulpwoods, such
separated lignin. Glass crucibles cannot be used if the lignin is
as the various species of spruce, pine, fir, hemlock, poplar,
to be ashed.
birch, beech, and maple. It is recommended that for these
6. Reagents
This test method is under the jurisdiction of ASTM Committee D-7 on Wood
6.1 Ethylene-Toluene Solution—Mix 1.0 L absolute ethanol
and is the direct responsibility of Subcommittee D07.01 on Fundamental Test
and 427 mL toluene.
Methods and Properties.
Current edition approved April 10, 1996. Published June 1996. Originally
NOTE 1—: Caution—Avoid inhalation of vapors and contact with skin.
published as D 1106 – 50. Last previous edition D 1106 – 84 (1990).
For further information on this test method the following references may be 6.2 Sulfuric Acid (72 %)—Carefully pour 665 mL of H
consulted:
SO (sp gr 1.84) into about 300 mL of water, with vigorous
Bray, M. W., “Methods Used at the Forest Products Laboratory for the Chemical
stirring, and after cooling, dilute to 1 L. Standardize against
Analysis of Pulps and Pulpwoods,” Paper Trade Journal, Vol 87, No. 25, December
standard NaOH solution, using methyl orange indicator. Adjust
20, 1928, p. 29.
Ritter, G. J., Seborg, R. M., Mitchell, R. L., Industrial and Engineering
the H SO to a strength of 72 6 0.1 % by addition of water or
2 4
Chemistry, Analytical Edition, Vol 4, 1932, p. 202.
H SO (sp gr 1.84) as may be found necessary. If desired, the
2 4
Ritter, G. J., and Barbour, J. H., Industrial and Engineering Chemistry,
solution may be standardized by an accurate determination of
Analytical Edition, Vol 7, 1935, p. 238.
Annual Book of ASTM Standards, Vol 04.10. its specific gravity. For 72 % H SO the specific gravity at
2 4
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