ASTM D1166-21

Standard Test Method for Methoxyl Groups in Wood and Related Materials

SIGNIFICANCE AND USE
3.1 Most of the methoxyl in wood is attributable to the lignin. This test method is used extensively in the study of lignin.
SCOPE
1.1 This test method covers the determination of methoxyl groups in wood and related materials (1-7).2 The test method is applicable to milled wood or sawdust, or by suitable adjustment in size of the test specimen, to fractions isolated from wood and lignin.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.  
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Mar-2021
• ICS: 79.040 - Wood, sawlogs and sawn timber
• ICS: 79.060.01 - Wood-based panels in general
• Technical Committee: D07 - Wood
• Drafting Committee: D07.01 - Fundamental Test Methods and Properties

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D1166 − 21
Standard Test Method for
1
Methoxyl Groups in Wood and Related Materials
This standard is issued under the fixed designation D1166; 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 3. Significance and Use
3.1 Most of the methoxyl in wood is attributable to the
1.1 This test method covers the determination of methoxyl
2
lignin. This test method is used extensively in the study of
groups in wood and related materials (1-7). The test method is
lignin.
applicable to milled wood or sawdust, or by suitable adjust-
ment in size of the test specimen, to fractions isolated from
4. Apparatus
wood and lignin.
4.1 The apparatus shall be similar to that illustrated in Fig.
1.2 This standard does not purport to address all of the
1 and shall consist of the following:
safety concerns, if any, associated with its use. It is the
4.1.1 Reaction Flask,
responsibility of the user of this standard to establish appro-
4.1.2 Heat Source—A temperature controlled heating
priate safety, health, and environmental practices and deter-
mantle,
mine the applicability of regulatory limitations prior to use.
4.1.3 Vertical Air-Cooled Condenser,
Specific precautionary statements are given in Section 6.
4.1.4 Scrubber, and
1.3 This international standard was developed in accor-
4.1.5 Two Absorption Vessels.
dance with internationally recognized principles on standard-
5. Purity of Reagents and Water
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5.1 Purity of Reagents—Reagent grade chemicals shall be
mendations issued by the World Trade Organization Technical
used in all tests. Unless otherwise indicated, it is intended that
Barriers to Trade (TBT) Committee.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
3
2. Principle of Method
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
2.1 Theprincipleofthetestmethodisthesameasthatinthe
sufficiently high purity to permit its use without lessening the
original method of Zeisel (1), except that the methyl iodide is
accuracy of the determination.
collected in an acetic acid solution of potassium acetate
containing bromine. The following reactions then occur:
5.2 Water—Unless otherwise indicated, references to water
shall be understood to mean distilled water.
CH I1Br →CH Br1IBr (1)
3 2 3
6. Reagents
IBr12Br 13H O→HIO 15HBr
2 2 3
6.1 Hydroiodic Acid (HI) (57 % in water sp gr 1.70)—This
The iodic acid is determined by titration of iodine liberated
best reagent grade HI, should be stored in the absence of light
by the reaction:
and at a low temperature to keep its purity.
HIO 15HI→3I 13H O (2)
3 2 2
6.2 Phenol.
From the above equations, it follows that one methoxyl
6.3 Cadmium Sulfate Solution (50 g CdSO /L)—Dissolve
4
group (CH O) liberates six atoms of iodine.
3 67.2 g of CdSO ·4H O in water and dilute to 1 L.
4 2
NOTE 1—A water suspension of red phosphorus is equally satisfactory
in the scrubber.
1
This test method is under the jurisdiction of ASTM Committee D07 on Wood
and is the direct responsibility of Subcommittee D07.01 on Fundamental Test
3
Methods and Properties. Reagent Chemicals, American Chemical Society Specifications , American
Current edition approved April 1, 2021. Published April 2021. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
approved in 1956. Last previous edition approved in 2013 as D1166 – 84 (2013). listed by the American Chemical Society, see Analar Standards for Laboratory
DOI: 10.1520/D1166-21. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
2
The boldface numbers in parentheses refer to the references listed at the end of and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
this test method. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D1166 − 21
solution should be prepared.
6.11 Sulfuric Acid (1 + 9) —Mix one volume of H SO (sp
2 4
gr 1.84) with nine volumes of water.
6.12 Standard Sodium Thiosulfate Solution (0.1 N)—
Dissolve 25 g of Na S O ·5H O in 200 mL of water and
2 2 3 2
dilute to 1 L. Use freshly boiled and cooled water. It is
pr
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1166 − 84 (Reapproved 2013) D1166 − 21
Standard Test Method for
1
Methoxyl Groups in Wood and Related Materials
This standard is issued under the fixed designation D1166; 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
2
1.1 This test method covers the determination of methoxyl groups in wood and related materials (1-7). The test method is
applicable to wood sawdust and, milled wood or sawdust, or by suitable adjustment in size of the test specimen, to fractions
isolated from wood and lignin.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Principle of Method
2.1 The principle of the test method is the same as that in the original method of Zeisel (1), except that the methyl iodide is
collected in an acetic acid solution of potassium acetate containing bromine. The following reactions then occur:
CH I1Br →CH Br1IBr (1)
3 2 3
IBr12Br 13H O→HIO 15HBr
2 2 3
The iodic acid is determined by titration of iodine liberated by the reaction:
HIO 15HI→3I 13H O (2)
3 2 2
From the above equations, it follows that one methoxyl group (CH O) liberates six atoms of iodine.
3
3. Significance and Use
3.1 Most of the methoxyl in wood is attributable to the lignin. This test method is used extensively in the study of lignin.
4. Apparatus
4.1 The apparatus shall be similar to that illustrated in Fig. 1 and shall consist of the following:
4.1.1 Reaction Flask,
1
This test method is under the jurisdiction of ASTM Committee D07 on Wood and is the direct responsibility of Subcommittee D07.01 on Fundamental Test Methods
and Properties.
Current edition approved Aug. 1, 2013April 1, 2021. Published August 2013April 2021. Originally approved in 1956. Last previous edition approved in 20072013 as
D1166 – 84 (2007).(2013). DOI: 10.1520/D1166-84R13.10.1520/D1166-21.
2
The boldface numbers in parentheses refer to the references listed at the end of this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D1166 − 21
FIG. 1 Apparatus for Methoxyl Determination
4.1.2 Heat Source—A microburner, provided with a cylindrical shield to eliminate the effect of air drafts,temperature controlled
heating mantle,
4.1.3 Vertical Air-Cooled Condenser,
4.1.4 Scrubber, and
4.1.5 Two Absorption Vessels.
5. Purity of Reagents and Water
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
3
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
5.2 Water—Unless otherwise indicated, references to water shall be understood to mean distilled water.
3
Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
2

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D1166 − 21
6. Reagents
6.1 Hydriodic Acid (sp Hydroiodic Acid (HI) (57 % in water sp gr 1.70)—TheThis best reagent grade HI, if should be stored in
the absence of light and at a low temperature, may be used without redistillation. If purification is neces
...