ASTM D4794-94(2017)

Standard Test Method for Determination of Ethoxyl or Hydroxyethoxyl Substitution in Cellulose Ether Products by Gas Chromatography

ABSTRACT
This test method is applicable to the determination of ethoxyl or hydroxyethoxyl substitution in cellulose ether products by a Zeisel gas chromatographic technique. The equipment and materials to be used shall include reagents, gas chromatograph, electronic integrator, column, syringe, reaction vials, caps, heating block, and a cover. The following reagents are as follows: iodoethane, O-xylene, toluene, hydrochloric acid, and colume packing. When a cellulose ether containing ethyl or hydroxyethyl substitutes is allowed to react with hydriodic acid, one mole of iodoethane is liberated for each mole of ethoxyl or hydroxyethoxyl ether substituted on the cellulose chain. The iodoethane is extracted in-situ with o-xylene and quantitated by gas chromatography using an internal standard technique. It is recommended to run duplicate samples.
SCOPE
1.1 This test method is applicable to the determination of ethoxyl or hydroxyethoxyl substitution in cellulose ether products by a Zeisel gas chromatographic technique.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5 and Note 3.  
1.4 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: Historical
• Publication Date: 30-Nov-2017
• ICS: 71.080.60 - Alcohols. Ethers
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4794 − 94 (Reapproved 2017)
Standard Test Method for
Determination of Ethoxyl or Hydroxyethoxyl Substitution in
1
Cellulose Ether Products by Gas Chromatography
This standard is issued under the fixed designation D4794; 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 3.3 Column—stainless steel, 1829 mm in length, 3.2 mm in
outside diameter, packed with the reagent in 4.6, coiled to fit
1.1 This test method is applicable to the determination of
the chromatograph used; or equivalent column and packing as
ethoxyl or hydroxyethoxyl substitution in cellulose ether prod-
appropriate.
ucts by a Zeisel gas chromatographic technique.
3.4 Syringe, 10 µL.
1.2 The values stated in SI units are to be regarded as
2
standard. No other units of measurement are included in this
3.5 Reaction Vials, Caps, and Heating Block.
standard.
3.6 Syringe,100µL.
1.3 This standard does not purport to address all of the
3.7 Cover, stainless steel, fabricated to cover the heating
safety concerns, if any, associated with its use. It is the
block.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Reagents and Materials
mine the applicability of regulatory limitations prior to use.
For specific hazard statements, see Section 5 and Note 3.
4.1 Purity of Reagents—Reagent grade chemicals shall be
1.4 This international standard was developed in accor-
used in all tests. Unless otherwise indicated, it is intended that
dance with internationally recognized principles on standard-
all reagents shall conform to the specifications of the Commit-
ization established in the Decision on Principles for the
tee onAnalytical Reagents of theAmerican Chemical Society,
3
Development of International Standards, Guides and Recom-
where such specifications are available. Other grades may be
mendations issued by the World Trade Organization Technical
used, provided it is first ascertained that the reagent is of
Barriers to Trade (TBT) Committee.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
2. Summary of Test Method
4.2 Iodoethane, 99 % minimum.
2.1 When a cellulose ether containing ethyl or hydroxyethyl
4.3 O-xylene.
substitutes is allowed to react with hydriodic acid, one mole of
iodoethane is liberated for each mole of ethoxyl or hydroxy-
4.4 Toluene.
ethoxyl ether substituted on the cellulose chain. The iodoeth-
4.5 Hydriodic Acid, 57 % (sp gr 1.69 to 1.70).
ane is extracted in situ with o-xylene and quantitated by gas
chromatography using an internal standard technique. It is
4.6 Column Packing, 10 % methyl silicone stationary phase
recommended to run duplicate samples.
USP code [G1] coated on inert diatomite solid support USP
code [S1A], 100/120 mesh.
3. Apparatus
3.1 Gas Chromatograph with thermal conductivity detector
2
and heated injection port.
The sole source of supply of a heating block, Silli-Therm Heating Module,
Reacti-Block 21, Reacti-Vials, and Minnert valve tops, known to the committee at
3.2 Electronic Integrator.
this time is the Pierce Chemical Company P.O. Box 117, Rockford, IL61105–9976.
If you are aware of alternative suppliers, please provide this information to ASTM
International Headquarters. Your comments will receive careful consideration at a
1
meeting of the responsible technical committee, which you may attend.
1 3
This test method is under the jurisdiction of ASTM Committee D01 on Paint Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, andApplications and is the direct responsibility of Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Subcommittee D01.36 on Cellulose and Cellulose Derivatives. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Dec. 1, 2017. Published December 2017. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1988. Last previous edition approved in 2009 as D4794 – 94 (2009). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D4794-94R17. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4794 − 94 (2017)
5. Hazards 8.1.1 Calibrate the integrator according to the manufactur-
er’s instructions.
5.1 Safety precautions must be taken for handling of hydri-
odic acid. 8.2 If an integrator is not available peak a
...

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: D4794 − 94 (Reapproved 2009) D4794 − 94 (Reapproved 2017)
Standard Test Method for
Determination of Ethoxyl or Hydroxyethoxyl Substitution in
1
Cellulose Ether Products by Gas Chromatography
This standard is issued under the fixed designation D4794; 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
1.1 This test method is applicable to the determination of ethoxyl or hydroxyethoxyl substitution in cellulose ether products by
a Zeisel gas chromatographic technique.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5 and Note 3.
1.4 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. Summary of Test Method
2.1 When a cellulose ether containing ethyl or hydroxyethyl substitutes is allowed to react with hydriodic acid, one mole of
iodoethane is liberated for each mole of ethoxyl or hydroxyethoxyl ether substituted on the cellulose chain. The iodoethane is
extracted in situ with o-xyleneo-xylene and quantitated by gas chromatography using an internal standard technique. It is
recommended to run duplicate samples.
3. Apparatus
3.1 Gas Chromatograph with thermal conductivity detector and heated injection port.
3.2 Electronic Integrator.
3.3 Column—stainless steel, 1829 mm in length, 3.2 mm in outside diameter, packed with the reagent in 4.6, coiled to fit the
chromatograph used; or equivalent column and packing as appropriate.
3.4 Syringe, 10 μL.
2
3.5 Reaction Vials, Caps, and Heating Block.
3.6 Syringe, 100 μ L.
3.7 Cover, stainless steel, fabricated to cover the heating block.
4. Reagents and Materials
4.1 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.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved Feb. 1, 2009Dec. 1, 2017. Published February 2009December 2017. Originally approved in 1988. Last previous edition approved in 20032009
as D4794 – 94 (2003).(2009). DOI: 10.1520/D4794-94R09.10.1520/D4794-94R17.
2
The sole source of supply of a heating block, Silli-Therm Heating Module, Reacti-Block 21, Reacti-Vials, and Minnert valve tops, known to the committee at this time
is the Pierce Chemical Company P.O. Box 117, Rockford, IL 61105–9976. If you are aware of alternative suppliers, please provide this information to ASTM International
1
Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.
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. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4794 − 94 (2017)
4.2 Iodoethane, 99 % minimum.
4.3 O-xylene.
4.4 Toluene.
4.5 Hydriodic Acid,
...