ASTM D4794-94(2009)
(Test Method)Standard Test Method for Determination of Ethoxyl or Hydroxyethoxyl Substitution in Cellulose Ether Products by Gas Chromatography
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 5 and Note 3.
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Designation: D4794 − 94 (Reapproved 2009)
Standard Test Method for
Determination of Ethoxyl or Hydroxyethoxyl Substitution in
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 3.5 Reaction Vials, Caps, and Heating Block.
3.6 Syringe,100µL.
1.1 This test method is applicable to the determination of
ethoxyl or hydroxyethoxyl substitution in cellulose ether prod-
3.7 Cover, stainless steel, fabricated to cover the heating
ucts by a Zeisel gas chromatographic technique.
block.
1.2 The values stated in SI units are to be regarded as
4. Reagents and Materials
standard. No other units of measurement are included in this
standard.
4.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
1.3 This standard does not purport to address all of the
all reagents shall conform to the specifications of the Commit-
safety concerns, if any, associated with its use. It is the
tee onAnalytical Reagents of theAmerican Chemical Society,
responsibility of the user of this standard to establish appro-
where such specifications are available. Other grades may be
priate safety and health practices and determine the applica-
used, provided it is first ascertained that the reagent is of
bility of regulatory limitations prior to use. For specific hazard
sufficiently high purity to permit its use without lessening the
statements, see Section 5 and Note 3.
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
4.4 Toluene.
iodoethane is liberated for each mole of ethoxyl or hydroxy-
4.5 Hydriodic Acid, 57 % (sp gr 1.69 to 1.70).
ethoxyl ether substituted on the cellulose chain. The iodoeth-
ane is extracted in situ with o-xylene and quantitated by gas
4.6 Column Packing, 10 % methyl silicone stationary phase
chromatography using an internal standard technique. It is
USP code [G1] coated on inert diatomite solid support USP
recommended to run duplicate samples.
code [S1A], 100/120 mesh.
3. Apparatus
5. Hazards
3.1 Gas Chromatograph with thermal conductivity detector
5.1 Safety precautions must be taken for handling of hydri-
and heated injection port.
odic acid.
3.2 Electronic Integrator.
5.2 During the reaction, the glass vials are under pressure.
Exercise precaution in handling the hot vials.
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.
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
3.4 Syringe, 10 µL.
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
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 Feb. 1, 2009. Published February 2009. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1988. Last previous edition approved in 2003 as D4794 – 94 (2003). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D4794-94R09. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4794 − 94 (2009)
6. Apparatus Preparation and Conditioning where:
RF = response factor,
6.1 Column (Note 1)—Columns are packed with reagent
A = peak height of internal standard (toluene),
under vacuum and mechanical vibration using silanized glass
w = weight of iodoethane, g,
wool to contain the packing. Install each in the gas chromato-
P = purity of iodoethane,
graph to facilitate on column injection. Condition the column
F =
at 200°C for 12 h, then allow it to come to equilibrium under factor of 0.289 for ethoxyl , 0.391 for
S D
the conditions described below:
hydroxyethoxyl,
Oven temperature, °C 130 isothermal
0.05 = weight of toluene, g,
Injection port temperature, °C 200
B = peak height of iodoethane, and
Detector temperature, °C 250
P = purity of
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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(Reapproved2003) Designation:D4794–94(Reapproved2009)
Standard Test Method for
Determination of Ethoxyl or Hydroxyethoxyl Substitution in
Cellulose Ether Products by Gas Chromatography
This standard is issued under the fixed designation D 4794; 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.
1.2The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. For specific hazard statements, see Section 5 and Note 3.
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 in situ with o-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,10µL.
3.5 Reaction Vials, Caps, and Heating Block.
3.6 Syringe,100µL.
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
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.
4.2 Iodoethane, 99 % minimum.
4.3 O-xylene.
4.4 Toluene.
4.5 Hydriodic Acid, 57 % (sp gr 1.69 to 1.70).
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 Oct.Feb. 1, 2003.2009. Published October 2003.February 2009. Originally approved in 1988. Last previous edition approved in 19942003 as
D4794–94(1998). D 4794 – 94 (2003).
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
Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.
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.
D4794–94 (2009)
4.6 Column Packing, 10 % methyl silicone stationary phase USP code [G1] coated on inert diatomite solid support USP code
[S1A], 100/120 mesh.
5. Hazards
5.1 Safety precautions must be taken for handling of hydriodic acid.
5.2 During the reaction, the glass vials are under pressure. Exercise precaution in handling the hot vials.
6. Apparatus Preparation and Conditioning
6.1 Column (Note 1) —Columns are packed with reagent under vacuum and mechanical vibration using silanized glass wool
to contain the packing. Install each in the gas chromatograph to facilitate on column injection. Condition the column at 200°C for
12 h, then allow it to come to equilibrium under the conditions described below:
Oven temperature, °C 130 isothermal
Injection port temperature, °C 200
Detector tem
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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(Reapproved2003) Designation:D4794–94(Reapproved2009)
Standard Test Method for
Determination of Ethoxyl or Hydroxyethoxyl Substitution in
Cellulose Ether Products by Gas Chromatography
This standard is issued under the fixed designation D 4794; 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.
1.2The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. For specific hazard statements, see Section 5 and Note 3.
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 in situ with o-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,10µL.
3.5 Reaction Vials, Caps, and Heating Block.
3.6 Syringe,100µL.
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
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.
4.2 Iodoethane, 99 % minimum.
4.3 O-xylene.
4.4 Toluene.
4.5 Hydriodic Acid, 57 % (sp gr 1.69 to 1.70).
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 Oct.Feb. 1, 2003.2009. Published October 2003.February 2009. Originally approved in 1988. Last previous edition approved in 19942003 as
D4794–94(1998). D 4794 – 94 (2003).
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
Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.
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.
D4794–94 (2009)
4.6 Column Packing, 10 % methyl silicone stationary phase USP code [G1] coated on inert diatomite solid support USP code
[S1A], 100/120 mesh.
5. Hazards
5.1 Safety precautions must be taken for handling of hydriodic acid.
5.2 During the reaction, the glass vials are under pressure. Exercise precaution in handling the hot vials.
6. Apparatus Preparation and Conditioning
6.1 Column (Note 1) —Columns are packed with reagent under vacuum and mechanical vibration using silanized glass wool
to contain the packing. Install each in the gas chromatograph to facilitate on column injection. Condition the column at 200°C for
12 h, then allow it to come to equilibrium under the conditions described below:
Oven temperature, °C 130 isothermal
Injection port temperature, °C 200
Detector tem
...
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