ASTM D3876-96

Standard Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography

SCOPE
1.1 This test method is applicable to the determination of methoxyl and hydroxypropyl substitution content in cellulose ether products by a Zeisel-gas chromatographic technique.
1.2 This test method is not suitable for use for the analysis of hydroxypropyl-cellulose due to its very high substitution level.  
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. For specific hazard statements, see Sections 2, 11.1.4 and 11.1.7.

General Information

• Status: Historical
• Publication Date: 31-Dec-2000
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaced By: ASTM D3876-96(2001) - Standard Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography
• Effective Date: 01-Jan-2001
• Referred By: ASTM D5400-15(2021) - Standard Test Methods for Hydroxypropylcellulose
• Effective Date: 01-Jan-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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.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 3876 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Methoxyl and Hydroxypropyl Substitution in Cellulose Ether
Products by Gas Chromatography
This standard is issued under the fixed designation D 3876; 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 4.2 Electronic Integrator
4.3 Stainless Steel Tubing, 9.5 mm in outside diameter and
1.1 This test method is applicable to the determination of
1981 mm in length, packed with reagent in 5.8.
methoxyl and hydroxypropyl substitution content in cellulose
4.4 Syringes, 10 and 100 μL.
ether products by a Zeisel-gas chromatographic technique.
4.5 Reaction Vials, Caps, and Heating Block.
1.2 This test method is not suitable for use for the analysis
of hydroxypropyl-cellulose due to its very high substitution
5. Reagents
level.
5.1 Purity of Reagents—Reagent grade chemicals shall be
1.3 This standard does not purport to address all of the
used in all tests. Unless otherwise indicated, it is intended that
safety concerns, if any, associated with its use. It is the
all reagents shall conform to the specifications of the Commit-
responsibility of the user of this standard to establish appro-
tee on Analytical Reagents of the American Chemical Society,
priate safety and health practices and determine the applica-
where such specifications are available. Other grades may be
bility of regulatory limitations prior to use. For specific hazard
2 used, provided it is first ascertained that the reagent is of
statements, see Section 2 and Note 2 and Note 3.
sufficiently high purity to permit its use without lessening the
2. Summary of Test Method accuracy of the determination.
5.2 o-Xylene, ACS.
2.1 When methyl cellulose or hydroxypropyl methyl cellu-
5.3 Toluene, ACS.
lose is reacted with hydriodic acid, 1 mol of methyl iodide and
5.4 Iodomethane, 99% min.
1 mol of isopropyl iodide are liberated for each mole of
5.5 2-Iodopropane, 97% min.
methoxyl and hydroxypropoxyl that is substituted on the
5.6 Hydriodic Acid (sp. gr. 1.69 to 1.70) 57%.
cellulose chain. The methyl iodide and isopropyl iodide are
5.7 Acetone.
extracted in situ with o-xylene and quantitated by gas chroma-
5.8 Packing Material.
tography using an internal standard technique.
6. Hazards
3. Significance and Use
6.1 Safety precautions must be taken for handling of hydri-
3.1 This test method determines the methoxyl and hydrox-
odic acid.
ypropoxyl content of cellulose ethers by a Zeisel-gas chro-
6.2 During the reaction, the glass vials are under pressure.
matographic technique.
Exercise caution in handling the hot vials.
3.2 Substitution levels affect solution properties, rheology,
viscosity, and many other properties of the polymer.
4. Apparatus
3 Hewlett-Packard Model 3380 has been found satisfactory for this purpose.
4.1 Gas Chromatograph, with thermal conductivity detec-
Tubing from Supelco, Inc., Supelco Park, Bellefonte, PA 16823 has been found
tor and heated injection port.
satisfactory for this purpose.
Reacti-therm Heating module, Reacti-Block Reacti-vials and Mininert valve
tops from Pierce Chemical Co., Box 117, Rockford, IL 61105 have been found
satisfactory for this purpose.
1 7
This test method is under the jurisdiction of ASTM Committee D-1 on Paint Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, and Applications 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 Jan. 10, 1996. Published March 1996. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
e1
published as D 3876 – 79. Last previous edition D 3876 – 79 (1989) . and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 06.03. MD.
3 8
Hewlett-Packard Model 5700, available from Hewlett-Packard, Route 41, Starr Columns packed with 10 % SP2100 on 100/120 Supelcoportt have been found
Rd, P.O. Box 900, Avondale, PA 19311, has been found satisfactory for this purpose. satisfactory for this purpose.
D 3876
mg toluene 5 internal standard solution concentrated 3 4 ml (3)
7. Sampling
7.1 A specific sampling method is currently under study by
10. Calibration of Electronic Integrator
the subcommittee.
10.1 Inject 1 μL of the upper layer of the prepared standard
8. Apparatus Preparation and Conditioning
solution (9.2) into the gas chromatograph and start the elec-
8.1 Install prepackaged columns in the chromatograph and tronic integrator.
condition them by heating to 150°C over 1 h and then holding 10.1.1 Calibrate in accordance with the manufacturer’s
at temperature for 16 h. Then set the chromatograph as instructions.
follows: 10.2 In the event an electronic integrator is not available the
peak areas can be measured manually and a factor determined
Oven temperature 130°C isothermal
Injection port temperature 200°C
for each component can be obtained using the following
Detector temperature 250°C
equation:
Detector curr
...