ASTM D3876-96(2001)

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
• ICS: 85.040 - Pulps
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaces: ASTM D3876-96 - Standard Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography
• Effective Date: 01-Jan-2001
• Replaced By: ASTM D3876-96(2007) - Standard Test Method for Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas Chromatography
• Effective Date: 01-Jun-2007
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D3876–96 (Reapproved 2001)
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 4.3 Stainless Steel Tubing, 9.5 mm in outside diameter and
1981 mm in length, packed with reagent in 5.8.
1.1 This test method is applicable to the determination of
4.4 Syringes, 10 and 100 µL.
methoxyl and hydroxypropyl substitution content in cellulose
4.5 Reaction Vials, Caps, and Heating Block.
ether products by a Zeisel-gas chromatographic technique.
1.2 This test method is not suitable for use for the analysis
5. Reagents
of hydroxypropyl-cellulose due to its very high substitution
5.1 Purity of Reagents—Reagent grade chemicals shall be
level.
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 Section2,11.1.4, and 11.1.7.
accuracy of the determination.
2. Summary of Test Method 5.2 o-Xylene, ACS.
5.3 Toluene, ACS.
2.1 When methyl cellulose or hydroxypropyl methyl cellu-
5.4 Iodomethane, 99% min.
lose is reacted with hydriodic acid, 1 mol of methyl iodide and
5.5 2-Iodopropane, 97% min.
1 mol of isopropyl iodide are liberated for each mole of
5.6 Hydriodic Acid (sp. gr. 1.69 to 1.70) 57%.
methoxyl and hydroxypropoxyl that is substituted on the
5.7 Acetone.
cellulose chain. The methyl iodide and isopropyl iodide are
5.8 Packing Material.
extracted in situ with o-xylene and quantitated by gas chroma-
tography using an internal standard technique.
6. Hazards
3. Significance and Use 6.1 Safety precautions must be taken for handling of hydri-
odic acid.
3.1 This test method determines the methoxyl and hydrox-
6.2 During the reaction, the glass vials are under pressure.
ypropoxyl content of cellulose ethers by a Zeisel-gas chro-
Exercise caution in handling the hot vials.
matographic technique.
3.2 Substitution levels affect solution properties, rheology,
7. Sampling
viscosity, and many other properties of the polymer.
7.1 A specific sampling method is currently under study by
4. Apparatus the subcommittee.
4.1 Gas Chromatograph, with thermal conductivity detec-
tor and heated injection port.
Tubing from Supelco, Inc., Supelco Park, Bellefonte, PA16823 has been found
satisfactory for this purpose.
4.2 Electronic Integrator
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.
This test method is under the jurisdiction of ASTM Committee D01 on Paint 6
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 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. Pharmacopeial Convention, Inc. (USPC), Rockville,
Hewlett-Packard Model 5700, available from Hewlett-Packard, Route 41, Starr
MD.
Rd, P.O. Box 900,Avondale, PA19311, has been found satisfactory for this purpose. 7
Columns packed with 10 % SP2100 on 100/120 Supelcoportt have been found
Hewlett-Packard Model 3380 has been found satisfactory for this purpose.
satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3876
8. Apparatus Preparation and Conditioning 10. Calibration of Electronic Integrator
8.1 Install prepackaged columns in the chromatograph and
10.1 Inject 1 µL of the upper layer of the prepared standard
condition them by heating to 150°C over 1 h and then holding
solution (9.2) into the gas chromatograph and start the elec-
at temperature for 16 h. Then set the chromatograph as
tronic integrator.
follows:
10.1.1 Calibrate in accordance with the manufacturer’s
Oven temperature 130°C isothermal instructions.
Injection port temperature 200°C
10.2 In the event an electronic integrator is not available the
Detector temperature 250°C
peak areas can be measured manually and a factor determined
Detector current 170 mA
Attenuation 1 for each component can be obtained using the following
Carrier gas helium
equation:
Column A 20 mL/min
Column B 20 mL/min A 3 B
F 5 (4)
C 3 D
NOTE 1—The conditions used here were determined to be optimum for
the column used. Optimum conditions should be determined for each
where:
column
...