ASTM D2364-15(2021)

Standard Test Methods for Hydroxyethylcellulose

SIGNIFICANCE AND USE
5.1 The results of this test are used for calculating the total solids in the sample; and, by common usage, all materials volatile at this test temperature are designated as moisture.  
5.2 Moisture analysis (along with sulfated ash) is a measure of the amount of active polymer in the material and must be considered when determining the amount of hydroxyethyl cellulose to use in various formulations.
SCOPE
1.1 These test methods cover the testing of hydroxyethylcellulose.  
1.2 The test procedures appear in the following order:    
Sections  
Moisture  
4 – 9  
Ash  
10 – 17  
Viscosity  
18 – 23    
Density  
24 – 30  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.4 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.  
1.5 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-May-2021
• ICS: 85.040 - Pulps
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Refers: ASTM D4794-94(2009) - Standard Test Method for Determination of Ethoxyl or Hydroxyethoxyl Substitution in Cellulose Ether Products by Gas Chromatography
• Effective Date: 01-Feb-2009
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D4794-94(2003) - Standard Test Method for Determination of Ethoxyl or Hydroxyethoxyl Substitution in Cellulose Ether Products by Gas Chromatography
• Effective Date: 01-Oct-2003
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM D2364-15(2021), "Standard Test Methods for Hydroxyethylcellulose," is an internationally recognized standard published by ASTM International. This standard specifies test methods for analyzing hydroxyethylcellulose (HEC), a widely used cellulose ether polymer. The procedures outlined enable laboratories and manufacturers to accurately determine critical properties such as moisture content, ash (sulfate) content, viscosity, and density of HEC samples. Ensuring consistent quality and correct formulation of hydroxyethylcellulose is essential across industries including pharmaceuticals, personal care, coatings, and construction.

ASTM D2364-15(2021) aligns with the World Trade Organization Technical Barriers to Trade (TBT) Committee’s principles for developing international standards, supporting global trade and regulatory compliance.

Key Topics

• Moisture Content: Determines volatile materials in HEC, which are commonly classified as moisture. Accurate results are critical for calculating total solids in the sample.
• Sulfated Ash Content: Measures inorganic residue after burning the sample. Alongside moisture, ash analysis indicates the amount of active polymer present.
• Viscosity: Evaluates the thickening ability of aqueous hydroxyethylcellulose solutions, a key functional property for many formulation applications.
• Density: Assesses the bulk density of HEC powders, relating to handling, packaging, dissolution, and storage considerations.
• Precision and Bias: The standard provides guidelines on the expected repeatability and reproducibility for each test, fostering reliable quality control.

Applications

Implementing ASTM D2364-15(2021) delivers practical benefits in various scenarios:

• Quality Control: Used by manufacturers and processors of hydroxyethylcellulose to ensure batch-to-batch consistency and adherence to product specifications.
• Formulation Development: Moisture and ash analysis help formulators determine the actual amount of active polymer needed for optimal product performance, resulting in cost-efficient and reliable formulations.
• Regulatory Compliance: Supports compliance with industry regulations and international trade requirements by providing demonstrable, standardized data on hydroxyethylcellulose properties.
• Research and Development: Provides a benchmark for evaluating new HEC grades or comparing different suppliers.
• Supply Chain Confidence: Facilitates transparent quality communication between suppliers and customers, reducing risks associated with ingredient variability.
• Product Labeling: Data from these test methods support accurate product labeling and documentation required for safety and regulatory submissions.

Related Standards

Professionals utilizing ASTM D2364-15(2021) may also reference the following standards to support a comprehensive analysis of cellulose ether products:

• ASTM D1193: Specification for Reagent Water, essential for preparing test solutions.
• ASTM D4794: Test Method for Determination of Ethoxyl or Hydroxyethoxyl Substitution in Cellulose Ether Products by Gas Chromatography.
• ISO and other ASTM standards on polymers, viscosity measurement, and bulk density determination complement these test methods.
• Good Laboratory Practice (GLP) and relevant safety and environmental standards should be considered to ensure safe and responsible testing.

Summary

ASTM D2364-15(2021) provides essential standardized methods for characterizing hydroxyethylcellulose, supporting quality assurance, regulatory compliance, and optimal product performance in diverse industries. By following these procedures, organizations can confidently assess key properties-moisture, ash, viscosity, and density-ensuring the reliable use of hydroxyethylcellulose in modern formulations.

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: D2364 − 15 (Reapproved 2021)
Standard Test Methods for
Hydroxyethylcellulose
This standard is issued under the fixed designation D2364; 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 conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
1.1 These test methods cover the testing of hydroxyethyl-
specifications are available. Other grades may be used, pro-
cellulose.
vided it is first ascertained that the reagent is of sufficiently
1.2 The test procedures appear in the following order:
high purity to permit its use without lessening the accuracy of
Sections
the determination.
Moisture 4–9
Ash 10–17 3.2 Unless otherwise indicated, reference to water shall be
Viscosity 18–23
understood to mean reagent water, conforming to Specification
Density 24–30
D1193.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information MOISTURE
only.
4. Scope
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.1 Thistestmethodcoversthedeterminationofthevolatile
responsibility of the user of this standard to establish appro-
content of hydroxyethylcellulose.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 5. Significance and Use
1.5 This international standard was developed in accor-
5.1 The results of this test are used for calculating the total
dance with internationally recognized principles on standard-
solids in the sample; and, by common usage, all materials
ization established in the Decision on Principles for the
volatile at this test temperature are designated as moisture.
Development of International Standards, Guides and Recom-
5.2 Moisture analysis (along with sulfated ash) is a measure
mendations issued by the World Trade Organization Technical
of the amount of active polymer in the material and must be
Barriers to Trade (TBT) Committee.
considered when determining the amount of hydroxyethyl
cellulose to use in various formulations.
2. Referenced Documents
2.1 ASTM Standards:
6. Apparatus
D1193 Specification for Reagent Water
6.1 Oven, gravity-convection, capable of maintaining a
D4794 Test Method for Determination of Ethoxyl or Hy-
temperature of 105 6 3°C.
droxyethoxyl Substitution in Cellulose Ether Products by
Gas Chromatography
6.2 Weighing Bottles, low-form, 50 mm in inside diameter
by 30 mm in height, or equivalent.
3. Purity of Reagents
6.3 Analytical Balance.
3.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
7. Procedure
7.1 Weigh5gofsampletothenearest0.001ginataredand
These test methods are under the jurisdiction of ASTM Committee D01 on covered weighing bottle.
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved June 1, 2021. Published June 2021. Originally
approved in 1965. Last previous edition approved in 2015 as D2364 – 15. DOI: ACS Reagent Chemicals, Specifications and Procedures for Reagents and
10.1520/D2364-15R21. Standard-Grade Reference Materials, American Chemical Society, Washington,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2364 − 15 (2021)
7.2 Place it in an oven at 105°C for 2 h with the cover 15.4 Remove the dish, allow to cool somewhat, place in a
removed. Replace the cover, cool in a desiccator, and weigh. desiccator, and cool to room temperature. Weigh the dish and
residue to the nearest 0.0001 g.
8. Calculation
16. Calculation
8.1 Calculate the percent moisture, M, as follows:
16.1 Calculate the percent of ash (as sulfate), C, as follows:
M 5 A/B 3100 (1)
~ !
C 5 A/B 3100 (2)
~ !
where:
where:
A = mass loss on heating, g, and
B = sample used, g. A = ash, g, and
B = sample used, g.
9. Precision and Bias
17. Precision and Bias
9.1 Statistical analysis of intralaboratory (repeatability) test
17.1 Statistical analysis of interlaboratory (reproducibility)
results on samples containing from about 3.5 % moisture
test results on samples containing 2 to 5 % ash (as sulfate)
indicate a precision of 60.5 % absolute at the 95 % confidence
indicates a precision of 60.3 % absolute at the 95 % level.
level.
17.2 No statement on bias can be made as no suitable
9.2 No statement on bias can be made as no suitable
reference material is available as a standard.
reference material is available as a standard.
VISCOSITY
ASH—AS SULFATE
18. Scope
10. Scope
18.1 This test method is an arbitrary method of determining
10.1 This test method covers the determination of the
the viscosity of aqueous solutions of hydroxyethylcellulose in
residue on ignition of hydroxyethylcellulose after a specimen
the viscosity range from 10 to 10 000 mPa·s (cP) at 25°C.
has been treated with sulfuric acid.
18.2 The concentration to be used for the test shall be
11. Summary of Test Method
agreed upon between the purchaser and the seller. It shall be
such that the viscosity of the solution will fall within the range
11.1 Aspecimen is moistened with sulfuric acid, the excess
of this test.
acid evaporated, the carbonaceous matter burned off, and the
residue ignited in a muffle furnace, cooled, and weighed.
18.3 The results for the viscosity of hydroxyethylcellulose
by this test method will not necessarily agree with results from
12. Significance and Use
other types of instruments used for viscosity measurements.
12.1 Excessive ash can affect solution clarity and film
18.4 The determinations are run on a calculated dry basis;
properties. The ash (along with moisture) is a measure of the
that is, the amount of hydroxyethylcellulose required for the
amount of active polymer in the material and must be consid-
desired concentration on a dry basis is calculated from the
eredwhendeterminingtheamountofhydroxyethylcelluloseto
known moisture content.
use in various formulations.
19. Significance and Use
13. Apparatus
19.1 This test method is intended for referee purposes.
13.1 Dishes, platinum, 50 to 75-mL capacity.
19.2 This test method determines the relative ability of the
13.2 Muffle Furnace, maintained at 825 6 25°C.
polymertothickenaqueoussolutionsandisthereforerelatedto
the concentration required in various formulations to achieve
14. Reagents
the desired finished product viscosity.
14.1 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
20. Apparatus
(H SO ).
2 4
20.1 Viscometer, Coaxial Rotational—The essential instru-
15. Procedure
mentation required providing the minimum rotational viscom-
eter analytical capabilities for this method include:
15.1 Weigh, to the nearest 0.0001 g, about2gofthe dried
sample into a tared platinum dish. Moisten the entire specimen
NOTE 1—Manufacturers of cellulose derivatives usually specify the
viscometer make, model, spindle, and speed to be used with their
with about 2 mL of H SO . Then cautiously heat over a small
2 4
products. It is highly recommended that these specifications be followed.
flame until sulfur trioxide (SO ) fumes cease to be evolved.
Use of a viscometer made by another company or even a different model
15.2 Increase the heat, ignite the specim
...