ASTM D4301-05(2019)

Standard Test Method for Total Chlorine in Epoxy Resins and Compounds

SIGNIFICANCE AND USE
5.1 The presence of residual chlorine in epoxy resins is deleterious to final product properties. This test method has been found to be applicable to resins or ethers with chlorine contents ranging from 50 ppm to 35 % by weight. Other halogen compounds react with the reagent but are distinguished from chlorine by the final potentiometric titration. Epoxy and other functional groups will consume reagent but do not affect the results.
SCOPE
1.1 This test method describes a procedure for the determination of total chlorine in epoxy resins and glycidyl ethers.  
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 8.  
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: Published
• Publication Date: 30-Sep-2019
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.33 - Polymers and Resins

Relations

• Replaces: ASTM D4301-05(2013) - Standard Test Method for Total Chlorine in Epoxy Resins and Compounds
• Effective Date: 01-Oct-2019
• Refers: ASTM D6440-10(2018) - Standard Terminology Relating to Hydrocarbon Resins
• Effective Date: 01-Sep-2018
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM D6440-10 - Standard Terminology Relating to Hydrocarbon Resins
• Effective Date: 01-Dec-2010
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM E691-05 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2005
• Refers: ASTM D6440-05 - Standard Terminology Relating to Hydrocarbon Resins
• Effective Date: 01-Sep-2005
• Refers: ASTM D6440-01 - Standard Terminology Relating to Hydrocarbon Resins
• Effective Date: 10-Dec-2001
• Refers: ASTM D6440-00A - Standard Terminology Relating to Hydrocarbon Resins
• Effective Date: 10-Dec-2001
• Refers: ASTM E691-99 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 10-May-1999
• 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 D4301-05(2019) - Standard Test Method for Total Chlorine in Epoxy Resins and Compounds, developed by ASTM, provides a reliable procedure for determining the total chlorine content in epoxy resins and glycidyl ethers. Accurate measurement of residual chlorine is critical, as its presence can negatively affect the final properties and performance of epoxy-based materials. The method is suitable for chlorine concentrations ranging from 50 ppm up to 35% by weight, ensuring broad applicability across various resin types. By employing potentiometric titration, this standard distinguishes chlorine from other halogens and prevents interference from other functional groups present in epoxy materials.

Key Topics

• Chlorine Determination: The standard outlines a method using sodium biphenyl to convert organic-bound chlorine to chloride, followed by potentiometric titration with silver nitrate.
• Applicable Range: Suitable for analyzing chlorine concentrations ranging from 50 parts per million to 35% by weight, making it versatile for both low and high chlorine content materials.
• Specificity: While other halogen compounds may react with the reagent, the final titration step ensures specific measurement of chlorine only.
• Interference Management: Functional groups inherent to epoxy and similar compounds do not impact the accuracy of chlorine determination.
• Safety Guidance: The standard emphasizes following appropriate laboratory safety, health, and environmental protocols, and refers to OSHA and other regulatory standards for handling chemicals and reagents.

Applications

ASTM D4301-05(2019) is widely used in industries where epoxy resins and glycidyl ethers play a central role, such as:

• Paints and Coatings: Ensuring that residual chlorine does not impair adhesion, color stability, or weathering properties.
• Electronics: Verifying low chlorine content in epoxy encapsulants and laminates, reducing the risk of corrosion and improving product reliability.
• Adhesives and Sealants: Supporting the formulation of high-performance adhesives with predictable mechanical and chemical characteristics.
• Quality Control: Assisting resin manufacturers and compounders in monitoring process contamination and confirming compliance with customer and regulatory requirements.

By implementing this test method, organizations can guarantee that their epoxy products meet stringent quality and performance standards, ultimately reducing product failures linked to chlorine contamination.

Related Standards

To ensure comprehensive testing and quality management, the following ASTM standards and referenced documents are commonly used in conjunction with ASTM D4301-05(2019):

• ASTM D1193: Specification for Reagent Water - defines water purity necessary for accurate chemical analysis.
• ASTM D6440: Terminology Relating to Hydrocarbon Resins - offers definitions key to resin testing.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method - supports validation and reproducibility assessments.
• Relevant OSHA Regulations: Including 29 CFR 1910.1000 and 1910.1200, for laboratory safety and chemical handling.

Practical Value

Utilizing ASTM D4301-05(2019) for total chlorine analysis in epoxy resins helps manufacturers, laboratories, and end users ensure product integrity, minimize the risk of corrosion, and comply with technical and regulatory specifications. This promotes higher quality, reliability, and durability in end-use applications, safeguarding both product performance and brand reputation within increasingly competitive global markets.

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: D4301 − 05 (Reapproved 2019)
Standard Test Method for
Total Chlorine in Epoxy Resins and Compounds
This standard is issued under the fixed designation D4301; 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 4. Summary of Test Method
1.1 This test method describes a procedure for the determi- 4.1 The material, dissolved in dimethoxyethane (DME) or
nation of total chlorine in epoxy resins and glycidyl ethers. other suitable inert solvent, is reacted with sodium biphenyl to
convert bound organic chlorine to the water soluble chloride.
1.2 The values stated in SI units are to be regarded as
The excess reagent is decomposed with isopropyl alcohol. The
standard. No other units of measurement are included in this
chloride ion is then titrated potentiometrically with silver
standard.
nitrate.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 The presence of residual chlorine in epoxy resins is
priate safety, health, and environmental practices and deter-
deleterious to final product properties. This test method has
mine the applicability of regulatory limitations prior to use.
been found to be applicable to resins or ethers with chlorine
For specific hazard statements, see Section 8.
contents ranging from 50 ppm to 35 % by weight. Other
1.4 This international standard was developed in accor-
halogen compounds react with the reagent but are distin-
dance with internationally recognized principles on standard-
guished from chlorine by the final potentiometric titration.
ization established in the Decision on Principles for the
Epoxyandotherfunctionalgroupswillconsumereagentbutdo
Development of International Standards, Guides and Recom-
not affect the results.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
6. Apparatus
6.1 Potentiograph.
2. Referenced Documents
6.2 Beaker, of appropriate size.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
6.3 Buret, of appropriate size.
D6440 Terminology Relating to Hydrocarbon Resins
6.4 Stirrer, magnetic or paddle.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
7. Reagents
2.2 Other Document:
7.1 Purity of Reagents—Reagent grade chemicals shall be
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
used in all tests. Unless otherwise indicated, it is intended that
1910.1200
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
3. Terminology
where such specifications are available. Other grades may be
3.1 Definitions: For definitions of terms used in this
used, provided it is first ascertained that the reagent is of
standard, See Terminology D6440.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
7.2 Purity of Water—Unless otherwise indicated, references
and Related Coatings, Materials, andApplications and is the direct responsibility of
towatershallbeunderstoodtomeanreagentwaterconforming
Subcommittee D01.33 on Polymers and Resins.
to Type II of Specification D1193.
Current edition approved Oct. 1, 2019. Published October 2019. Originally
approved in 1984. Last previous edition approved in 2013 as D4301 – 05(2013).
DOI: 10.1520/D4301-05R19.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or ACS Reagent Chemicals, Specifications and Procedures for Reagents and
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standard-Grade Reference Materials, American Chemical Society, Washington,
Standards volume information, refer to the standard’s Document Summary page on DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
the ASTM website. Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
A suitable mechanical holder is available from the Gardner Laboratory, Inc., U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
5521 Landy Lane, Washington, DC, Item 660. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4301 − 05 (2019)
7.3 Sodium Biphenyl Reagent —(in ether solution). AgNO and for high chlorine
...