ASTM E3399-23

Standard Test Method for Non-volatile Residue in Ethanol and Ethanol Solutions

SIGNIFICANCE AND USE
5.1 Manufacturers of ethanol are responsible for identifying and controlling impurities according to regulatory standards. Impurities in ethanol that are non-volatile are critical quality attributes for applications in the food, feed and pharmaceutical, personal care applications. Non-volatile residue is an attribute important to users of ethanol for these applications.
SCOPE
1.1 This test method covers the determination of the non-volatile residue content of ethanol and ethanol solutions at the time of test.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 The accepted SI unit of pressure is the Pascal (Pa); the accepted SI unit for temperature is degrees Celsius.  
1.3 Warning—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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. For specific warning statements, see 6.4, 7.4, and 9.1.  
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: 30-Jun-2023
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: E48 - Bioenergy and Industrial Chemicals from Biomass
• Drafting Committee: E48.A0 - Product Specifications

Relations

• Refers: ASTM E1-13 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-May-2013
• Refers: ASTM D4057-06(2011) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 01-Jun-2011
• Refers: ASTM E29-08 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-Oct-2008
• Refers: ASTM E1-07 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2007
• Refers: ASTM E29-06b - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Nov-2006
• Refers: ASTM E29-06a - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Sep-2006
• Refers: ASTM E29-06 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-May-2006
• Refers: ASTM E1-05 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2005
• Refers: ASTM E29-04 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-Dec-2004
• Refers: ASTM E1-03a - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2003
• Refers: ASTM E1-03 - Standard Specification for ASTM Thermometers
• Effective Date: 10-May-2003
• Refers: ASTM E29-02e1 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 10-May-2002
• Refers: ASTM E1-98 - Standard Specification for ASTM Thermometers
• Effective Date: 10-Oct-2001
• Refers: ASTM E1-01 - Standard Specification for ASTM Thermometers
• Effective Date: 10-Oct-2001
• Refers: ASTM E1-98e1 - Standard Specification for ASTM Thermometers
• Effective Date: 10-Oct-2001

Overview

ASTM E3399-23: Standard Test Method for Non-volatile Residue in Ethanol and Ethanol Solutions is a crucial standard developed by ASTM International. This method specifies the procedure for determining the amount of non-volatile residue present in ethanol and ethanol solutions. Non-volatile residue refers to the soluble, suspended, or particulate material that remains after the evaporation of ethanol. Monitoring non-volatile residue is essential for producers and users in various industries-including food, feed, pharmaceuticals, and personal care-to ensure product quality and regulatory compliance. The standard exclusively uses SI units and highlights important safety and environmental considerations, particularly regarding mercury use and handling.

Key Topics

• Non-volatile Residue Determination: Emphasizes testing for impurities that do not evaporate with ethanol, affecting product purity and suitability for sensitive applications.
• Applicability in Sensitive Industries: Non-volatile impurities may impact food, pharmaceutical, feed, and personal care products, making their detection a critical quality control step.
• Procedural Guidance: Outlines requirements for sample preparation, standardized evaporation, and residue measurement under controlled laboratory conditions.
• Equipment and Materials: Specifies the use of balances (to 0.1 mg resolution), glassware, controlled temperature evaporative baths (100-180°C), and safe handling tools.
• Safety Practices: Provides warnings on mercury usage, encourages adherence to local and international safety regulations, and stresses environmentally responsible practices.
• Regulatory Alignment: Developed in accordance with WTO Technical Barriers to Trade principles, ensuring international acceptance and harmonization.

Applications

The ASTM E3399-23 standard is widely applicable for:

• Ethanol Manufacturers: helps identify and control impurities within regulatory limits for products destined for strictly regulated sectors.
• Quality Assurance Laboratories: enables reliable assessment of non-volatile residues in ethanol supplied for food, feed, pharmaceuticals, and cosmetics.
• Regulatory Compliance: supports documentation and evidence of product purity as required by food safety authorities, pharmaceutical agencies, and other regulatory bodies.
• Process Optimization: assists in monitoring and improving ethanol purification and storage procedures by highlighting residue levels.
• Supply Chain Integrity: assures downstream users-such as beverage, biofuel, and healthcare product manufacturers-that supplied ethanol meets rigorous purity standards.

Related Standards

Several standards and regulations interact with or support the ASTM E3399-23 method:

• ASTM D4057: Practice for Manual Sampling of Petroleum and Petroleum Products - referenced for appropriate sampling techniques.
• ASTM E1: Specification for ASTM Liquid-in-Glass Thermometers - ensures accurate temperature readings in controlled processes.
• ASTM E29: Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications - guides data reporting.
• U.S. CFR Title 27, Part 21: Formulas for Denatured Alcohol and Rum - related to regulatory constraints for alcohol products.
• U.S. CFR Title 27, Part 30.31: Determination of Proof - relevant for regulatory proof testing of ethanol solutions.

Keywords: non-volatile residue, ethanol, ethanol solutions, ASTM E3399-23, analytical chemistry, quality control, regulatory compliance, food safety, pharmaceutical purity, laboratory test method

By implementing ASTM E3399-23, organizations can ensure effective monitoring and control of non-volatile impurities in ethanol, maintaining safety, compliance, and product quality across critical industries.

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: E3399 − 23
Standard Test Method for
Non-volatile Residue in Ethanol and Ethanol Solutions
This standard is issued under the fixed designation E3399; 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 D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of the non-
E1 Specification for ASTM Liquid-in-Glass Thermometers
volatile residue content of ethanol and ethanol solutions at the
E29 Practice for Using Significant Digits in Test Data to
time of test.
Determine Conformance with Specifications
1.2 The values stated in SI units are to be regarded as
2.2 U.S. Federal Standards
standard. No other units of measurement are included in this
United States Code of Federal Regulations, Title 27, Part
standard.
21 Formulas for Denatured Alcohol and Rum
1.2.1 The accepted SI unit of pressure is the Pascal (Pa); the
United States Code of Federal Regulations, Title 27, Part
accepted SI unit for temperature is degrees Celsius.
30.31 Determination of Proof
1.3 Warning—Mercury has been designated by many regu-
latory agencies as a hazardous substance that can cause serious
3. Terminology
medical issues. Mercury, or its vapor, has been demonstrated to
3.1 Definitions of Terms Specific to This Standard:
be hazardous to health and corrosive to materials. Use caution
3.1.1 ethanol (ethyl alcohol, grain alcohol),
when handling mercury and mercury-containing products. See
n—CH3CH2OH; can be produced chemically from ethylene or
the applicable product Safety Data Sheet (SDS) for additional
biologically from the fermentation of various sugars from
information. The potential exists that selling mercury or
carbohydrates found in agricultural crops and cellulosic resi-
mercury-containing products, or both, is prohibited by local or
dues from crops or wood.
national law. Users must determine legality of sales in their
3.1.2 non-volatile residue, n—the soluble, suspended, or
location.
particulate material remaining following the evaporation of a
1.4 This standard does not purport to address all of the
sample.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety, health, and environmental practices and deter-
4.1 When testing ethanol or ethanol solutions, a 100 mL 6
mine the applicability of regulatory limitations prior to use.
For specific warning statements, see 6.4, 7.4, and 9.1. 0.5 mL quantity of ethanol or ethanol solution is evaporated
under controlled temperature conditions of minimum 100 °C,
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard- but not to exceed 180 °C.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 5. Significance and Use
mendations issued by the World Trade Organization Technical
5.1 Manufacturers of ethanol are responsible for identifying
Barriers to Trade (TBT) Committee.
and controlling impurities according to regulatory standards.
Impurities in ethanol that are non-volatile are critical quality
2. Referenced Documents
attributes for applications in the food, feed and pharmaceutical,
2.1 ASTM Standards:
personal care applications. Non-volatile residue is an attribute
important to users of ethanol for these applications.
This test method is under the jurisdiction of ASTM Committee E48 on
6. Apparatus/Materials
Bioenergy and Industrial Chemicals from Biomass and is the direct responsibility of
Subcommittee E48.A0 on Product Specifications.
6.1 Balance, capable of weighing test specimens to the
Current edition approved July 1, 2023. Published August 2023. DOI: 10.1520/
nearest 0.1 mg.
E3399-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.2 Beakers, of 100 mL capacity. Mark each beaker in the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
set, including the tare beaker, with an identifying number or
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. letter.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E3399 − 23
6.3 Cooling Vessel—A tightly covered vessel, such as a 7.3 If suspended or settled solid matter is present, mix or
desiccator without desiccant, for cooling the beakers before shake the contents of the sample container thoroughly using an
weighing. appropriate method (see Practice D4057).
7.4 Measure a 100 mL 6 0.5 mL test specimen in a gradu-
NOTE 1—The use of a desiccant could lead to erroneous results.
ated cylinder (see 6.6), and transfer it to a weighed beaker (see
6.4 Evaporation Bath—(Warning—If a liquid-filled evapo-
6.2). Use one beaker for each test specimen to be tested and fill
ration bath is used, care must be t
...