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ASTM E3399-23

(Test Method)

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

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
Current Stage
Ref Project

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ASTM E3399-23 - Standard Test Method for Non-volatile Residue in Ethanol and Ethanol SolutionsASTM E3399-23 - Standard Test Method for Non-volatile Residue in Ethanol and Ethanol Solutions
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ASTM E3399-23 - Standard Test Method for Non-volatile Residue in Ethanol and Ethanol Solutions
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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
1
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
2.1 ASTM Standards:
personal care applications. Non-volatile residue is an attribute
important to users of ethanol for these applications.
1
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.
2
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 service@astm.org. 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
1

---------------------- Page: 1 ----------------------
E3399 − 23
6.3 Cooling Vessel—A tightly covered vessel, such as a 7.3 If suspended or settled sol
...

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4.1 Titration techniques using KF reagent are one of the most widely used for the determination of water.  
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Ketones, stable (Note 4)  
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Orthoesters  
Amines, weak (Note 3)  
Peroxides (hydro, dialkyl)  
Anhydrides  
Sulfides  
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Thiocyanates  
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Acids (Note 5)  
Cupric oxide  
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Desiccants  
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Salts of organic and inorganic acids (Note 6)  
Barium dioxide  
Calcium carbonate  
Note 1: Some acids, such as formic, acetic, and adipic acid, are slowly esterified. For high accuracy with pyridine-based reagents, use 30 % to 50 % pyridine in methanol as the solvent. When using pyridine-free reagents, commercially available buffer solutions can be added to the sample prior to titration. With formic acid, it may be necessary to use methanol-free solvents and titrants (1).4
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5.1 New and used petroleum products can contain basic constituents that are present as additives. The relative amount of these materials can be determined by titration with acids. The base number is a measure of the amount of basic substances in the oil always under the conditions of the test. It is sometimes used as a measure of lubricant degradation in service. However, any condemning limit shall be empirically established.  
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1.1 This test method covers a procedure for the determination of basic constituents in petroleum products and new and used lubricants. This test method resolves these constituents into groups having weak-base and strong-base ionization properties, provided the dissociation constants of the more strongly basic compounds are at least 1000 times than that of the next weaker groups. This test method covers base numbers up to 250.  
1.2 In new and used lubricants, the constituents that can be considered to have basic properties are primarily organic and inorganic bases, including amino compounds. This test method uses hydrochloric acid as the titrant, whereas Test Method D2896 uses perchloric acid as the titrant. This test method may or may not titrate these weak bases and, if so, it will titrate them to a lesser degree of completion; some additives such as inhibitors or detergents may show basic characteristics.  
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5.1 This practice is intended for use in sampling liquid hydrocarbons including crude oils, condensates, refinery process intermediates, and refined products. Generally these samples are expected to contain mercury from the parts per billion (10–9 mass) to parts per million (10–6 mass) range.  
5.2 This practice is not intended for use when sampling aqueous systems where the concentrations of mercury are often in the parts per trillion (10–12 mass) range. These samples are often better addressed by using the rigorously clean techniques from the EPA Method 1669 “clean hands, dirty hands” sampling procedures.  
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5.4 This practice is only suitable for stabilized samples which remain 100 % liquid at ambient conditions. For samples that on depressurization lose some of the light hydrocarbon ends it is important to note that elemental mercury may be lost during sampling. Sampling modules which inject unstabilized liquid hydrocarbons close to process conditions directly to the mercury analyzer can be used to overcome this issue.  
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5.7 The presence of mercury during crude oil production, transport, and refining can be an environmental and industrial hygiene concern.
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1.2 This practice was developed for sampling streams where the mercury speciation is predominantly Hg(0) present as a mixture of dissolved Hg(0) atoms, adsorbed Hg(0) on particulates (for example, carbonaceous or mineral fines and Fe2O3) and suspended droplets of metallic mercury.  
1.3 The presence of suspended droplets of metallic mercury (often called “colloidal” mercury, since the droplet size can be very small) can make obtaining a representative sample very difficult for a variety of reasons (for example, non-isokinetic sampling of the liquid can result in over- or under-collection of suspended droplets and collection of mercury that has accumulated in dense larger drops and pools on the bottom of piping and in sample taps). Pay strict attention to the detailed procedure (Section 7) to ensure representative samples are collected.  
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SCOPE
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