ASTM D5761-23

Standard Practice for Emulsification/Suspension of Multiphase Fluid Waste Materials

SIGNIFICANCE AND USE
5.1 This practice is intended as a solution to the difficulty of obtaining reproducible test results from heterogeneous samples.  
5.2 This practice works best with multilayered liquids, but can also be applied to samples with solid particles that are sufficiently small in size to be suspended in an emulsion.  
5.3 The emulsified/suspended sample can be used for all bulk property testing such as microwave digestion/inductively coupled argon plasma (ICAP), ion chromatography, heat of combustion, ash content, water, nonvolatile residue, and pH. It may be prudent to retain a portion of the sample in its original, multiphase form for some types of analyses.
SCOPE
1.1 This practice covers the generation of a uniform mixture or emulsion from multiphase samples which are primarily liquid in order to facilitate sample preparation, transfer, and analysis.  
1.2 This practice is designed to keep a multiphase fluid sample in an emulsified/suspended state long enough to take a single, composite sample that is representative of the sample as a whole. The sample may reform multiple layers after standing.  
1.3 The emulsion/suspension generated by following this practice can be used only for analytical procedures designed for the total sample and procedures not significantly affected by the emulsifier or the presence of an emulsion/suspension.  
1.4 This practice assumes that a representative sample of not more than 1 L has been obtained.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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: 13.060.30 - Sewage water
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Refers: ASTM D4057-06(2011) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 01-Jun-2011
• Refers: ASTM D4057-95(2000) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 10-Apr-2000

Overview

ASTM D5761-23 is the standard practice for the Emulsification/Suspension of Multiphase Fluid Waste Materials, developed and published by ASTM International. This standard provides a consistent method for converting primarily liquid, multiphase samples-such as those containing both organic and aqueous phases, and potentially small solid particles-into a uniform mixture or emulsion. By creating a stable, representative sample, labs and industry professionals can achieve reproducible results during analysis and testing of otherwise heterogeneous waste materials. The practice addresses challenges in sample preparation, transfer, and analytical consistency for complex fluid waste matrices.

Key Topics

• Emulsification and Suspension Processes: The standard details procedures for achieving a uniform emulsion or suspension from multiphase fluid wastes, essential for accurate and representative analytical testing.
• Applicability to Complex Samples: While most effective with layered liquid samples, ASTM D5761-23 can be applied to samples containing small solids that remain suspended in the emulsion.
• Sample Stability: Guidance is provided to maintain the sample in a homogenized state long enough for aliquoting, acknowledging that separation may reoccur after standing.
• Use of Emulsifiers: Recommendations are included for selecting appropriate emulsifiers based on the sample’s organic or aqueous composition, or a mixture of both.
• Sample Size and Handling: Procedures are designed for sample volumes up to 1 liter, with notes on adjustments for larger volumes and the importance of maintaining safety and compliance with regulatory standards.
• Mitigating Analytical Variability: By providing instructions to reduce the inherent variability in sampling heterogeneous wastes, the standard supports more reliable and comparable data.

Applications

ASTM D5761-23 is widely applicable in laboratories and industries dealing with multiphase fluid waste analysis, including but not limited to:

• Hazardous and non-hazardous waste management: Ensuring samples from storage tanks, drums, or process streams can be uniformly tested for regulatory and quality control purposes.
• Environmental laboratories: Preparation of waste samples for advanced analytical techniques such as microwave digestion/inductively coupled argon plasma (ICAP), ion chromatography, heat of combustion, measurement of ash content, water content, nonvolatile residues, and pH.
• Petroleum and chemical industries: Assisting in the consistent sampling and analysis of process waste streams and by-products that exhibit phase separation.
• Regulatory compliance testing: Providing a standardized approach to meet requirements for representative sample analysis as mandated by environmental and safety agencies.
• Research and development: Supporting experimental work where the uniformity of complex waste samples is critical for obtaining valid and repeatable results.

Related Standards

ASTM D5761-23 aligns with and supplements various other standards, enhancing consistency in sample handling and analytical practices:

• ASTM D4057 - Practice for Manual Sampling of Petroleum and Petroleum Products: Reference technique for obtaining representative samples.
• ASTM D4177 - Practice for Automatic Sampling of Petroleum and Petroleum Products: Provides automated methods complementing manual procedures.
• EPA SW-846 - Test Methods for Evaluating Solid Waste, Physical/Chemical Methods: Established protocols for waste testing referenced for compliance.
• Guidance follows internationally recognized standardization principles, supporting global applicability in compliance frameworks.

Keywords: emulsification, heterogeneous sample, multiphase waste, sample preparation, ASTM D5761-23, emulsifier, analytical testing, representative sampling.

By following ASTM D5761-23, organizations ensure systematic, reproducible sample preparation for complex waste matrices, laying the foundation for reliable environmental, regulatory, and industrial waste analysis.

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: D5761 − 23
Standard Practice for
Emulsification/Suspension of Multiphase Fluid Waste
Materials
This standard is issued under the fixed designation D5761; 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* 2. Referenced Documents
2.1 ASTM Standards:
1.1 This practice covers the generation of a uniform mixture
D4057 Practice for Manual Sampling of Petroleum and
or emulsion from multiphase samples which are primarily
Petroleum Products
liquid in order to facilitate sample preparation, transfer, and
D4177 Practice for Automatic Sampling of Petroleum and
analysis.
Petroleum Products
1.2 This practice is designed to keep a multiphase fluid
2.2 EPA Standard:
sample in an emulsified/suspended state long enough to take a
SW846 Test Methods for Evaluating Solid Waste, Physical/
single, composite sample that is representative of the sample as 3
Chemical Methods
a whole. The sample may reform multiple layers after standing.
3. Terminology
1.3 The emulsion/suspension generated by following this
3.1 Definitions:
practice can be used only for analytical procedures designed
3.1.1 emulsion, n—a suspension of fine particles or
for the total sample and procedures not significantly affected by
globules, or both, of one or more liquids in another liquid.
the emulsifier or the presence of an emulsion/suspension.
3.2 Definitions of Terms Specific to This Standard:
1.4 This practice assumes that a representative sample of
3.2.1 emulsifier, n—a substance which when added to a
not more than 1 L has been obtained.
multiphase mixture aids in the stabilization of an emulsion of
1.5 The values stated in SI units are to be regarded as
the phases.
standard. No other units of measurement are included in this
3.2.2 multiphase fluid waste material, n—a substance or
standard.
mixture of chemicals that is no longer useful for its original
1.6 This standard does not purport to address all of the
purpose that visibly involves a solid and at least one liquid
safety concerns, if any, associated with its use. It is the
phase or more than one liquid phase without any solid present.
responsibility of the user of this standard to establish appro-
4. Summary of Practice
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.1 An emulsifier is added and mixed well with a sample of
multiphase fluid waste material, to produce a uniform mixture
1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard- suitable for subsequent aliquoting. A satisfactory homogeniza-
tion has been attained when the sample appears to remain as a
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- single phase for 30 s or longer.
mendations issued by the World Trade Organization Technical
4.2 A calcium sulfonate emulsifier is used when the original
Barriers to Trade (TBT) Committee.
sample is primarily organic in nature; a polyethylene glycol
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- Standards volume information, refer to the standard’s Document Summary page on
mittee D02.03 on Elemental Analysis. the ASTM website.
Current edition approved July 1, 2023. Published July 2023. Originally approved Available from United States Environmental Protection Agency (EPA), William
in 1995. Last previous edition approved in 2017 as D5761 – 96 (2017). DOI: Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
10.1520/D5761-23. http://www.epa.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5761 − 23
monoalky ester is used when the original sample is primarily
aqueous in nature. A blend of the two emulsifiers is used when
the original sample contains roughly equal volumes of organic
and aqueous material.
5. Significance and Use
5.1 This practice is intended as a solution to the difficulty of
obtaining reproducible test results from heterogeneous
samples.
5.2 This practice works best with multilayered liquids, but
can also be applied to samples with solid particles that are
sufficiently small in size to be suspended in an emulsion.
5.3 The emulsified/suspended sample can be used for all
bulk property testing such as microwave digestion/inductively
coupled argon plasma (ICAP), ion chromatography, heat of
combustion, ash content, water, nonvolatile residue, and pH. It
may be prudent to retain a portion of the sample in its original,
multiphase form for some types of analyses.
FIG. 1 Sample Splitter Funnel
6. Interferences
6.1 Not all samples can be emulsified, due to varying
8. Reagents and Materials
chemical reactions with the surfactants. If the emulsion is not
8.1 Aqueous Emulsifier—Polyethylene glycol monoalky
stable for at least 30 s after shaking, it may not be suitable for 5
ester, also known as PEG400.
testing as an emulsion.
8.2 Organic Emulsifier—Calcium sulfonate (60 % weight)
6.2 Due to their physical composition, some samples are not 5
in heavy aromatic naphtha.
suitable for splitting and, as a result, cannot be emulsified if a
nonemulsified retain is required. For example, excessive
9. Procedure
amounts of solids and semisolids or tars do not permit splitting.
9.1 Representative samples are to be provided to the labo-
6.3 In some instances, the amount of sample submitted may
ratory using standard techniques such as those described in
not be sufficient for splitting and, as a result, cannot be Practices D4057 or D4177 and EPA/SW846. It is assumed for
emulsified if some unemulsified sample must be retained.
purposes of this practice that the size of the sample in the
laboratory is one litre or less. Adjustments in procedure will be
6.4 Erroneous results can be obtained if precautions are not
necessary for larger volumes.
taken to avoid the loss of volatile material. Do not open
containers unnecessarily. Results for samples from leaky con- 9.2 Vigorously shake multiphase samples by hand, or by
tainers must be marked to indicate that the sample integrity was
mechanical means, for up to 30 s. If within 1 min after shaking,
not maintained during shipping/storage.
the sample appears to separat
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5761 − 96 (Reapproved 2017) D5761 − 23
Standard Practice for
Emulsification/Suspension of Multiphase Fluid Waste
Materials
This standard is issued under the fixed designation D5761; 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 Scope*
1.1 This practice covers the generation of a single-phase suspensionuniform mixture or emulsion from multiphase samples which
are primarily liquid in order to facilitate sample preparation, transfer, and analysis.
1.2 This practice is designed to keep a multiphase fluid sample in an emulsified/suspended state long enough to take a single,
composite sample that is representative of the sample as a whole. The sample may reform multiple layers after standing.
1.3 The emulsion/suspension generated by following this practice can be used only for analytical procedures designed for the total
sample and procedures not significantly affected by the emulsifier or the presence of an emulsion/suspension.
1.4 This practice assumes that a representative sample of not more than 1 L has been obtained.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 healthsafety, health, and environmental practices and determine
the applicability of regulatory limitations prior to use.
1.7 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.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
2.2 EPA Standard:
SW846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved May 1, 2017July 1, 2023. Published June 2017July 2023. Originally approved in 1995. Last previous edition approved in 20122017 as
D5761 – 96 (2012).(2017). DOI: 10.1520/D5761-96R17.10.1520/D5761-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from United States Environmental Protection Agency (EPA), William Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5761 − 23
3. Terminology
3.1 Definitions:
3.1.1 emulsion, n—a suspension of fine particles or globules, or both, of one or more liquids in another liquid.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 emulsifier, n—a substance which when added to a multiphase mixture aids in the stabilization of an emulsion of the phases.
3.2.2 multiphase fluid waste material, n—a substance or mixture of chemicals that is no longer useful for its original purpose that
visibly involves a solid and at least one liquid phase or more than one liquid phase without any solid present.
4. Summary of Practice
4.1 An emulsifier is added and mixed well with a sample of multiphase fluid waste material, to produce a uniform mixture suitable
for subsequent aliquoting. A satisfactory homogenization has been attained when the sample appears to remain as a single phase
for 30 s or longer.
4.2 A calcium sulfonate emulsifier is used when the original sample is primarily organic in nature; a polyethylene glycol monoalky
ester is used when the original sample is primarily aqueous in nature. A blend of the two emulsifiers is used when the original
sample contains roughly equal volumes of organic and aqueous material.
5. Significance and Use
5.1 This practice is intended as a solution to the difficulty of obtaining reproducible test results from heterogeneous samples.
5.2 This practice works best with multilayered liquids, but can also be applied to samples with solid particles that are sufficiently
small in size to be suspended in an emulsion.
5.3 The emulsified/suspended sample can be used for all bulk property testing such as microwave digestion/inductively coupled
argon plasma (ICAP), ion chromatography, heat of combustion, ash content, water, nonvolatile residue, and pH. It may be prudent
to retain a portion of the sample in its original, multiphase form for some types of analyses.
6. Interferences
6.1 Not all samples can be emulsified, due to varying chemical reactions with the surfactants. If the emulsion is not stable for at
least 30 s after shaking, it may not be suitable for testing as an emulsion.
6.2 Due to their physical composition, some samples are not suitable for splitting and, as a result, cannot be emulsified if a
nonemulsified retain is required. For example, excessive amounts of solids and semisolids or tars do not permit splitting.
6.3 In some instances, the amount of sample submitted may not be sufficient for splitting and, as a result, cannot be emulsified
if some unemulsified sample must be retained.
6.4 Erroneous results can be obtained if precautions are not taken to avoid the loss of volatile material. Do not open containers
unnecessarily. Results for samples from leaky containers must be marked to indicate that the sample integrity was not maintained
during shipping/storage.
7. Apparatus
7.1 Funnel, Splitting—2 L separatory funnel fitted with twin 0.7 mm inside diameter glass discharge tubes as shown in Fig. 1.
The sole source of supply of the apparatus known to the committee at this time is Universal Instrument Co., 315 W. Colfax, Palatine, IL 60067 (Part No. F-4001). If
you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting
of the responsible technical committee, which you may attend.
D5761 − 23
FIG. 1 Sample Splitter F
...