ASTM D5761-96(2017)
(Practice)Standard Practice for Emulsification/Suspension of Multiphase Fluid Waste Materials
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 single-phase suspension 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 health 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.
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Designation: D5761 − 96 (Reapproved 2017)
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
1.1 This practice covers the generation of a single-phase 2.1 ASTM Standards:
suspension or emulsion from multiphase samples which are D4057 Practice for Manual Sampling of Petroleum and
primarily liquid in order to facilitate sample preparation, Petroleum Products
transfer, and analysis. D4177 Practice for Automatic Sampling of Petroleum and
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
Chemical Methods
a whole. The sample may reform multiple layers after standing.
3. Terminology
1.3 The emulsion/suspension generated by following this
practice can be used only for analytical procedures designed
3.1 Definitions:
for the total sample and procedures not significantly affected by
3.1.1 emulsion, n—a suspension of fine particles or
the emulsifier or the presence of an emulsion/suspension.
globules, or both, of one or more liquids in another liquid.
1.4 This practice assumes that a representative sample of
3.2 Definitions of Terms Specific to This Standard:
not more than 1 L has been obtained.
3.2.1 multiphase fluid waste material, n—a substance or
mixture of chemicals that is no longer useful for its original
1.5 The values stated in SI units are to be regarded as
purpose that visibly involves a solid and at least one liquid
standard. No other units of measurement are included in this
phase or more than one liquid phase without any solid present.
standard.
1.6 This standard does not purport to address all of the
4. Summary of Practice
safety concerns, if any, associated with its use. It is the
4.1 An emulsifier is added and mixed well with a sample of
responsibility of the user of this standard to establish appro-
multiphase fluid waste material, to produce a uniform mixture
priate safety and health practices and determine the applica-
suitable for subsequent aliquoting. A satisfactory homogeniza-
bility of regulatory limitations prior to use.
tion has been attained when the sample appears to remain as a
1.7 This international standard was developed in accor-
single phase for 30 s or longer.
dance with internationally recognized principles on standard-
4.2 A calcium sulfonate emulsifier is used when the original
ization established in the Decision on Principles for the
sample is primarily organic in nature; a polyethylene glycol
Development of International Standards, Guides and Recom-
monoalky ester is used when the original sample is primarily
mendations issued by the World Trade Organization Technical
aqueous in nature. A blend of the two emulsifiers is used when
Barriers to Trade (TBT) Committee.
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 service@astm.org. 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 May 1, 2017. Published June 2017. Originally Available from United States Environmental Protection Agency (EPA), William
approved in 1995. Last previous edition approved in 2012 as D5761 – 96 (2012). Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
DOI: 10.1520/D5761-96R17. http://www.epa.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5761 − 96 (2017)
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
FIG. 1 Sample Splitter Funnel
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
8.2 Organic Emulsifier—Calcium sulfonate (60 % weight)
testing as an emulsion.
in heavy aromatic naphtha.
6.2 Due to their physical composition, some samples are not
9. Procedure
suitable for splitting and, as a result, cannot be emulsified if a
nonemulsified retain is required. For example, excessive 9.1 Representative samples are to be provided to the labo-
amounts of solids and semisolids or tars do not permit splitting. ratory using standard techniques such as those described in
Practices D4057 or D4177 and EPA/SW846. It is assumed for
6.3 In some instances, the amount of sample submitted may
purposes of this practice that the size of the sample in the
not be sufficient for splitting and, as a result, cannot be
laboratory is one litre or less. Adjustments in procedure will be
emulsified if some unemulsified sample must be retained.
necessary for larger volumes.
6.4 Erroneous results can be obtained if precautions are not
9.2 Vigorously shake multiphase samples by hand, or by
taken to avoid the loss of volatile material. Do not open
mechanical means, for up to 30 s. If within 1 min after shaking,
containers unnecessarily. Results for samples from leaky con-
the sample appears to separate and each of the layers consists
tainers must be marked to indicate that the sample integrity was
of at least 10 % by volume of the total, and if there is a
not maintained during shipping/storage.
sufficient sample available based on su
...
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 2012) D5761 − 96 (Reapproved 2017)
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
1.1 This practice covers the generation of a single-phase suspension 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 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 health 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
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 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 30 s or longer.
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 April 15, 2012May 1, 2017. Published May 2012June 2017. Originally approved in 1995. Last previous edition approved in 20062012 as
D5761–96(2006).D5761 – 96 (2012). DOI: 10.1520/D5761-96R12.10.1520/D5761-96R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from the Environmental Protection Agency, 401 M Street, SW, Washington, DC 20460.United States Environmental Protection Agency (EPA), William
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://www.epa.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5761 − 96 (2017)
FIG. 1 Sample Splitter Funnel
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 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-L2 L separatory funnel fitted with twin 0.7-mm0.7 mm inside diameter glass discharge tubes as shown
in Fig. 1.
7.2 High-Intensity Lamp.
7.3 Polyethylene Transfer Pipet, 3.5-mL3.5 mL draw.
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 w
...
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