ASTM D5761-96(2006)
(Practice)Standard Practice for Emulsification/Suspension of Multiphase Fluid Waste Materials
Standard Practice for Emulsification/Suspension of Multiphase Fluid Waste Materials
SIGNIFICANCE AND USE
This practice is intended as a solution to the difficulty of obtaining reproducible test results from heterogeneous samples.
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.
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
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 one litre has been obtained.
1.5 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.
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.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5761 – 96 (Reapproved 2006)
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 SW846 Test Methods for Evaluating Solid Waste, Physical/
Chemical Methods
1.1 This practice covers the generation of a single-phase
suspension or emulsion from multiphase samples which are
3. Terminology
primarily liquid in order to facilitate sample preparation,
3.1 Definitions:
transfer, and analysis.
3.1.1 emulsion, n—a suspension of fine particles or glob-
1.2 This practice is designed to keep a multiphase fluid
ules, or both, of one or more liquids in another liquid.
sample in an emulsified/suspended state long enough to take a
3.2 Definitions of Terms Specific to This Standard:
single,compositesamplethatisrepresentativeofthesampleas
3.2.1 multiphase fluid waste material, n—a substance or
awhole.Thesamplemayreformmultiplelayersafterstanding.
mixture of chemicals that is no longer useful for its original
1.3 The emulsion/suspension generated by following this
purpose that visibly involves a solid and at least one liquid
practice can be used only for analytical procedures designed
phase or more than one liquid phase without any solid present.
forthetotalsampleandproceduresnotsignificantlyaffectedby
the emulsifier or the presence of an emulsion/suspension.
4. Summary of Practice
1.4 This practice assumes that a representative sample of
4.1 An emulsifier is added and mixed well with a sample of
not more than one litre has been obtained.
multiphase fluid waste material, to produce a uniform mixture
1.5 The values stated in SI units are to be regarded as
suitable for subsequent aliquoting.Asatisfactory homogeniza-
standard. No other units of measurement are included in this
tion has been attained when the sample appears to remain as a
standard.
single phase for 30 s or longer.
1.6 This standard does not purport to address all of the
4.2 Acalcium sulfonate emulsifier is used when the original
safety concerns, if any, associated with its use. It is the
sample is primarily organic in nature; a polyethylene glycol
responsibility of the user of this standard to establish appro-
monoalky ester is used when the original sample is primarily
priate safety and health practices and determine the applica-
aqueous in nature.Ablend of the two emulsifiers is used when
bility of regulatory limitations prior to use.
the original sample contains roughly equal volumes of organic
and aqueous material.
2. Referenced Documents
2.1 ASTM Standards:
5. Significance and Use
D4057 Practice for Manual Sampling of Petroleum and
5.1 This practice is intended as a solution to the difficulty of
Petroleum Products
obtaining reproducible test results from heterogeneous
D4177 Practice for Automatic Sampling of Petroleum and
samples.
Petroleum Products
5.2 This practice works best with multilayered liquids, but
2.2 EPA Standard:
can also be applied to samples with solid particles that are
sufficiently small in size to be suspended in an emulsion.
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
5.3 The emulsified/suspended sample can be used for all
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
bulk property testing such as microwave digestion/inductively
Elemental Analysis.
coupled argon plasma (ICAP), ion chromatography, heat of
Current edition approved May 1, 2006. Published June 2006. Originally
approved in 1995. Last previous edition approved in 2001 as D5761 – 96 (2001). combustion, ash content, water, nonvolatile residue, and pH. It
DOI: 10.1520/D5761-96R06.
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 Available from the Environmental Protection Agency, 401 M Street, SW,
the ASTM website. Washington, DC 20460.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5761 – 96 (2006)
FIG. 1 Sample Splitter Funnel
may be prudent to retain a portion of the sample in its original, 8. Reagents and Materials
multiphase form for some types of analyses.
8.1 Aqueous Emulsifier—Polyethylene glycol monoalky es-
ter, also known as PEG400.
6. Interferences
8.2 Organic Emulsifier—Calcium sulfonate (60 % weight)
6.1 Not all samples can be emulsified, due to varying in heavy aromatic naphtha.
chemical reactions with the surfactants. If the emulsion is not
9. Procedure
stable for at least 30 s after shaking, it may not be suitable for
9.1 Representative samples are to be provided to the labo-
testing as an emulsion.
ratory using standard techniques such as those described in
6.2 Duetotheirphysicalcomposition,somesamplesarenot
Practices D4057 or D4177 and EPA/SW846. It is assumed for
suitable for splitting and, as a result, cannot be emulsified if a
purposes of this practice that the size of the sample in the
nonemulsified retain is required. For example, excessive
laboratory is one litre or less.Adjustments in procedure will be
amountsofsolidsandsemisolidsortarsdonotpermitsplitting.
necessary for larger volumes.
6.3 In some instances, the amount of sample submitted may
9.2 Vigorously shake multiphase samples by hand, or by
not be sufficient for splitting and, as a result, cannot be
mechanicalmeans,forupto30s.Ifwithin1minaftershaking,
emulsified if some unemulsified sample must be retained.
the sample appears to separate and each of the layers consists
6.4 Erroneous results can be obtained if precautions are not
of at least 10 % by volume of the total, and if there is a
taken to avoid the loss of volatile material. Do not open
sufficientsampleavailablebasedonsubsequenttestingrequire-
containers unnecessarily. Results for samples from leaky con-
ments, then the sample is a candidate for the emulsification
tainersmustbemarkedtoindicatethatthesampleintegritywas
procedure.
not maintained during shipping
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