ASTM D5761-96(2012)
(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.
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.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5761 −96 (Reapproved 2012)
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 EPA Standard:
SW846Test Methods for Evaluating Solid Waste, Physical/
1.1 This practice covers the generation of a single-phase
Chemical Methods
suspension or emulsion from multiphase samples which are
primarily liquid in order to facilitate sample preparation,
3. Terminology
transfer, and analysis.
3.1 Definitions:
1.2 This practice is designed to keep a multiphase fluid
3.1.1 emulsion, n—a suspension of fine particles or
sample in an emulsified/suspended state long enough to take a
globules, or both, of one or more liquids in another liquid.
single,compositesamplethatisrepresentativeofthesampleas
3.2 Definitions of Terms Specific to This Standard:
awhole.Thesamplemayreformmultiplelayersafterstanding.
3.2.1 multiphase fluid waste material, n—a substance or
1.3 The emulsion/suspension generated by following this
mixture of chemicals that is no longer useful for its original
practice can be used only for analytical procedures designed
purpose that visibly involves a solid and at least one liquid
forthetotalsampleandproceduresnotsignificantlyaffectedby
phase or more than one liquid phase without any solid present.
the emulsifier or the presence of an emulsion/suspension.
4. Summary of Practice
1.4 This practice assumes that a representative sample of
not more than 1 L has been obtained.
4.1 An emulsifier is added and mixed well with a sample of
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 Acalciumsulfonateemulsifierisusedwhentheoriginal
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
D4057Practice for Manual Sampling of Petroleum and
5.1 Thispracticeisintendedasasolutiontothedifficultyof
Petroleum Products
obtaining reproducible test results from heterogeneous
D4177Practice for Automatic Sampling of Petroleum and
samples.
Petroleum Products
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.
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- 5.3 The emulsified/suspended sample can be used for all
mittee D02.03 on Elemental Analysis.
bulk property testing such as microwave digestion/inductively
Current edition approved April 15, 2012. Published May 2012. Originally
coupled argon plasma (ICAP), ion chromatography, heat of
approved in 1995. Last previous edition approved in 2006 as D5761–96(2006).
combustion, ash content, water, nonvolatile residue, and pH. It
DOI: 10.1520/D5761-96R12.
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 (2012)
8. Reagents and Materials
8.1 Aqueous Emulsifier—Polyethylene glycol monoalky
ester, also known as PEG400.
8.2 Organic Emulsifier—Calcium sulfonate (60% weight)
in heavy aromatic naphtha.
9. Procedure
9.1 Representative samples are to be provided to the labo-
ratory using standard techniques such as those described in
Practices D4057 or D4177 and EPA/SW846. It is assumed for
purposes of this practice that the size of the sample in the
laboratoryisonelitreorless.Adjustmentsinprocedurewillbe
necessary for larger volumes.
9.2 Vigorously shake multiphase samples by hand, or by
mechanicalmeans,forupto30s.Ifwithin1minaftershaking,
the sample appears to separate and each of the layers consists
of at least 10% by volume of the total, and if there is a
sufficient sample available based on subsequent testing
FIG. 1 Sample Splitter Funnel
requirements, then the sample is a candidate for the emulsifi-
cation procedure.
9.3 (Optional.) If some unemulsified sample is to be
retained, split the sample into two separate samples using the
maybeprudenttoretainaportionofthesampleinitsoriginal,
splitter funnel shown in Fig. 1.
multiphase form for some types of analyses.
9.4 Tentatively classify any liquid phase, using information
known about the sample, as organic or aqueous and determine
6. Interferences
their volume percentages relative to the whole sample. See
6.1 Not all samples can be emulsified, due to varying
AppendixX1foranexampleworksheetonwhichtorecordthe
chemical reactions with the surfactants. If the emulsion is not
information.
stable for at least 30 s after shaking, it may not be suitable for
9.4.1 As a guide to classifying a sample in a clear glass jar,
testing as an emulsion.
measure phase height from the inside bottom of the jar, not
6.2 Duetotheirphysicalcomposition,somesamplesarenot from the bench top, using a ruler held up to the outer vertical
suitable for splitting and, as a result, cannot be emulsified if a
side
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