ASTM D4281-95
(Test Method)Standard Test Method for Oil and Grease (Fluorocarbon Extractable Substances) by Gravimetric Determination
Standard Test Method for Oil and Grease (Fluorocarbon Extractable Substances) by Gravimetric Determination
SCOPE
1.1 These test methods cover the estimation of oil and grease in water and wastewater by a gravimetric determination of fluorocarbon extractable substances from an acidified sample. Also included in this estimation of oil and grease are any other compounds soluble in chlorofluorocarbon-113 and non-volatile under the conditions of test.
1.2 The following two test methods are included:SectionsTest Method A-Liquid-Liquid Extraction10-15Test Method B-Soxhlet Extraction16-23
1.3 These test methods are applicable to natural waters and domestic wastewaters. They are also suitable for most industrial wastewaters, although certain wastes may yield low results because of the presence of either excessive concentrations of natural greases or synthetic or modified compounds that are not well recovered by these test methods.
1.4 These test methods measure those groups of substance called oil and grease, whether soluble or insoluble, polar or non-polar, or biological or mineral in origin, to the extent these substances partition from the matrix into chlorofluorocarbon-113 and are not volatilized under conditions of the test. (See the Introduction and Section 3 of these test methods.)
1.5 Because these test methods include an acidification step prior to extraction, soluble metallic soaps are hydrolyzed and recovered as fatty acids in the extraction step.
1.6 These test methods were fully validated by collaborative testing in reagent Type IV water. The information on precision may not apply to other waters.
Note 1--Refer to companion procedures (Test Method D3921).
1.7 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.8 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. For specific hazard statements, see 12.1, 13.2, 20.1, and 20.5.
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NOTICE: This standard has either been superseded and replaced by a new version or
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Designation: D 4281 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Oil and Grease (Fluorocarbon Extractable Substances) by
1
Gravimetric Determination
This standard is issued under the fixed designation D 4281; 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 (e) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
In the determination of oil and grease, an absolute quantity of a specific substance is not measured.
Rather, groups of substances with similar physical characteristics are determined quantitatively on the
basis of their common solubility in a specified fluorocarbon solvent. Oil and grease may therefore, be
said to include hydrocarbons, fatty acids, soaps, fats, waxes, oil, and any other material that is
extracted by the solvent from an acidified sample of the test. It is important that this limitation be
clearly understood. Unlike some constituents—which represent distinct chemical elements, ions,
compounds, or groups of compounds, oils and greases are defined by the method used for their
determination.
1. Scope 1.6 These test methods were fully validated by collaborative
testing in reagent Type IV water. The information on precision
1.1 These test methods cover the estimation of oil and
may not apply to other waters.
grease in water and wastewater by a gravimetric determination
of fluorocarbon extractable substances from an acidified
NOTE 1—Refer to companion procedures (Test Method D 3921).
sample. Also included in this estimation of oil and grease are
1.7 The values stated in SI units are to be regarded as the
any other compounds soluble in chlorofluorocarbon-113 and
standard. The values given in parentheses are for information
non-volatile under the conditions of test.
only.
1.2 The following two test methods are included: 1.8 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 appro-
Sections
Test Method A—Liquid-Liquid Extraction 8-15
priate safety and health practices and determine the applica-
Test Method B—Soxhlet Extraction 16-23
bility of regulatory limitations prior to use. For specific hazard
1.3 These test methods are applicable to natural waters and statements, see 12.1, 13.2, 20.1, and 20.5.
domestic wastewaters. They are also suitable for most indus-
2. Referenced Documents
trial wastewaters, although certain wastes may yield low
2.1 ASTM Standards:
results because of the presence of either excessive concentra-
2
D 1129 Terminology Relating to Water
tions of natural greases or synthetic or modified compounds
D 1192 Specification for Equipment for Sampling Water
that are not well recovered by these test methods.
2
and Steam in Closed Conduits
1.4 These test methods measure those groups of substance
2
D 1193 Specification for Reagent Water
called oil and grease, whether soluble or insoluble, polar or
D 3370 Practices for Sampling Water from Closed Con-
non-polar, or biological or mineral in origin, to the extent these
2
duits
substances partition from the matrix into chlorofluorocarbon-
D 3856 Guide for Good Laboratory Practices in Laborato-
113 and are not volatilized under conditions of the test. (See the
ries Engaged in Sampling and Analysis of Water and Waste
Introduction and Section 3 of these test methods.)
2
Water
1.5 Because these test methods include an acidification step
D 3921 Test Method for Oil and Grease and Petroleum
prior to extraction, soluble metallic soaps are hydrolyzed and 3
Hydrocarbons in Water
recovered as fatty acids in the extraction step.
D 4210 Practice for Interlaboratory Quality Control Proce-
2
dures and a Discussion on Reporting Low-Level Data
D 5789 Practice for Writing Quality Control Specifications
1
This test method is under the jurisdiction of ASTM Committee D-19 on Water
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
2
Current edition approved Dec. 10, 1995. Published February 1996. Originally Annual Book of ASTM Standards, Vol 11.01.
3
published as D4281 – 83. Last previous edition D4281 – 93. Annual Book of ASTM Standards, Vol 11.02.
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D 4281
3
for Standard Test Methods for Organic Constituents 5.6 Suspended solids may interfere by contributing to emul-
sions.
3. Terminology
6. Purity of Reagents
3.1 Definitions—For definitions of terms used in these test
6.1 Reagent grade chemicals shall be used in all tests.
method
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