ASTM D3921-96(2003)e1
(Test Method)Standard Test Method for Oil and Grease and Petroleum Hydrocarbons in Water
Standard Test Method for Oil and Grease and Petroleum Hydrocarbons in Water
SIGNIFICANCE AND USE
The presence of oil and grease in domestic and industrial waste water is of concern to the public because of its deleterious aesthetic effect and its impact on aquatic life. Regulations and standards have been established that require monitoring of oil and grease in water and waste water. This test method provides an analytical procedure to measure oil and grease in water and waste water.
SCOPE
1.1 This test method covers the determination of fluorocarbon-extractable substances as an estimation of the combined oil and grease and the petroleum hydrocarbon contents of a sample of water or waste water in the range from 0.5 to 100 mg/L. It is the user's responsibility to assume the validity of the standard for untested types of water.
1.2 This test method defines oil and grease in water and waste water as that matter which is extractable in the test method and measured by infrared absorption. Similarly, this test method defines petroleum hydrocarbons in water and waste water as that oil and grease which is not adsorbed by silica gel in the test method and that is measured by infrared absorption.
1.3 Low-boiling organic materials are lost by evaporation during the manipulative transfers. However, these evaporative losses are generally much lower than those experienced with gravimetric procedures that require solvent evaporation before the residue is weighed.
1.4 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.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3921–96 (Reapproved 2003)
Standard Test Method for
Oil and Grease and Petroleum Hydrocarbons in Water
This standard is issued under the fixed designation D3921; 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.
This standard has been approved for use by agencies of the Department of Defense.
´ NOTE—Editorial changes were made throughout in January 2003.
1. Scope D3370 Practices for Sampling Water from Closed Conduits
D3856 Guide for Good Laboratory Practices in Laborato-
1.1 This test method covers the determination of
ries Engaged in Sampling and Analysis of Water
fluorocarbon-extractable substances as an estimation of the
D5847 Practice for Writing Quality Control Specifications
combined oil and grease and the petroleum hydrocarbon
for Standard Test Methods for Water Analysis
contents of a sample of water or waste water in the range from
E168 Practices for General Techniques of Infrared Quanti-
0.5 to 100 mg/L. It is the user’s responsibility to assume the
tative Analysis
validity of the standard for untested types of water.
1.2 This test method defines oil and grease in water and
3. Terminology
waste water as that matter which is extractable in the test
3.1 Definitions—For definitions of terms used in this test
method and measured by infrared absorption. Similarly, this
method, refer to Terminology D1129 and Practices E168.
testmethoddefinespetroleumhydrocarbonsinwaterandwaste
3.2 Definitions of Terms Specific to This Standard:
water as that oil and grease which is not adsorbed by silica gel
3.2.1 oil and grease—the organic matter extracted from
in the test method and that is measured by infrared absorption.
water or waste water and measured by this test method.
1.3 Low-boiling organic materials are lost by evaporation
3.2.2 petroleum hydrocarbons—the oil and grease remain-
during the manipulative transfers. However, these evaporative
ing in solution after contact with silica gel and measured by
losses are generally much lower than those experienced with
this test method.
gravimetric procedures that require solvent evaporation before
the residue is weighed.
4. Summary of Test Method
1.4 This standard does not purport to address all of the
4.1 The acidified sample of water or waste water is ex-
safety concerns, if any, associated with its use. It is the
tractedseriallywiththree30-mLvolumesof1,1,2-trichloro-1,
responsibility of the user of this standard to establish appro-
2, 2-trifluoroethane (referred to in this test method as sol-
priate safety and health practices and determine the applica-
vent). The extract is diluted to 100 mL and a portion is
bility of regulatory limitations prior to use.
examined by infrared spectroscopy to measure the amount of
oil and grease removed from the original sample. A major
2. Referenced Documents
2 portion of the remaining extract is contacted with silica gel to
2.1 ASTM Standards:
remove polar substances, thereby providing a solution of
D1129 Terminology Relating to Water
petroleum hydrocarbons. This treated extract is then similarly
D1193 Specification for Reagent Water
examined by infrared spectroscopy.
D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
5. Significance and Use
D3325 PracticeforPreservationofWaterborneOilSamples
5.1 The presence of oil and grease in domestic and indus-
trial waste water is of concern to the public because of its
This test method is under the jurisdiction ofASTM Committee D19 on Water
deleterious aesthetic effect and its impact on aquatic life.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Regulations and standards have been established that require
Organic Substances in Water.
Current edition approved Jan. 10, 2003. Published January 2003. Originally
approved in 1980. Last previous edition approved in 1996 as D3921–96. DOI:
10.1520/D3921-96R03E01. Gruenfeld, M., “Extraction of Dispersed Oils from Water for Quantitative
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Analysis by Infrared Spectrophotometry,” Environmental Science and Technology,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Vol 7, 1973, pp. 636–639.
Standards volume information, refer to the standard’s Document Summary page on Consult the manufacturer’s operation manual for the specific instructions
the ASTM website. related to the infrared spectrometer or analyzer to be used.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D3921–96 (2003)
monitoringofoilandgreaseinwaterandwastewater.Thistest 8.3 Calibration Oil and Grease, similar in composition to
method provides an analytical procedure to measure oil and oil and grease determined by this test method for possible use
grease in water and waste water. as calibration material.
8.4 Cetane (n-Hexadecane), 99% minimum purity, for
6. Interferences
possible use in calibration mixture.
6.1 Since the constituents oil and grease and petroleum
8.5 Isooctane (2,2,4-Trimethylpentane), 99% minimum pu-
hydrocarbons are defined as the results of the test procedure,
rity, for possible use in calibration mixture.
interferences are precluded by definition. Interpretation of test
8.6 Silica Gel , 100 to 200 mesh, which has been deacti-
resultsonthebasisofchemicalstructure,pollutionpotential,or
vated with 2% water.
treatability should be approached with caution, however, be-
8.7 Sodium Bisulfate (NaHSO ), monohydrate.
cause of the diversity of substances measured by this proce-
8.8 Sodium Sulfate (Na SO ), anhydrous, granular.
2 4
dure.
8.9 Solvent —1, 1, 2-trichloro-1, 2, 2- trifluoroethane.
6.2 Organic solvents and certain other organic compounds
NOTE 1—Frequently, this solvent will extract plasticizer from the liner
not considered as oil and grease on the basis of chemical
of its shipping container. Check for such contamination by evaporating
structure may be extracted and measured as oil and grease. Of
100 mL of solvent in a steam bath and weighing its residue. If this value
those measured, certain ones may be adsorbed by silica gel
exceeds 0.1 mg, purify the solvent by distillation and check the overhead
while others may not. Those which are not adsorbed are
material for residue. Store the purified solvent in clean, glass bottles
having TFE-Fluorocarbon cap liners. Purification of this solvent as a
measured as petroleum hydrocarbons.
matter of course is highly desirable.
7. Apparatus
8.10 Sulfuric Acid (1 + 1)—Slowly and carefully add 1
7.1 Cell(s), quartz, 10-mm path length, two required for
volume of sulfuric acid (H SO , sp gr 1.84) to 1 volume of
2 4
double-beam operation, one required for single-beam opera-
water, stirring and cooling the solution during the addition.
tion, or built-in cell for nondispersive infrared analyzer opera-
tion. 9. Sampling
7.2 Filter Paper, ashless, quantitative, general-purpose,
9.1 Collect the sample in accordance with the principles
11-cm or equivalent.
described in Practices D3370, using a glass bottle equipped
7.3 Glass Bottle, approximately 1000-mL, with screw cap
with a screw cap having a TFE-fluorocarbon liner.
having a TFE-fluorocarbon liner.
9.2 Asample of about 750 mL is required for this test. Use
7.4 Graduated Cylinder, 1000-mL.
theentiresamplesincenoportionshouldberemovedforother
7.5 Infrared Spectrometer, double-beam dispersive, single-
tests.
beam dispersive, Fourier transform, or nondispersive infrared
9.3 Preserve the sample with a sufficient quantity of either
analyzer.
sulfuric acid (see 8.10) or sodium bisulfate (see 8.7) to attain a
7.6 Magnetic Stirrer, with small TFE-fluorocarbon stirring
pH of 2 or lower. The amount of reagent required will be
bar.
dependent upon the pH of the sample at the time of collection
7.7 Separatory Funnel, 2000-mL, with TFE-fluorocarbon
and upon its buffer capacity.
stopcock (one for each sample analyzed during any one period
of time).
10. Calibration
7.8 Volumetric Flask,100-mL(minimumofsixrequiredfor
NOTE 2—Achoiceoftwocalibrationspeciesisavailabletotheanalyst.
calibration plus one for each sample analyzed during any one
Thepreferredmaterialisasampleofthesameoilandgreasethatisknown
period of time).
tobepresentinthesampleofwaterorwastewaterawaitinganalysis.The
other material is a mixture of isooctane and cetane. This latter blend is to
8. Reagents
be used when the same (as described) material is not available.
8.1 Purity of Reagents—Reagent grade chemicals shall be
10.1 If the blend of isooctane and cetane is to be used for
used in all tests. Unless otherwise indicated, it is intended that
calibration,prepareacalibrationmixturebypipetting15mLof
allreagentsshallconformtothespecificationoftheCommittee
isooctane and 15 mL of cetane into a glass-stoppered bottle.
on Analytical Reagents of the American Chemical Society,
Mixthecontentswellandmaintaintheintegrityofthemixture
where such specifications are available. Other grades may be
by keeping the container tightly sealed except when a portion
used, provided it is first ascertained that the reagent is of
is withdrawn for blending.
sufficiently high purity to permit its use without lessening the
10.2 Calibration Solution Blend A—Place about 20 mL of
accuracy of the determination.
solventintoa100-mLvolumetricflask,stopper,andweigh.To
8.2 Purity of Water— Unless otherwise indicated, refer-
this flask quickly add about 1 mL of either the calibration oil
ences to water (not sample water) shall be understood to mean
and grease or the calibration mixture of isooctane and cetane.
reagent water conforming to Specification D1193, Type II.
Obtain its exact weight by difference. Fill to the mark with
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not Silica Gel, Davison Chemical Grade 923 has been found to be satisfactory for
listed by the American Chemical Society, see Analar Standards for Laboratory this purpose. Other available types from the same or different suppliers may be
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia suitable.
and National Formulary,U.S.PharmaceuticalConvention,Inc.(USPC),Rockville, This solvent is available also as Freon 113, Freon TF, Freon PCA, Genetron
MD. 113, Genesolve D, and as other names.
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D3921–96 (2003)
solvent and mix the liquid well by shaking the flask. Calculate should be obtained. If it is not, check cells for cleanliness,
theexactconcentrationofthecalibratingmaterialinsolutionin matching, etc. Drain and clean the sample cell. Obtain spectral
terms of mg/100 mL. If the calibration oil and grease is used, data for the solvent at this time for single-beam and nondis-
proceedto10.3.Ifthecalibrationmixtureisused,multiplythis persive infrared instruments, also. After running, drain, and
calculated concentration (about 730 mg/100 mL) by 1.4 (refer clean the sample cell.
to Note 3). This new concentration value (about 1022 mg/100 10.9 Fill the sample cell with Blend B. Scan as in 10.8;
mL) is to be used for BlendAthroughout the remainder of this drain, and clean the sample cell.
test method. 10.10 Fill the sample cell with Blend C. Scan as in 10.8;
drain, and clean the sample cell.
NOTE 3—Dating back to at least 1951, for many years a mixture of
10.11 Fill the sample cell with Blend D. Scan as in 10.8;
isooctane, cetane, and benzene was accepted as a standard for calibration.
drain, and clean the sample cell.
Concern regarding the hazards of exposure to benzene, which acts here
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only as a diluent having no contribution at 2930 cm (3.41 µm), has 10.12 Fill the sample cell with Blend E. Scan as in 10.8;
prompted elimination of this chemical as a component for calibration. To
drain, and clean the sample cell.
maintain relevance between current and future analytical data with those
10.13 Fill the sample cell with Blend F. Scan as in 10.8;
of the past, it is necessary to compensate for differences in concentration
drain, and clean the sample cell.
and in density between the former and the present calibration standards.
10.14 For each double-beam spectrum obtained in 10.9
The factor of 1.4 accomplishes this because the weight ratio of combined
through 10.13, draw a baseline similar to that found in Fig. 1.
isooctane plus cetane in the new two-way mixture to that in the older
Obtain the net absorbance for the peak that occurs near 2930
three-way mixture is 1.000 to 0.714, or 1.40. Henceforth, all concentra-
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tions involving the calibration mixture will be based upon the converted cm (3.41 µm). Obtain net values for single-beam and
value obtained in 10.2.
nondispersive infrared runs as recommended.
10.3 CalibrationSolutionBlendB—Dilute4mLofBlendA
NOTE 5—For infrared instruments having computer capability, data
with solvent in a 100-mL volumetric flask (about 41 mg/100
maybeobtainedautomaticallyorasdescribedin10.14.However,alldata
mL). must be obtained consistently by one means or the other, not a combina-
tion of the two.
10.4 CalibrationSolutionBlendC—Dilute3mLofBlendA
with solvent in a 100-mL volumetric flask (about 31 mg/100
10.15 On linear graph paper, plot the new absorbance
mL).
values, found in 10.14 or as permitted in Note 5, versus the
10.5 Calibration Solution Blend D—Dilute 50 mLof Blend
respective mg/100 mLvalues for each of the blends examined.
B with solvent in a 100-mLvolumetric flask (about 20 mg/100
The points should lie very nearly in a straight line. Draw the
mL).
best-fitting straight line through the points and keep this
10.6 Calibration Solution Blend E—Dilute 30 mLof Blend
calibration graph for use with the test samples. Alternatively,
C with solvent in a 100-mL volumetric flask (about 9 mg/100
determine the equation of the best-fitting straight line calcu-
mL).
lated by a linear regression technique. Record this equation for
10.7 Calibration Solution Blend F—Dilute 10 mLof Blend
use with the test samples.
Ewithsolventina100-mLvolumetricflask(about0.9mg/100
mL).
11. Procedure
NOTE 4—During the calibration events which follow, the cell used for
NOTE 6—Thisprocedureappliestoallsamplesregardlessofthetypeof
the blends must be thoroughly cleaned with fresh solvent and then dried
infrared instrumentation used for measurement.Thus, to comply with this
priortotheadditionofanewblend.Takecaretoavoidinsertionofthecell
test method, no extraction is to be attempted in a nondispersive infrared
stopper so tightly tha
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