ASTM D3921-96(2011)
(Test Method)Standard Test Method for Oil and Grease and Petroleum Hydrocarbons in Water (Withdrawn 2013)
Standard Test Method for Oil and Grease and Petroleum Hydrocarbons in Water (Withdrawn 2013)
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
WITHDRAWN RATIONALE
Formerly under the jurisdiction of Committee D19 on Water, this test method was withdrawn in December 2012. This standard is being withdrawn without replacement due to its limited use by industry.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3921 − 96(Reapproved 2011)
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.
1. Scope D2777Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.1 This test method covers the determination of
D3325Practice for Preservation of Waterborne Oil Samples
fluorocarbon-extractable substances as an estimation of the
D3370Practices for Sampling Water from Closed Conduits
combined oil and grease and the petroleum hydrocarbon
D3856Guide for Management Systems in Laboratories
contents of a sample of water or waste water in the range from
Engaged in Analysis of Water
0.5 to 100 mg/L. It is the user’s responsibility to assume the
D5847Practice for Writing Quality Control Specifications
validity of the standard for untested types of water.
for Standard Test Methods for Water Analysis
1.2 This test method defines oil and grease in water and
E168Practices for General Techniques of Infrared Quanti-
waste water as that matter which is extractable in the test
tative Analysis
method and measured by infrared absorption. Similarly, this
testmethoddefinespetroleumhydrocarbonsinwaterandwaste
3. Terminology
water as that oil and grease which is not adsorbed by silica gel
3.1 Definitions—For definitions of terms used in this test
in the test method and that is measured by infrared absorption.
method, refer to Terminology D1129 and Practices E168.
1.3 Low-boiling organic materials are lost by evaporation
3.2 Definitions of Terms Specific to This Standard:
during the manipulative transfers. However, these evaporative
3.2.1 oil and grease—the organic matter extracted from
losses are generally much lower than those experienced with
water or waste water and measured by this test method.
gravimetric procedures that require solvent evaporation before
3.2.2 petroleum hydrocarbons—the oil and grease remain-
the residue is weighed.
ing in solution after contact with silica gel and measured by
1.4 The values stated in SI units are to be regarded as
this test method.
standard. No other units of measurement are included in this
standard.
4. Summary of Test Method
1.5 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- 3
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
portion of the remaining extract is contacted with silica gel to
2.1 ASTM Standards:
remove polar substances, thereby providing a solution of
D1129Terminology Relating to Water petroleum hydrocarbons. This treated extract is then similarly
D1193Specification for Reagent Water
examined by infrared spectroscopy.
5. Significance and Use
This test method is under the jurisdiction ofASTM Committee D19 on Water
5.1 The presence of oil and grease in domestic and indus-
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
trial waste water is of concern to the public because of its
Organic Substances in Water.
Current edition approved May 1, 2011. Published June 2011. Originally
´1
approved in 1980. Last previous edition approved in 2003 as D3921–96 (2003) .
DOI: 10.1520/D3921-96R11. 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
D3921 − 96 (2011)
deleterious aesthetic effect and its impact on aquatic life. used, provided it is first ascertained that the reagent is of
Regulations and standards have been established that require sufficiently high purity to permit its use without lessening the
monitoringofoilandgreaseinwaterandwastewater.Thistest accuracy of the determination.
method provides an analytical procedure to measure oil and
8.2 PurityofWater—Unlessotherwiseindicated,references
grease in water and waste water.
to water (not sample water) shall be understood to mean
reagent water conforming to Specification D1193, Type II.
6. Interferences
8.3 Calibration Oil and Grease, similar in composition to
6.1 Since the constituents oil and grease and petroleum
oil and grease determined by this test method for possible use
hydrocarbons are defined as the results of the test procedure,
as calibration material.
interferences are precluded by definition. Interpretation of test
8.4 Cetane (n-Hexadecane), 99% minimum purity, for
resultsonthebasisofchemicalstructure,pollutionpotential,or
possible use in calibration mixture.
treatability should be approached with caution, however, be-
cause of the diversity of substances measured by this proce-
8.5 Isooctane (2,2,4-Trimethylpentane) , 99% minimum
dure.
purity, for possible use in calibration mixture.
6.2 Organic solvents and certain other organic compounds
8.6 Silica Gel , 100 to 200 mesh, which has been deacti-
not considered as oil and grease on the basis of chemical
vated with 2% water.
structure may be extracted and measured as oil and grease. Of
8.7 Sodium Bisulfate (NaHSO ), monohydrate.
those measured, certain ones may be adsorbed by silica gel
8.8 Sodium Sulfate (Na SO ), anhydrous, granular.
while others may not. Those which are not adsorbed are
2 4
measured as petroleum hydrocarbons.
8.9 Solvent —1, 1, 2-trichloro-1, 2, 2- trifluoroethane.
NOTE 1—Frequently, this solvent will extract plasticizer from the liner
7. Apparatus
of its shipping container. Check for such contamination by evaporating
7.1 Cell(s), quartz, 10-mm path length, two required for
100 mL of solvent in a steam bath and weighing its residue. If this value
double-beam operation, one required for single-beam opera- exceeds 0.1 mg, purify the solvent by distillation and check the overhead
material for residue. Store the purified solvent in clean, glass bottles
tion, or built-in cell for nondispersive infrared analyzer opera-
having TFE-Fluorocarbon cap liners. Purification of this solvent as a
tion.
matter of course is highly desirable.
7.2 Filter Paper, ashless, quantitative, general-purpose,
8.10 Sulfuric Acid (1 + 1) —Slowly and carefully add 1
11-cm or equivalent.
volume of sulfuric acid (H SO , sp gr 1.84) to 1 volume of
2 4
7.3 Glass Bottle, approximately 1000-mL, with screw cap
water, stirring and cooling the solution during the addition.
having a TFE-fluorocarbon liner.
9. Sampling
7.4 Graduated Cylinder, 1000-mL.
9.1 Collect the sample in accordance with the principles
7.5 Infrared Spectrometer, double-beam dispersive, single-
described in Practices D3370, using a glass bottle equipped
beam dispersive, Fourier transform, or nondispersive infrared
with a screw cap having a TFE-fluorocarbon liner.
analyzer.
9.2 Asample of about 750 mL is required for this test. Use
7.6 Magnetic Stirrer, with small TFE-fluorocarbon stirring
theentiresamplesincenoportionshouldberemovedforother
bar.
tests.
7.7 Separatory Funnel, 2000-mL, with TFE-fluorocarbon
9.3 Preserve the sample with a sufficient quantity of either
stopcock (one for each sample analyzed during any one period
sulfuric acid (see 8.10) or sodium bisulfate (see 8.7) to attain a
of time).
pH of 2 or lower. The amount of reagent required will be
7.8 Volumetric Flask,100-mL(minimumofsixrequiredfor
dependent upon the pH of the sample at the time of collection
calibration plus one for each sample analyzed during any one
and upon its buffer capacity.
period of time).
10. Calibration
NOTE2—Achoiceoftwocalibrationspeciesisavailabletotheanalyst.
8. Reagents
Thepreferredmaterialisasampleofthesameoilandgreasethatisknown
8.1 Purity of Reagents—Reagent grade chemicals shall be
tobepresentinthesampleofwaterorwastewaterawaitinganalysis.The
used in all tests. Unless otherwise indicated, it is intended that other material is a mixture of isooctane and cetane. This latter blend is to
be used when the same (as described) material is not available.
allreagentsshallconformtothespecificationoftheCommittee
on Analytical Reagents of the American Chemical Society,
10.1 If the blend of isooctane and cetane is to be used for
where such specifications are available. Other grades may be
calibration,prepareacalibrationmixturebypipetting15mLof
isooctane and 15 mL of cetane into a glass-stoppered bottle.
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.
D3921 − 96 (2011)
calibration procedure. Rely upon sole recommendations of the manufac-
Mixthecontentswellandmaintaintheintegrityofthemixture
turerforsingle-beamandnondispersiveinfraredanalyzerssincevariations
by keeping the container tightly sealed except when a portion
in design make it impractical to offer instructions for their use with this
is withdrawn for blending.
method.Also, in relation to nondispersive infrared operation, reference to
scanning or running, or both, should be interpreted to mean obtaining a
10.2 Calibration Solution Blend A—Place about 20 mL of
−1
reading or a plot of the 2930-cm (3.41-µm) band.
solventintoa100-mLvolumetricflask,stopper,andweigh.To
10.8 Fill the reference cell (for double-beam operation) and
this flask quickly add about 1 mL of either the calibration oil
−1
and grease or the calibration mixture of isooctane and cetane. the sample cell with solvent and scan from 3200 cm (3.13
−1
µm) to 2700 cm (3.70 µm).Anearly horizontal, straight line
Obtain its exact weight by difference. Fill to the mark with
solvent and mix the liquid well by shaking the flask. Calculate should be obtained. If it is not, check cells for cleanliness,
matching, etc. Drain and clean the sample cell. Obtain spectral
theexactconcentrationofthecalibratingmaterialinsolutionin
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-
persive infrared instruments, also. After running, drain, and
proceedto10.3.Ifthecalibrationmixtureisused,multiplythis
calculated concentration (about 730 mg/100 mL) by 1.5 (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;
NOTE 3—Dating back to at least 1951, for many years a mixture of
drain, and clean the sample cell.
isooctane, cetane, and benzene was accepted as a standard for calibration.
10.11 Fill the sample cell with Blend D. Scan as in 10.8;
Concern regarding the hazards of exposure to benzene, which acts here
−1
only as a diluent having no contribution at 2930 cm (3.41 µm), has
drain, and clean the sample cell.
prompted elimination of this chemical as a component for calibration. To
10.12 Fill the sample cell with Blend E. Scan as in 10.8;
maintain relevance between current and future analytical data with those
drain, and clean the sample cell.
of the past, it is necessary to compensate for differences in concentration
and in density between the former and the present calibration standards.
10.13 Fill the sample cell with Blend F. Scan as in 10.8;
The factor of 1.5 accomplishes this because the weight ratio of combined
drain, and clean the sample cell.
isooctane plus cetane in the new two-way mixture to that in the older
three-way mixture is 1.000 to 0.714, or 1.40. Henceforth, all concentra-
10.14 For each double-beam spectrum obtained in 10.9
tions involving the calibration mixture will be based upon the converted
through 10.13, draw a baseline similar to that found in Fig. 1.
value obtained in 10.2.
Obtain the net absorbance for the peak that occurs near 2930
10.3 Calibration Solution Blend B—Dilute4mLofBlendA
−1
cm (3.41 µm). Obtain net values for single-beam and
with solvent in a 100-mL volumetric flask (about 41 mg/100
nondispersive infrared runs as recommended.
mL).
NOTE5—Forinfraredinstrumentshavingcomputercapability,datamay
10.4 Calibration Solution Blend C—Dilute3mLofBlendA
beobtainedautomaticallyorasdescribedin10.14.However,alldatamust
with solvent in a 100-mL volumetric flask (about 31 mg/100
be obtained consistently by one means or the other, not a combination of
mL). the two.
10.15 On linear graph paper, plot the new absorbance
10.5 Calibration Solution Blend D—Dilute 50 mLof Blend
values, found in 10.14 or as permitted in Note 5, versus the
B with solvent in a 100-mLvolumetric flask (about 20 mg/100
respective mg/100 mLvalues for each of the blends examined.
mL).
The points should lie very nearly in a straight line. Draw the
10.6 Calibration Solution Blend E—Dilute 30 mL of Blend
best-fitting straight line through the points and keep this
C with solvent in a 100-mL volumetric flask (about 9 mg/100
calibration graph for use with the test samples. Alternatively,
mL).
determine the equation of the best-fitting straight line calcu-
10.7 Calibration Solution Blen
...
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