ASTM D7066-04
(Test Method)Standard Test Method for dimer/trimer of chlorotrifluoroethylene (S-316) Recoverable Oil and Grease and Nonpolar Material by Infrared Determination
Standard Test Method for dimer/trimer of chlorotrifluoroethylene (S-316) Recoverable Oil and Grease and Nonpolar Material by Infrared Determination
SIGNIFICANCE AND USE
The presence and concentration of oil and grease in domestic and industrial wastewater 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 wastewater.
SCOPE
1.1 This test method covers the determination of oil and grease and nonpolar material in water and wastewater by an infrared (IR) determination of dimer/trimer of chlorotrifluoroethylene (S-316) extractable substances from an acidified sample. Included in this estimation of oil and grease are any other compounds soluble in the solvent.
1.2 The method is applicable to measurement of the light fuel although loss of some light ends during extraction can be expected.
1.3 This method defines oil and grease in water and wastewater as that which is extractable in the test method and measured by IR absorption at 2930 cm-1 or 3.4 microns. Similarly, this test method defines nonpolar material in water and wastewater as that oil and grease which is not adsorbed by silica gel in the test method and measured by IR absorption at 2930 cm-1.
1.4 This method covers the range of 5 to 100 mg/L and may be extended to a lower or higher level by extraction of a larger or smaller sample volume collected separately.
1.5 This standard does not purport to address all of the safety problems, 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 (D 3856 Guide for Good Laboratory Practices) the applicability of regulatory limitations prior to use.
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An American National Standard
Designation: D 7066 – 04
Standard Test Method for
dimer/trimer of chlorotrifluoroethylene (S-316) Recoverable
Oil and Grease and Nonpolar Material by Infrared
Determination
This standard is issued under the fixed designation D 7066; 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.
1. Scope Sampling and Analysis of Water
D 2777 Practice for the Determination of Precision and
1.1 This test method covers the determination of oil and
Bias of Applicable Methods of Committee D19 on Water
grease and nonpolar material in water and wastewater by an
D 5810 Guide for Spiking into Aqueous Samples
infrared (IR) determination of dimer/trimer of chlorotrifluoro-
D 5847 Practice for Writing Quality Control Specifications
ethylene (S-316) extractable substances from an acidified
for Standard Test Methods for Water Analysis
sample. Included in this estimation of oil and grease are any
E 168 Practices for General Techniques of Infrared Quanti-
other compounds soluble in the solvent.
tative Analysis
1.2 The method is applicable to measurement of the light
E 178 Practice for Dealing With Outlying Observations
fuel although loss of some light ends during extraction can be
expected.
3. Terminology
1.3 This method defines oil and grease in water and waste-
3.1 Definitions—For definitions of terms used in this test
water as that which is extractable in the test method and
method, refer to Terminology D 1129 and Practices E 168.
measured by IR absorption at 2930 cm- or 3.4 microns.
3.2 Definitions of Terms Specific to This Standard:
Similarly, this test method defines nonpolar material in water
3.2.1 oil and grease—the organic matter extracted from
and wastewater as that oil and grease which is not adsorbed by
water or wastewater and measured by this test method.
silica gel in the test method and measured by IR absorption at
3.2.2 nonpolar material—the oil and grease remaining in
2930 cm- .
solution after contact with silica gel and measured by this test
1.4 This method covers the range of 5 to 100 mg/Land may
method.
be extended to a lower or higher level by extraction of a larger
3.2.3 solvent—dimer/trimer of chlorotrifluoroethylene (S-
or smaller sample volume collected separately.
316)
1.5 This standard does not purport to address all of the
safety problems, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 An acidified 250-mL sample of water or wastewater is
priate safety and health practices and determine (D 3856
extracted serially with three 15-mLvolumes of dimer/trimer of
Guide for Good Laboratory Practices ) the applicability of
chlorotrifluoroethylene (S-316).The extract is diluted to 50mL
regulatory limitations prior to use.
and a portion is examined by infrared spectroscopy (IR) for an
2. Referenced Documents oil and grease measurement. A portion of the extract is
contacted with silica gel to remove polar substances, thereby
2.1 ASTM Standards:
producing a solution containing nonpolar material. The non-
D 1129 Terminology Relating to Water
polar material is measured by infrared spectroscopy.
D 1193 Specification for Reagent Water
D 3370 PracticesforSamplingWaterfromClosedConduits
5. Significance and Use
D 3856 Guide for Good Laboratory Practices Engaged in
5.1 The presence and concentration of oil and grease in
domestic and industrial wastewater is of concern to the public
because of its deleterious aesthetic effect and its impact on
This test method is under the jurisdiction of ASTM Committee D19 on Water
aquatic life.
and is the direct responsibility of Subcommittee 19.06 on Methods forAnalysis for
5.2 Regulations and standards have been established that
Organic Substances in Water.
require monitoring of oil and grease in water and wastewater.
Current edition approved June 1, 2004. Published July 2004.
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 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.
D7066–04
6. Interferences 8.3 Isooctane (2,2,4-trimethylpentane) 98 % minimum pu-
rity, for use in calibration.
6.1 Soaps, detergents, surfactants and other materials may
8.4 Octanoic acid 98 % minimum purity, for use in calibra-
form emulsions that may reduce the amount of oil and grease
tion.
extracted from a sample. This test method contains procedures
8.5 Silica Gel, Anhydrous, 75 - 150 micrometers, Davisil
that can assist the analyst in breaking such emulsions.
Grade 923 (Supelco 21447-7A, or equivalent). Dry at
6.2 Organic compounds and other materials not considered
200–250°C for 24 hour minimum and store in a desiccator or
as oil and grease on the basis of chemical structure may be
tightly sealed container. Determine the dimer/trimer of chlo-
extracted and measured as oil and grease. Of those measured,
rotrifluoroethylene (S-316) soluble material content of the
certain ones may be adsorbed by silica gel while others may
silica gel by extracting 10 g of silica gel with 25 mL of
not. Those not adsorbed are measured as nonpolar material.
dimer/trimer of chlorotrifluoroethylene (S-316) and collect the
elute in a flask. Filter and fill a quartz cell for analysis by IR.
7. Apparatus
The dimer/trimer of chlorotrifluoroethylene (S-316) soluble
Allglasswarethatwillcomeincontactwiththesamplemust
material must be less than 5 mg/L.
be rinsed with dimer/trimer of chlorotrifluoroethylene (S-316)
8.6 Sodium Sulfate (Na SO ), ACS, granular anhydrous.
2 4
prior to beginning this procedure.
Dry at 200-250 °C for 24 hours minimum and store in a tightly
7.1 Cell(s), quartz, 10-mm path length (lower concentra-
sealed container until use. (Note: Powdered sodium sulfate
tions may require a longer pathlength), two required for
should not be used because water may cause it to solidify.)
double-beam operation, one required for single-beam opera-
8.7 Solvent - dimer/trimer of chlorotrifluoroethylene,IR
tion, or built-in or drop-in cell for infrared filtometer analyzer
spectroscopy grade, for example S-316 manufactured by
operation.
HoribaInstruments,IrvineCA,800-446-7422(ASTMdoesnot
7.2 Filter Paper, ashless, quantitative, general-purpose, 11-
advocate the use of one vendor over another)
cm, Whatman #40 or equivalent.
8.8 Sulfuric Acid (1 + 1)—Slowly and carefully add 1
7.3 Glass Funnel
volume of sulfuric acid (H SO , sp gr 1.84) to 1 volume of
2 4
7.4 Glass Wide Mouth Sample Bottle, minimum 250-mL,
water, stirring and cooling the solution during the addition
with screw cap having a fluoropolymer liner.
(optional HCl replacement).
7.5 Glass Graduated Cylinder, 100-mL
8.9 Hydrochloric acid, ACS, 1 + 1. Mix equal volumes of
7.6 Infrared Spectrometer, double-beam dispersive, single-
concentrated HCl and water
beam dispersive, Fourier transform, filtometers or other ca-
8.10 Sodium Chloride (NaCl), crystalline, ACS—or use in
pable of making measurements at 2930 cm- .
breaking emulsions, if needed. Wet thoroughly with solvent
7.7 Magnetic Stirrer, with small TFE-fluorocarbon stirring
before using.
bar.
7.8 Glass Separatory-Funnel, 500mL, with fluoropolymer
9. Sampling
stopcock and stopper.
9.1 Collect the sample in accordance with the principles
7.9 Volumetric Flasks, glass, various (10, 25, 50, 100, and
described in Practices D 3370, using a glass bottle equipped
200-mL)
with a screw cap having a fluoropolymer liner. Prerinse the
7.10 Teflon spritz bottle, one-piece wash bottle for rinsing
sample bottle and cap with the solvent prior to sample
7.11 Repeating pipetter, glass, 15-mL, (optional)
collection. Do not rinse the sample bottle with the sample to be
7.12 Volumetric Pipettes, glass, various (0.50, 1.00, 5.00,
analyzed. Fill bottle with minimal headspace to prevent loss of
10.0 and 25.0-mL, including a 1.00 serological pipet graduated
volatile constituants. Do not allow the sample to overflow the
in 0.01-mL increments and a 5.00-mL serological pipet gradu-
bottle during collection. Preventing overflow may not be
ated in 0.1-mL increments, or equivalent)
possible in all sampling situations, however, measures should
7.13 Benchtop shaker, (optional)
be taken to minimize overflow at all times.
7.14 Glass Stirring Rod, (optional)
9.2 A sample of about 250mL is required for this test. Use
7.15 Analytical Balance,
the entire sample because removing a portion would not
7.16 Syringes, 50 and 500 mL
apportion the oil and grease that adheres to the bottle surfaces.
The high probability that extractable matter may adhere to
8. Reagents
samplingequipmentandresultinmeasurementsthatarebiased
8.1 Purity of Reagents—Reagent grade chemicals shall be low precludes the collection of composite samples for deter-
used in all tests. Unless otherwise indicated, it is intended that mination of oil and grease. Therefore, samples must be
allreagentsshallconformtothespecificationoftheCommittee collected as grab samples. If a composite measurement is
on Analytical Reagents of the American Chemical Society, required, individual grab samples collected at prescribed time
where such specifications are available. Other grades may be intervals may be analyzed separately and the concentrations
used, provided it is first ascertained that the reagent is of averaged. Alternatively, samples can be collected in the field
sufficiently high purity to permit its use without lessening the and composited in the laboratory. For example, collect four
accuracy of the determination. individual 63-mL samples over the course of a day. In the
8.2 Purity of Water—Unless otherwise indicated, references laboratory, pour each 63-mLsample into the separatory funnel,
to laboratory or reagent water shall be understood to mean rinse each of the four bottles (and caps) sequentially with
reagent water conforming to Specification D 1193, Type II. 10mLofsolvent,andusethesolventfortheextraction(Section
D7066–04
12.2.2). Do not exceed 50 mL of total solvent during the 10.1.2 Diluted Stock Solution—Place 2.5 mL of the Stock
extraction and rinse procedure. Solution to a 50-mL volumetric flask and fill to mark with
9.3 Preserve the sample with a sufficient quantity of either solvent. Diluted Stock Solution = 5.0 mg/mL (5000 µg/mL).
sulfuric(seeSection8.8)orhydrochloricacid(seeSection8.9)
10.1.3 Calibration Solution A—Place 1.0 mL of Diluted
to a pH of 2 or lower and refrigerate at 0-4 °C from the time
Stock Solution in a 10-mLvolumetric flask and fill to the mark
of collection until extraction. The amount of acid required will
withsolvent.CalibrationSolutionA=0.5mg/mL(500µg/mL),
be dependent upon the pH and buffer capacity of the sample at
equivalent to 100 mg/L oil and grease in a 250-mL water
the time of collection. If the amount of acid required is not sample extracted into a 50-mL volume of solvent.
known, make the pH measurement on a separate sample that
10.1.4 Calibration Solution B—Place 0.50 mL of Diluted
will not be analyzed. Introduction of pH paper to an actual
Stock Solution in a 10-mLvolumetric flask and fill to the mark
sample or sample cap may remove some oil from the sample.
with solvent. Calibration Solution B = 0.25 mg/mL (250
To more accurately calculate the final oil concentration of the
µg/mL), equivalent to 50 mg/L oil and grease in a 250-mL
extract, the volume of acid added to each sample can be
water sample extracted into a 50-mL volume of solvent.
recorded, then subtracted from the final measured sample
10.1.5 Calibration Solution C—Place 0.20 mL of Diluted
volume.
Stock Solution in a 10-mLvolumetric flask and fill to the mark
If the sample is to be shipped by commercial carrier, U.S.
with solvent. Calibration Solution C = 0.1 mg/mL (100
Department of Transportation regulations limit the pH to a
µg/mL), equivalent to 20 mg/L of oil and grease in a 250-mL
minimum (see 40CFR Part 136, Table II Footnote 3) of 1.96 if
water sample extracted into a 50-mL solvent volume.
HCl is used and 1.15 if H SO is used (see 49 CFR part 172).
2 4
10.1.6 Calibration Solution D—Place 0.10 mL of Diluted
Collectanadditional1or2samplealiquotsforthematrixspike
Stock Solution in a 10-mLvolumetric flask and fill to the mark
and matrix spike duplicate (Section 14.5) and preserve with
with solvent. Calibration Solution D = 0.050 mg/mL (50
acid.
µg/mL), equivalent to 10 mg/L of oil and grease in a 250-mL
9.4 Refrigerate the sample at <4°C from the time of
water sample extracted into a 50-mL solvent volume.
collection until extraction. Freezing the sample may break the
10.1.7 Calibration Solution E—Place 0.05 mL of Diluted
bottle.
Stock Solution in a 10-mLvolumetric flask and fill to the mark
with solvent. Calibration Solution E = 0.025 mg/mL (25
10. Preparation of Calibration and Spiking Solutions
µg/mL), equivalent to 5 mg/L of oil and grease in a 250-mL
water sample extracted into a 50-mL solvent volume.
NOTE 1—The calibration standard specified in this procedure reflects
the objective of the test to detect recoverable oil and grease and nonpolar 10.2 Spiking Solution—
material in wastewater with an unknown composition of oil and grease. In
10.2.1 Transfer equal volumes of octanoic acid and isooc-
a few cases, the composition of the oil and grease in a sample will be
tane in a volumetric flask, beaker, or jar. Mix well.
known.However,inordertoobtainconsistentresultsbetweensamplesets
10.2.2 Pour 220 to 250 mL of water into a sample bottle.
and between laboratories with different wastewater matrices, calibration
Record the volume.
with the known oil and grease in a sample should not be used in this
method.
10.2.3 Using a syringe, dispense 15 µL of the octanoic
acid/isooctane solution under the surface of the water. Cap the
10.1 Calibration and Solvent Mixtures
bottle and shake well.
NOTE 2—The calibration procedure below calls for transferring, by
10.2.4 Calculate the total oil and grease concentration by
pipette or syringe, a volume of standard into a volumetric flask to obtain
dividing 12.0 mg (mass of 15 µL for solution density of 0.801
a desired concentration. Transfer volumes have been rounded for ease of
g/mL assuming no loss of volume due to mixing) by the water
measurement and calculation. It is highly recommended that
...
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