ASTM D7066-04(2011)
(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 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 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 (D3856 Guide for Good Laboratory Practices ) the applicability of regulatory limitations prior to use.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D7066 −04 (Reapproved 2011) An American National Standard
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 D7066; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers the determination of oil and 2.1 ASTM Standards:
grease and nonpolar material in water and wastewater by an D1129 Terminology Relating to Water
infrared (IR) determination of dimer/trimer of chlorotrifluoro- D1193 Specification for Reagent Water
ethylene (S-316) extractable substances from an acidified D3370 Practices for Sampling Water from Closed Conduits
sample. Included in this estimation of oil and grease are any D3856 Guide for Management Systems in Laboratories
other compounds soluble in the solvent. Engaged in Analysis of Water
D2777 Practice for Determination of Precision and Bias of
1.2 The method is applicable to measurement of the light
Applicable Test Methods of Committee D19 on Water
fuel although loss of some light ends during extraction can be
D5810 Guide for Spiking into Aqueous Samples
expected.
D5847 Practice for Writing Quality Control Specifications
1.3 This method defines oil and grease in water and waste-
for Standard Test Methods for Water Analysis
water as that which is extractable in the test method and
E168 Practices for General Techniques of Infrared Quanti-
measured by IR absorption at 2930 cm- or 3.4 microns.
tative Analysis
Similarly, this test method defines nonpolar material in water
E178 Practice for Dealing With Outlying Observations
and wastewater as that oil and grease which is not adsorbed by
silica gel in the test method and measured by IR absorption at 3. Terminology
2930 cm- .
3.1 Definitions—For definitions of terms used in this test
1.4 This method covers the range of 5 to 100 mg/Land may method, refer to Terminology D1129 and Practices E168.
be extended to a lower or higher level by extraction of a larger
3.2 Definitions of Terms Specific to This Standard:
or smaller sample volume collected separately.
3.2.1 oil and grease—the organic matter extracted from
1.5 The values stated in SI units are to be regarded as
water or wastewater and measured by this test method.
standard. No other units of measurement are included in this
3.2.2 nonpolar material—the oil and grease remaining in
standard.
solution after contact with silica gel and measured by this test
1.6 This standard does not purport to address all of the method.
safety problems, if any, associated with its use. It is the
3.2.3 solvent—dimer/trimer of chlorotrifluoroethylene (S-
responsibility of the user of this standard to establish appro-
316)
priatesafetyandhealthpracticesanddetermine(D3856Guide
for Good Laboratory Practices)the applicability of regulatory 4. Summary of Test Method
limitations prior to use.
4.1 An acidified 250-mL sample of water or wastewater is
extracted serially with three 15-mLvolumes of dimer/trimer of
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2011. Published June 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ε1
approved in 2004. Last previous edition approved in 2004 as D7066 – 04 . DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7066-04R11. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7066−04 (2011)
chlorotrifluoroethylene (S-316).The extract is diluted to 50mL 7.11 Repeating pipetter, glass, 15-mL, (optional).
and a portion is examined by infrared spectroscopy (IR) for an
7.12 Volumetric Pipettes, glass, various (0.50, 1.00, 5.00,
oil and grease measurement. A portion of the extract is
10.0 and 25.0-mL, including a 1.00 serological pipet graduated
contacted with silica gel to remove polar substances, thereby
in 0.01-mL increments and a 5.00-mL serological pipet gradu-
producing a solution containing nonpolar material. The non-
ated in 0.1-mL increments, or equivalent).
polar material is measured by infrared spectroscopy.
7.13 Benchtop shaker, (optional).
5. Significance and Use
7.14 Glass Stirring Rod, (optional).
5.1 The presence and concentration of oil and grease in
7.15 Analytical Balance.
domestic and industrial wastewater is of concern to the public
7.16 Syringes, 50 and 500 mL.
because of its deleterious aesthetic effect and its impact on
aquatic life.
8. Reagents
5.2 Regulations and standards have been established that
8.1 Purity of Reagents—Reagent grade chemicals shall be
require monitoring of oil and grease in water and wastewater.
used in all tests. Unless otherwise indicated, it is intended that
6. Interferences allreagentsshallconformtothespecificationoftheCommittee
on Analytical Reagents of the American Chemical Society,
6.1 Soaps, detergents, surfactants and other materials may
where such specifications are available. Other grades may be
form emulsions that may reduce the amount of oil and grease
used, provided it is first ascertained that the reagent is of
extracted from a sample. This test method contains procedures
sufficiently high purity to permit its use without lessening the
that can assist the analyst in breaking such emulsions.
accuracy of the determination.
6.2 Organic compounds and other materials not considered
8.2 Purity of Water—Unless otherwise indicated, references
as oil and grease on the basis of chemical structure may be
to laboratory or reagent water shall be understood to mean
extracted and measured as oil and grease. Of those measured,
reagent water conforming to Specification D1193, Type II.
certain ones may be adsorbed by silica gel while others may
not. Those not adsorbed are measured as nonpolar material.
8.3 Isooctane (2,2,4-trimethylpentane) 98 % minimum
purity, for use in calibration.
7. Apparatus
8.4 Octanoic Acid 98 % minimum purity, for use in calibra-
All glassware that will come in contact with the sample
tion.
must be rinsed with dimer/trimer of chlorotrifluoroethylene
(S-316) prior to beginning this procedure. 8.5 Silica Gel, Anhydrous, 75 - 150 micrometers, Davisil
Grade 923 (Supelco 21447-7A, or equivalent). Dry at
7.1 Cell(s), quartz, 10-mm path length (lower concentra-
200–250°C for 24 hour minimum and store in a desiccator or
tions may require a longer pathlength), two required for
tightly sealed container. Determine the dimer/trimer of chloro-
double-beam operation, one required for single-beam
trifluoroethylene (S-316) soluble material content of the silica
operation, or built-in or drop-in cell for infrared filtometer
gel by extracting 10 g of silica gel with 25 mLof dimer/trimer
analyzer operation.
of chlorotrifluoroethylene (S-316) and collect the elute in a
7.2 Filter Paper, ashless, quantitative, general-purpose, 11-
flask. Filter and fill a quartz cell for analysis by IR. The
cm, Whatman #40 or equivalent.
dimer/trimer of chlorotrifluoroethylene (S-316) soluble mate-
7.3 Glass Funnel. rial must be less than 5 mg/L.
7.4 Glass Wide Mouth Sample Bottle, minimum 250-mL,
8.6 Sodium Sulfate (Na SO ), ACS, granular anhydrous.
2 4
with screw cap having a fluoropolymer liner. Dry at 200-250 °C for 24 hours minimum and store in a tightly
sealed container until use. (Note: Powdered sodium sulfate
7.5 Glass Graduated Cylinder, 100-mL
should not be used because water may cause it to solidify.)
7.6 Infrared Spectrometer, double-beam dispersive, single-
8.7 Solvent - dimer/trimer of chlorotrifluoroethylene,IR
beam dispersive, Fourier transform, filtometers or other ca-
spectroscopy grade, for example S-316 manufactured by
pable of making measurements at 2930 cm- .
HoribaInstruments,IrvineCA,800-446-7422(ASTMdoesnot
7.7 Magnetic Stirrer, with small TFE-fluorocarbon stirring
advocate the use of one vendor over another)
bar.
8.8 Sulfuric Acid (1 + 1)—Slowly and carefully add 1
7.8 Glass Separatory-Funnel, 500mL, with fluoropolymer
volume of sulfuric acid (H SO , sp gr 1.84) to 1 volume of
2 4
stopcock and stopper.
water, stirring and cooling the solution during the addition
7.9 Volumetric Flasks, glass, various (10, 25, 50, 100, and
(optional HCl replacement).
200-mL).
8.9 Hydrochloric acid,ACS,1+1.Mix equal volumes of
7.10 Teflon spritz bottle, one-piece wash bottle for rinsing.
concentrated HCl and water
8.10 Sodium Chloride (NaCl), crystalline, ACS—or use in
breaking emulsions, if needed. Wet thoroughly with solvent
Consult the manufacturer’s operation manual for the specific instructions
related to the infrared spectrometer or analyzer to be used. before using.
D7066−04 (2011)
and between laboratories with different wastewater matrices, calibration
9. Sampling
with the known oil and grease in a sample should not be used in this
9.1 Collect the sample in accordance with the principles
method.
described in Practices D3370, using a glass bottle equipped
10.1 Calibration and Solvent Mixtures:
with a screw cap having a fluoropolymer liner. Prerinse the
NOTE 2—The calibration procedure below calls for transferring, by
sample bottle and cap with the solvent prior to sample
pipette or syringe, a volume of standard into a volumetric flask to obtain
collection. Do not rinse the sample bottle with the sample to be
a desired concentration. Transfer volumes have been rounded for ease of
analyzed. Fill bottle with minimal headspace to prevent loss of
measurement and calculation. It is highly recommended that calibration
volatile constituants. Do not allow the sample to overflow the
standards be prepared on a weight basis (that is, pipette a volume into a
bottle during collection. Preventing overflow may not be
tared flask and weigh the amount pipetted), then converted to mg/mL by
using the densities of octanoic acid (0.9100 g/mL) and isooctane (0.6920
possible in all sampling situations, however, measures should
g/mL). A solution containing equal volumes of isooctane and octanoic
be taken to minimize overflow at all times.
acid will have a density of 0.801 g/mL.To assure the most accurate
9.2 A sample of about 250mL is required for this test. Use
concentrations, use the smallest serological pipet or syringe for
the entire sample because removing a portion would not 1
measurements. The volume should always be greater than ⁄2
apportion the oil and grease that adheres to the bottle surfaces.
the volume of the pipet or syringe.
The high probability that extractable matter may adhere to
Ideally,alinearcalibrationcurvewillbeobtainedfromthese
samplingequipmentandresultinmeasurementsthatarebiased
standards. As discussed in Section 11, the concentrations of
low precludes the collection of composite samples for deter-
these standards can be adjusted to stay within the linear range
mination of oil and grease. Therefore, samples must be
of the IR instrument.
collected as grab samples. If a composite measurement is
10.1.1 Calibration Stock Solution—Place 0.55 mL of oc-
required, individual grab samples collected at prescribed time
tanoic acid and 0.72 mL of isooctane in a 10-mL volumetric
intervals may be analyzed separately and the concentrations
flask and fill to the mark with solvent. Mix well. The resulting
averaged. Alternatively, samples can be collected in the field
concentration is 50 mg/mL each octanoic acid and isooctane
and composited in the laboratory. For example, collect four
(100 mg/mLtotal oil and grease). This solution will be termed
individual 63-mL samples over the course of a day. In the
“Stock Solution”.
laboratory, pour each 63-mLsample into the separatory funnel,
10.1.2 Diluted Stock Solution—Place 2.5 mL of the Stock
rinse each of the four bottles (and caps) sequentially with
Solution to a 50-mL volumetric flask and fill to mark with
10mLofsolvent,andusethesolventfortheextraction(Section
solvent. Diluted Stock Solution = 5.0 mg/mL (5000 µg/mL).
12.2.2). Do not exceed 50 mL of total solvent during the
10.1.3 Calibration Solution A—Place 1.0 mL of Diluted
extraction and rinse procedure.
Stock Solution in a 10-mLvolumetric flask and fill to the mark
9.3 Preserve the sample with a sufficient quantity of either
withsolvent.CalibrationSolutionA=0.5mg/mL(500µg/mL),
sulfuric(seeSection8.8)orhydrochloricacid(seeSection8.9)
equivalent to 100 mg/L oil and grease in a 250-mL water
to a pH of 2 or lower and refrigerate at 0-4°C from the time of
sample extracted into a 50-mL volume of solvent.
collection until extraction.The amount of acid required will be
10.1.4 Calibration Solution B—Place 0.50 mL of Diluted
dependentuponthepHandbuffercapacityofthesampleatthe
Stock Solution in a 10-mLvolumetric flask and fill to the mark
time of collection. If the amount of acid required is not known,
with solvent. Calibration Solution B = 0.25 mg/mL (250
makethepHmeasurementonaseparatesamplethatwillnotbe
µg/mL), equivalent to 50 mg/L oil and grease in a 250-mL
analyzed. Introduction of pH paper to an actual sample or
water sample extracted into a 50-mL volume of solvent.
sample cap may remove some oil from the sample. To more
10.1.5 Calibration Solution C—Place 0.20 mL of Diluted
accurately calculate the final oil concentration of the extract,
Stock Solution in a 10-mLvolumetric flask and fill to the mark
the volume of acid added to each sample can be recorded, then
with solvent. Calibration Solution C = 0.1 mg/mL (100
subtracted from the final measured sample volume.
µg/mL), equivalent to 20 mg/L of oil and grease in a 250-mL
If the sample is to be shipped by commercial carrier, U.S.
water sample extracted into a 50-mL solvent volume.
Department of Transportation regulations limit the pH to a
10.1.6 Calibration Solution D—Place 0.10 mL of Diluted
minimum (see 40CFR Part 136, Table II Footnote 3) of 1.96 if
Stock Solution in a 10-mLvolumetric flask and fill to the mark
HCl is used and 1.15 if H SO is used (see 49 CFR part 172).
2 4 with solvent. Calibration Solution D = 0.050 mg/mL (50
Collectanadditional1or2samplealiquotsforthematrixspike
µg/mL), equivalent to 10 mg/L of oil and grease in a 250-mL
and matrix spike duplicate (Section 14.5) and preserve with
water sample extracted into a 50-mL solvent volume.
acid.
10.1.7 Calibration Solution E—Place 0.05 mL of Diluted
Stock Solution in a
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