Standard Test Method for Solvent-Free Membrane Recoverable Oil and Grease 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 health, environmental, safety, and aesthetic effects.
Regulations and standards have been established that require monitoring of oil and grease in water and wastewater.  
Note 1—Different oil and grease materials may have different infrared absorptivities. Certain materials, such as synthetic silicone-based or perfluorinated oils, may have absoptivities inconsistent with those of naturally occurring oil and grease materials. Caution should be taken when testing matrices suspected of containing proportions of these materials. In such cases, laboratory spike samples, laboratory check samples, equivalency testing, or combinations thereof, using these materials in question may be appropriate.
SCOPE
1.1 This test method covers the determination of oil and grease in water extracted with an infrared-amenable membrane and measured by infrared transmission through the membrane.
1.2 This method defines oil and grease in water as that which is extractable in the test method and measured by infrared transmission.
1.3 The method detection limit (MDL) and recommended reporting range are listed in Table 1.
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.

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Historical
Publication Date
31-Dec-2009
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ASTM D7575-10 - Standard Test Method for Solvent-Free Membrane Recoverable Oil and Grease by Infrared Determination
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D7575–10
Standard Test Method for
Solvent-Free Membrane Recoverable Oil and Grease by
Infrared Determination
This standard is issued under the fixed designation D7575; 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.
TABLE 1 MDL and Reporting Range
1. Scope
A A
Analyte MDL (mg/L) Reporting Range (mg/L)
1.1 This test method covers the determination of oil and
Oil and Grease 1.0 5–200
grease in water extracted with an infrared-amenable membrane
A
and measured by infrared transmission through the membrane. MDL and recommended reporting range determined by Section 12.4, which
follows the Code of Federal Regulations, 40 CFR Part 136, Appendix B; limits
1.2 This method defines oil and grease in water as that
should be determined by each operator.
which is extractable in the test method and measured by
infrared transmission.
1.3 The method detection limit (MDL) and recommended
2.2 EPA Standards
reporting range are listed in Table 1.
EPA Method 1664 Revision A: N-Hexane Extractable Ma-
1.4 The values stated in SI units are to be regarded as
terial (HEM; Oil and Grease) and Silica Gel Treated
standard. No other units of measurement are included in this
N-Hexane Extractable Material (SGT-HEM; Non-polar
standard.
Material) By Extraction and Gravimetry
1.5 This standard does not purport to address all of the
40 CFR
safety concerns, if any, associated with its use. It is the
49 CFR
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
3.1 Definitions: For definitions of terms used in this test
method, refer to Terminology D1129 and Practices E168.
2. Referenced Documents
3.2 Definitions of Terms Specific to This Standard:
2.1 ASTM Standards:
3.2.1 oil and grease, n—“membrane-recoverable oil and
D1129 Terminology Relating to Water
grease” is a method-defined analyte; that is, the definition of
D1193 Specification for Reagent Water
membrane-recoverable oil and grease is dependent on the
D2777 Practice for Determination of Precision and Bias of
procedure used.
Applicable Test Methods of Committee D19 on Water
3.2.1.1 Discussion—The nature of the oils or greases (or
D5847 Practice for Writing Quality Control Specifications
both), and the presence of recoverable non-oily matter in the
for Standard Test Methods for Water Analysis
sample will influence the material measured and interpretation
E168 Practices for General Techniques of Infrared Quanti-
of results.
tative Analysis
3.2.2 extractor, n—a device that contains an infrared-
E178 Practice for Dealing With Outlying Observations
amenable oil-and-grease solid-phase-extraction-membrane and
directs water flow through the membrane under applied pres-
sure.
4. Summary of Test Method
4.1 This is a performance-based method and modifications
This test method is under the jurisdiction of ASTM Committee D19 on Water
are allowed to improve performance.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water. 4.2 A sample of water is processed through an extractor.
Current edition approved Jan. 1, 2010. Published January 2010. DOI: 10.1520/
D7575-10.
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 Available from United States Environmental Protection Agency (EPA), Ariel
Standards volume information, refer to the standard’s Document Summary page on Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://
the ASTM website. www.epa.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7575–10
4.3 The extractor is then sufficiently dried of water so as to extractor. Each set contains devices with a specified amount of
allow infrared analysis. oil and grease; set should include seven devices that cover the
4.4 The extractor is examined by an infrared analyzer for an reporting range.
oil and grease measurement.
7.3 Syringe—A one-time use plastic syringe with low-
4.5 Calibrations and data are processed manually or with
extractable components and connection to attach to the extrac-
appropriate software.
tor, capable of flowing the sample volume to be processed.
7.4 Infrared Instrument—Infrared absorption measurement
5. Significance and Use
instrument; the instrument may be spectroscopic, dispersive,
5.1 The presence and concentration of oil and grease in
radiometricorfiltometricbased.Themethodwasvalidatedand
domestic and industrial wastewater is of concern to the public
the detection limit was determined with an MB3000 FTIR
because of its deleterious health, environmental, safety, and
spectrometer manufactured by ABB according to 12.4; the
aesthetic effects.
detection limit and reporting range may vary with the instru-
5.2 Regulations and standards have been established that
ment chosen to perform the analysis; the user should perform
require monitoring of oil and grease in water and wastewater.
a detection limit study as described in 12.4 to determine the
method detection limit and reporting range when using the
NOTE 1—Different oil and grease materials may have different infrared
absorptivities. Certain materials, such as synthetic silicone-based or chosen instrument.
perfluorinated oils, may have absoptivities inconsistent with those of
7.5 Homogenizer—Adevice capable of sufficiently homog-
naturally occurring oil and grease materials. Caution should be taken
enizing a collected sample, if a grab sample is collected and
when testing matrices suspected of containing proportions of these
stored prior to testing; examples are a paint can shaker or table
materials. In such cases, laboratory spike samples, laboratory check
shaker (optional).
samples, equivalency testing, or combinations thereof, using these mate-
7.6 Fluid Flow Device—A device capable of forcing the
rials in question may be appropriate.
fluid through the extractor, such as a syringe pump (optional).
6. Interferences
7.7 Drying System—Asystem capable of drying the extrac-
6.1 Method interferences may be caused by contaminants in
tor sufficiently for infrared analysis without compromising
instrumentation, reagents, glassware and other apparatus pro-
analyte retention; an example is a clean, compressed air line at
ducing artifacts. Routine laboratory method blanks will dem-
80 psi (552 kPa).
onstrate all these materials are free from interferences.
6.2 Matrix interference may be caused by contaminants that
8. Reagents and Materials
are co-extracted from the sample. The extent of matrix inter-
8.1 Purity of Reagents—Reagent grade chemicals shall be
ferences can vary considerably from sample to sample.
used in all tests. Unless otherwise indicated, it is intended that
6.3 In cases of samples which contain a relatively large
allreagentsshallconformtothespecificationoftheCommittee
amount of particulate or biological material, processing the
on Analytical Reagents of the American Chemical Society,
standard 10 mLamount of sample may not be possible. Note 2
where such specifications are available. Other grades may be
andNote10discusshowtodealwithprocessingsuchsamples.
used, provided it is first ascertained that the reagent is of
NOTE 2—It is important to note that the capture of solid matter on the sufficiently high purity to permit its use without lessening the
extractordoesnotprecludeIRmeasurement;inthemajorityofcasesthere
accuracy of the determination.
is sufficient IR throughput to still perform the measurement as described
8.2 Purity of Water—Unless otherwise indicated, references
herein. This is the case with most metal-oxide materials (that is, clay or
to water shall be understood to mean reagent water that meets
sand) and biological material (that is, algae or cellulose). There may of
the purity specifications of Type II water, presented in Speci-
course be samples encountered wherein the solid matter is not sufficiently
fication D1193.
IR transmitting; one example may be a sample containing a large
concentration of metal particulate. In these instances a different measure-
8.3 Hydrochloric Acid—Concentration of 12.1 M.
ment technique may be necessary.
8.4 Sulfuric Acid—Concentration of 18.4 M; optional re-
placement for hydrochloric acid for preservation.
7. Apparatus
8.5 Acetone—ACS, residue less than 1 mg/L.
7.1 Extractor—Device which contains an infrared-
8.6 Hexadecane—98 % minimum purity.
amenable oil and grease solid phase extraction membrane,
8.7 Stearic Acid—98 % minimum purity.
includes a connection to a syringe, such as a Luer connection,
and is designed for pressurized flow of water through the
membrane.
7.2 Calibration Standard Devices Set—Calibration stan-
The sole source of supply of the apparatus known to the committee at this time
dards have the same or similar outward appearance as the
is Orono Spectral Solutions, P/N 1018SPE-CSD. If you are aware of alternative
suppliers, please provide this information to ASTM International Headquarters.
Your comments will receive careful consideration at a meeting of the responsible
40 CFR 136 technical committee, which you may attend.
5 7
The sole source of supply of the apparatus known to the committee at this time Reagent Chemicals, American Chemical Society Specifications, American
is Orono Spectral Solutions, P/N 1018SPE (US Patent Application number Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
12/324,688). If you are aware of alternative suppliers, please provide this informa- listed by the American Chemical Society, see Annual Standards for Laboratory
tion to ASTM International Headquarters. Your comments will receive careful Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
consideration at a meeting of the responsible technical committee, which you may and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
attend. MD.
D7575–10
9. Hazards 100–150 mL vial with fluoropolymer-lined cap. Mark the
solution level on the vial and store in the dark at room
9.1 Normal laboratory safety applies to this method. Ana-
temperature.
lysts should wear safety glasses, gloves, and lab coats when
11.3 Immediately prior to the first use, verify the level on
workingwithacids.AnalystsshouldreviewtheMaterialSafety
the vial and bring to volume with acetone, if required.Warm to
Data Sheets (MSDS) for all reagents used in this method.
redissolveallvisibleprecipitate,ifrequired.Ifthereisdoubtof
Additional hazards may be presented by the particular sample
the concentration, remove 10.0 6 0.1 mL with a volumetric
being tested so proper care must be taken.
pipet, place in a tared weighing pan, and evaporate to dryness
in a fume hood.The weight must be 80 6 1 mg. If not, prepare
10. Sampling
a fresh solution (Section 11.1).
10.1 Fill the sample container. Do not fill the container to
11.4 The spiking solutions should be checked frequently for
the brim; sufficient headspace is required to allow vigorous
signs of degradation or evaporation using the test in Section
homogenization. Do not rinse the sample container with the
11.3.
sampletobeanalyzed.Donotallowthesampletooverflowthe
11.5 If necessary, this solution can be made more or less
container during collection. Preventing overflow may not be
concentrated to suit the concentration needed for the matrix
possible in all sampling situations; however, measures should
spike. A fresh spiking solution should be prepared weekly or
be taken to minimize overflow at all times.
bi-weekly.
NOTE 3—About 5–10 % of volume headspace has been found to be
12. Calibration and Standardization
suitable for homogenization.
12.1 To ensure analytical values obtained using this test
10.2 Add a sufficient quantity of either sulfuric (see Section
method are valid and accurate within the confidence limits of
8.4) or hydrochloric acid (see Section 8.3)toapHof2.If
the test, the instrument manufacturer’s instructions and the
analysis is to be delayed for more than four hours, refrigerate
following procedures must be followed when performing the
to 6°C or less, without freezing, from the time of collection
test method.
untilextraction.Theamountofacidrequiredwillbedependent
upon the pH and buffer capacity of the sample at the time of
NOTE 6—Instruments other than FTIR spectrometers may have differ-
collection. If the amount of acid required is not known, make ent procedures that should be followed according to the manufacturer’s
instructions.
the pH measurement on a separate sample that will not be
analyzed. Introduction of pH paper to an actual sample or
12.2 Calibration is carried out using the set of calibration
sample cap may remove some oil from the sample. To more
standard devices (CSD).
accurately calculate the final oil and grease concentration the
12.2.1 Take a background reference file through the CSD
following equation can be used:
labeled “Background” according to the instrument manufac-
turer’s instructions.
C 5 C 3 ~V 1V !/ V (1)
S i S A S
12.2.2 Scan each of the other CSDs according to the
where C is the measured concentration, V is the sample
i S
instrument manufacturer’s instructions.
volume, V is the volume of acid added to the sample, and C
A S
12.2.3 Measure and record the absorbance of the peak
is the sample concentration before the acid was added.
–1
centered near 2920 cm (3.42 micron) according to Practices
10.3 If the sample is to be shipped by commercial carrier,
E168. The instrument may include automatic measurement
U.S. Department of Transportation regulations (see 49 CFR
software; if so follow instrument manufacturer’s instructions
part 172) limit the pH to a minimum of 1.96 if HCl is used and
for using the software.
1.15 if H SO is used. (see 40 CFR Part 136,Table II Footnote
2 4
NOTE 7—Other peaks associated with the methylene moiety may also
3).
be used; detection limits will be affected so the operator should follow
NOTE 4—For those circumstances requiring the collection of multiple Section 12.4 to determine the detection limit for the absorbance peaks
aliquots of one sample, each aliquot is to be collected in either of the chosen.
following ways: (1) collect simultaneously in parallel, if possible, or (2)
12.2.4 Linear calibration may be used if the coefficient of
collect as grab samples in rapid succession, filling ⁄3 of each container at
determination, r , is >0.95 for the analyte
...

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