ASTM D7575-11 (2024) 红外测定法测定无溶剂膜可回收油脂的标准试验方法

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Designation: D7575 −11 (Reapproved 2024)
Standard Test Method for
Solvent-Free Membrane Recoverable Oil and Grease by
Infrared Determination
1
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.
1. Scope
1.1 This test method covers the determination of oil and
grease in produced and waste water samples over the concen-
tration range outlined in Table 1 that can be extracted with an
infrared-amenable membrane and measured by infrared trans-
mission through the membrane.
1.2 This test method deﬁnes oil and grease in water as that
which is extractable in this 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 appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
D1129 Terminology Relating to Water
D1193 Speciﬁcation for Reagent Water
D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
D5847 Practice for Writing Quality Control Speciﬁcations
for Standard Test Methods for Water Analysis
E168 Practices for General Techniques of Infrared Quanti-
tative Analysis
E178 Practice for Dealing With Outlying Observations
2.2 EPA Standards:
3
EPA Method 1664 Revision A: N-Hexane Extractable Ma-
terial (HEM; Oil and Grease) and Silica Gel Treated
N-Hexane Extractable Material (SGT-HEM; Non-polar
Material) By Extraction and Gravimetry
40 CFR Title 40: Protection of Environment
49 CFR Title 49: Transportation
3. Terminology
3.1 Deﬁnitions:
3.1.1 For deﬁnitions of terms used in this standard, refer to
Terminology D1129 and Practices E168.
3.2 Deﬁnitions of Terms Speciﬁc to This Standard:
3.2.1 extractor, n—a device that contains an infrared-
amenable oil-and-grease solid-phase-extraction-membrane and
directs water ﬂow through the membrane under applied pres-
sure.
3.2.2 oil and grease, n—“membrane-recoverable oil and
grease” is a method-deﬁned analyte; that is, the deﬁnition of
membrane-recoverable oil and grease is dependent on the
procedure used.
3.2.2.1 Discussion—The nature of the oils or greases (or
both), and the presence of recoverable non-oily matter in the
sample will inﬂuence the material measured and interpretation
of results.
4. Summary of Test Method
4.1 This is a performance-based test method and modiﬁca-
tions are allowed to improve performance.
4.2 A sample of water is processed through an extractor.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved April 1, 2024. Published May 2024. Originally
approved 2010. Last current version approved in 2017 as D7575 – 11 (2017). DOI:
10.1520/D7575-11R24.
2
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
the ASTM website.
3
Available from United States Environmental Protection Agency (EPA), William
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1

4.3 The extractor is then sufficiently dried of water so as to

allow infrared analysis.

4.4 The extractor is examined by an infrared analyzer for an

oil and grease measurement.

4.5 Calibrations and data are processed manually or with

appropriate software.

5. Signiﬁcance and Use

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 health, environmental, safety, and

aesthetic effects.

5.2 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 mate-

rials in question may be appropriate.

6. Interferences

6.1 Method interferences may be caused by contaminants in

instrumentation, reagents, glassware, and other apparatus pro-

ducing artifacts. Routine laboratory method blanks will dem-

onstrate all these materials are free from interferences.

6.2 Matrix interference may be caused by contaminants that

are co-extracted from the sample. The extent of matrix inter-

ferences can vary considerably from sample to sample.

6.3 In cases of samples which contain a relatively large

amount of particulate or biological material, processing the

standard 10 mL amount of sample may not be possible. Note 2

and Note 10 discuss how to deal with processing such samples.

NOTE 2—It is important to note that the capture of solid matter on the

extractor does not preclude IR measurement; in the majority of cases there

is sufficient IR throughput to still perform the measurement as described

herein. This is the case with most metal-oxide materials (that is, clay or

sand) and biological material (that is, algae or cellulose). There may of

course be samples encountered wherein the solid matter is not sufficiently

IR transmitting; one example may be a sample containing a large

concentration of metal particulate. In these instances a different measure-

ment technique may be necessary.

7. Apparatus

7.1 Extractor—Device which contains an infrared-amenable

oil and grease solid phase extraction membrane, 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-

dards have the same or similar outward appearance as the

extractor. Each set contains devices with a speciﬁed amount of

oil and grease; set should include seven devices that cover the

reporting range.

7.3 Syringe—A one-time use plastic syringe with low-

extractable components and connection to attach to the

extractor, capable of ﬂowing the sample volume to be pro-

cessed.

7.4 Infrared Instrument—Infrared absorption measurement

instrument; the instrument may be spectroscopic, dispersive,

radiometric, or ﬁltometric-based. This test method was vali-

dated and the detection limit was determined with an ABB

MB3000 FTIR spectrometer

according to 12.4; the detection

limit and reporting range may vary with the instrument chosen

to perform the analysis; the user should perform a detection

limit study as described in 12.4 to determine the MDL and

reporting range when using the chosen instrument.

7.5 Homogenizer—A device capable of sufficiently homog-

enizing a collected sample, if a grab sample is collected and

stored prior to testing; examples are a paint can shaker or table

shaker (optional).

7.6 Fluid Flow Device—A device capable of forcing the

ﬂuid through the extractor, such as a syringe pump (optional).

7.7 Drying System—A system capable of drying the extrac-

tor sufficiently for infrared analysis without compromising

analyte retention; an example is a clean, compressed air line at

80 psi (552 kPa).

8. Reagents and Materials

8.1 Purity of Reagents—Reagent grade chemicals shall be

used in all tests. Unless otherwise indicated, it is intended that

all reagents shall conform to the speciﬁcation of the Committee

on Analytical Reagents of the American Chemical Society,

where such speciﬁcations are available.

Other grades may be

used, provided it is ﬁrst ascertained that the reagent is of

sufficiently high purity to permit its use without lessening the

accuracy of the determination.

40 CFR 136.

The sole source of supply of the apparatus known to the committee at this time

is Orono Spectral Solutions, P/N 1018SPE (US Patent Application number

12/324,688). If you are aware of alternative suppliers, please provide this informa-

tion to ASTM International Headquarters. Your comments will receive careful

consideration at a meeting of the responsible technical committee, which you may

attend.

The sole source of supply of the apparatus known to the committee at this time

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

technical committee, which you may attend.

The ABB MB3000 FTIR spectrometer manufactured by ABB, Ltd., of Zurich,

Switzerland, or equivalent, may be suitable for use.

Reagent Chemicals, American Chemical Society Speciﬁcations, American

Chemical Society, Washington, DC. For Suggestions on the testing of reagents not

listed by the American Chemical Society, see Annual Standards for Laboratory

Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia

and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,

MD.

TABLE 1 Method Detection Limit (MDL) and Reporting Range

Analyte MDL

(mg/L) Reporting Range

(mg/L)

Oil and Grease 1.0 5–200

MDL and recommended reporting range determined by 12.4, which follows the

Code of Federal Regulations, 40 CFR, Part 136, Appendix B; limits should be

determined by each operator.

D7575 − 11 (2024)

8.2 Purity of Water—Unless otherwise indicated, references

to water shall be understood to mean reagent water that meets

the purity speciﬁcations of Type II water, presented in Speci-

ﬁcation D1193.

8.3 Hydrochloric Acid—Concentration of 12.1 M.

8.4 Sulfuric Acid—Concentration of 18.4 M; optional re-

placement for hydrochloric acid for preservation.

8.5 Acetone—ACS, residue less than 1 mg/L.

8.6 Hexadecane—98 % minimum purity.

8.7 Stearic Acid—98 % minimum purity.

9. Hazards

9.1 Normal laboratory safety applies to this test method.

Analysts should wear safety glasses, gloves, and lab coats

when working with acids. Analysts should review the Material

Safety Data Sheets (MSDS) for all reagents used in this test

method. Additional hazards may be presented by the particular

sample being tested so proper care must be taken.

10. Sampling

10.1 Fill the sample container. Do not ﬁll the container to

the brim; sufficient headspace is required to allow vigorous

homogenization. Do not rinse the sample container with the

sample to be analyzed. Do not allow the sample to overﬂow the

container during collection. Preventing overﬂow may not be

possible in all sampling situations; however, measures should

be taken to minimize overﬂow at all times.

NOTE 3—About 5 % to 10 % of volume headspace has been found to be

suitable for homogenization.

10.2 Add a sufficient quantity of either sulfuric (see 8.4) or

hydrochloric acid (see 8.3) to a pH of 2. If analysis is to be

delayed for more than four hours, refrigerate to 6 °C or less,

without freezing, from the time of collection until extraction.

The amount of acid required will be dependent upon the pH

and buffer capacity of the sample at the time of collection. If

the amount of acid required is not known, make the pH

measurement on a separate sample that will not be analyzed.

Introduction of pH paper to an actual sample or sample cap

may remove some oil from the sample. To more accurately

calculate the ﬁnal oil and grease concentration the following

equation can be used:

(1)

where C

is the measured concentration, V

is the sample

volume, V

is the volume of acid added to the sample, and C

is the sample concentration before the acid was added.

10.3 If the sample is to be shipped by commercial carrier,

U.S. Department of Transportation regulations (see 49 CFR,

Part 172) limit the pH to a minimum of 1.96 if HCl is used and

1.15 if H

is used (see 40 CFR, Part 136, Table II, Footnote

3).

NOTE 4—For those circumstances requiring the collection of multiple

aliquots of one sample, each aliquot is to be collected in either of the

following ways: (1) collect simultaneously in parallel, if possible, or (2)

collect as grab samples in rapid succession, ﬁlling

⁄

of each container at

a time and continuing until all containers are 90 % to 95 % full, consistent

with Note 3.

11. Preparation of Apparatus

11.1 Hexadecane and Stearic Acid (1+1) Spiking Solution—

Place 400 mg 64 mg hexadecane and 400 mg 64 mg stearic

acid in a 100 mL volumetric ﬂask and ﬁll to the bottom of the

neck, not to the mark, with acetone.

NOTE 5—The solution may require warming for complete dissolution of

stearic acid.

11.2 After the hexadecane and stearic acid has dissolved,

allow to cool to room temperature and add acetone to the mark.

Stopper the volumetric ﬂask or transfer the solution to a

100 mL to 150 mL vial with ﬂuoropolymer-lined cap. Mark the

solution level on the vial and store in the dark at room

temperature.

11.3 Immediately prior to the ﬁrst use, verify the level on

the vial and bring to volume with acetone, if required. Warm to

redissolve all visible precipitate, if required. If there is doubt of

the concentration, remove 10.0 mL 60.1 mL with a volumet-

ric pipet, place in a tared weighing pan, and evaporate to

dryness in a fume hood. The weight must be 80 mg 61 mg. If

not, prepare a fresh solution (11.1).

11.4 The spiking solutions should be checked frequently for

signs of degradation or evaporation using the test in 11.3.

11.5 If necessary, this solution can be made more or less

concentrated to suit the concentration needed for the matrix

spike (MS). A fresh spiking solution should be prepared

weekly or bi-weekly.

12. Calibration and Standardization

12.1 To ensure analytical values obtained using this test

method are valid and accurate within the conﬁdence limits of

the test, the instrument manufacturer’s instructions and the

following procedures must be followed when performing this

test method.

NOTE 6—Instruments other than FTIR spectrometers may have different

procedures that should be followed according to the manufacturer’s

instructions.

12.2 Calibration is carried out using the set of calibration

standard devices (CSD).

12.2.1 Take a background reference ﬁle through the CSD

labeled “Background” according to the instrument manufac-

turer’s instructions.

12.2.2 Scan each of the other CSDs according to the

instrument manufacturer’s instructions.

12.2.3 Measure and record the absorbance of the peak

centered near 2920 cm

–1

(3.42 µm) according to Practices

E168. The instrument may include automatic measurement

software; if so follow instrument manufacturer’s instructions

for using the software.

NOTE 7—Other peaks associated with the methylene moiety may also

be used; detection limits will be affected so the operator should follow

12.4 to determine the detection limit for the absorbance peaks chosen.

12.2.4 Linear calibration may be used if the coefficient of

determination, r

, is >0.95 for the analyte. If one of the

calibration standards other than the high or low point causes

the r

to be <0.95 this point must be reanalyzed. If the point

still causes the r

to be <0.95, it may be excluded but minimally

D7575 − 11 (2024)

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标签： #红外测定法 #无溶剂膜 #可回收油脂

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ASTM D7575-11 2024 Standard Test Method for Solvent-Free Membrane Recoverable Oil and Grease by Infrared Determination 红外测定法测定无溶剂膜可回收油脂的标准试验方法

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