1、Designation: D7575 11 (Reapproved 2017)Standard Test Method forSolvent-Free Membrane Recoverable Oil and Grease byInfrared Determination1This standard is issued under the fixed designation D7575; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of oil andgrease in produced and waste water sample
3、s over the concen-tration range outlined in Table 1 that can be extracted with aninfrared-amenable membrane and measured by infrared trans-mission through the membrane.1.2 This test method defines oil and grease in water as thatwhich is extractable in this test method and measured byinfrared transmi
4、ssion.1.3 The method detection limit (MDL) and recommendedreporting range are listed in Table 1.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any,
5、 associated with its use. It is theresponsibility 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 international
6、ly recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1129 Termino
7、logy Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE168 Practices for General Techniq
8、ues of Infrared Quanti-tative AnalysisE178 Practice for Dealing With Outlying Observations2.2 EPA Standards:3EPA Method 1664 Revision A: N-Hexane Extractable Ma-terial (HEM; Oil and Grease) and Silica Gel TreatedN-Hexane Extractable Material (SGT-HEM; Non-polarMaterial) By Extraction and Gravimetry4
9、0 CFR Title 40: Protection of Environment49 CFR Title 49: Transportation3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer toTerminology D1129 and Practices E168.3.2 Definitions of Terms Specific to This Standard:3.2.1 extractor, na device that contains an infr
10、ared-amenable oil-and-grease solid-phase-extraction-membrane anddirects water flow through the membrane under applied pres-sure.3.2.2 oil and grease, n“membrane-recoverable oil andgrease” is a method-defined analyte; that is, the definition ofmembrane-recoverable oil and grease is dependent on thepr
11、ocedure used.3.2.2.1 DiscussionThe nature of the oils or greases (orboth), and the presence of recoverable non-oily matter in thesample will influence the material measured and interpretationof results.4. Summary of Test Method4.1 This is a performance-based test method and modifica-tions are allowe
12、d to improve performance.4.2 A sample of water is processed through an extractor.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Dec. 15, 2
13、017. Published December 2017. Originallyapproved 2010. Last current version approved in 2011 as D7575 11. DOI:10.1520/D7575-11R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informat
14、ion, refer to the standards Document Summary page onthe ASTM website.3Available from United States Environmental ProtectionAgency (EPA), WilliamJefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700
15、, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the Wor
16、ld Trade Organization Technical Barriers to Trade (TBT) Committee.14.3 The extractor is then sufficiently dried of water so as toallow infrared analysis.4.4 The extractor is examined by an infrared analyzer for anoil and grease measurement.4.5 Calibrations and data are processed manually or withappr
17、opriate software.5. Significance and Use5.1 The presence and concentration of oil and grease indomestic and industrial wastewater is of concern to the publicbecause of its deleterious health, environmental, safety, andaesthetic effects.5.2 Regulations and standards have been established thatrequire
18、monitoring of oil and grease in water and wastewater.4NOTE 1Different oil and grease materials may have different infraredabsorptivities. Certain materials, such as synthetic silicone-based orperfluorinated oils, may have absoptivities inconsistent with those ofnaturally occurring oil and grease mat
19、erials. Caution should be takenwhen testing matrices suspected of containing proportions of thesematerials. In such cases, laboratory spike samples, laboratory checksamples, equivalency testing, or combinations thereof, using these mate-rials in question may be appropriate.6. Interferences6.1 Method
20、 interferences may be caused by contaminants ininstrumentation, 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 thatare co-extracted
21、 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 largeamount of particulate or biological material, processing thestandard 10 mL amount of sample may not be possible. Note 2and Note 10 discuss how to
22、deal with processing such samples.NOTE 2It is important to note that the capture of solid matter on theextractor does not preclude IR measurement; in the majority of cases thereis sufficient IR throughput to still perform the measurement as describedherein. This is the case with most metal-oxide mat
23、erials (that is, clay orsand) and biological material (that is, algae or cellulose). There may ofcourse be samples encountered wherein the solid matter is not sufficientlyIR transmitting; one example may be a sample containing a largeconcentration of metal particulate. In these instances a different
24、 measure-ment technique may be necessary.7. Apparatus7.1 ExtractorDevice which contains an infrared-amenableoil and grease solid phase extraction membrane, includes aconnection to a syringe, such as a Luer connection, and isdesigned for pressurized flow of water through the membrane.57.2 Calibration
25、 Standard Devices SetCalibration stan-dards have the same or similar outward appearance as theextractor. Each set contains devices with a specified amount ofoil and grease; set should include seven devices that cover thereporting range.67.3 SyringeA one-time use plastic syringe with low-extractable
26、components and connection to attach to theextractor, capable of flowing the sample volume to be pro-cessed.7.4 Infrared InstrumentInfrared absorption measurementinstrument; the instrument may be spectroscopic, dispersive,radiometric, or filtometric-based. This test method was vali-dated and the dete
27、ction limit was determined with an ABBMB3000 FTIR spectrometer7according to 12.4; the detectionlimit and reporting range may vary with the instrument chosento perform the analysis; the user should perform a detectionlimit study as described in 12.4 to determine the MDL andreporting range when using
28、the chosen instrument.7.5 HomogenizerA device capable of sufficiently homog-enizing a collected sample, if a grab sample is collected andstored prior to testing; examples are a paint can shaker or tableshaker (optional).7.6 Fluid Flow DeviceA device capable of forcing thefluid through the extractor,
29、 such as a syringe pump (optional).7.7 Drying SystemA system capable of drying the extrac-tor sufficiently for infrared analysis without compromisinganalyte retention; an example is a clean, compressed air line at80 psi (552 kPa).8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals
30、 shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specification of the Committeeon Analytical Reagents of the American Chemical Society,where such specifications are available.8Other grades may beused, provided it is first ascertained that t
31、he reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.440 CFR 136.5The sole source of supply of the apparatus known to the committee at this timeis Orono Spectral Solutions, P/N 1018SPE (US Patent Application number12/324,688). If you are aware
32、 of alternative suppliers, please provide this informa-tion to ASTM International Headquarters. Your comments will receive carefulconsideration at a meeting of the responsible technical committee, which you mayattend.6The sole source of supply of the apparatus known to the committee at this timeis O
33、rono Spectral Solutions, P/N 1018SPE-CSD. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee, which you may attend.7The ABB MB3000 FTIR spectr
34、ometer manufactured by ABB, Ltd., of Zurich,Switzerland, or equivalent, may be suitable for use.8Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual St
35、andards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Method Detection Limit (MDL) and Reporting RangeAnalyte MDLA(mg/L) Reporting RangeA(mg/L)Oil and Grease 1.0 5200A
36、MDL and recommended reporting range determined by 12.4, which follows theCode of Federal Regulations, 40 CFR, Part 136, Appendix B; limits should bedetermined by each operator.D7575 11 (2017)28.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water
37、that meetsthe purity specifications of Type II water, presented in Speci-fication D1193.8.3 Hydrochloric AcidConcentration of 12.1 M.8.4 Sulfuric AcidConcentration of 18.4 M; optional re-placement for hydrochloric acid for preservation.8.5 AcetoneACS, residue less than 1 mg/L.8.6 Hexadecane98 % mini
38、mum purity.8.7 Stearic Acid98 % minimum purity.9. Hazards9.1 Normal laboratory safety applies to this test method.Analysts should wear safety glasses, gloves, and lab coatswhen working with acids. Analysts should review the MaterialSafety Data Sheets (MSDS) for all reagents used in this testmethod.
39、Additional hazards may be presented by the particularsample being tested so proper care must be taken.10. Sampling10.1 Fill the sample container. Do not fill the container tothe brim; sufficient headspace is required to allow vigoroushomogenization. Do not rinse the sample container with thesample t
40、o be analyzed. Do not allow the sample to overflow thecontainer during collection. Preventing overflow may not bepossible in all sampling situations; however, measures shouldbe taken to minimize overflow at all times.NOTE 3About 510 % of volume headspace has been found to besuitable for homogenizati
41、on.10.2 Add a sufficient quantity of either sulfuric (see 8.4)orhydrochloric acid (see 8.3) to a pH of 2. If analysis is to bedelayed for more than four hours, refrigerate to 6C or less,without freezing, from the time of collection until extraction.The amount of acid required will be dependent upon
42、the pHand buffer capacity of the sample at the time of collection. Ifthe amount of acid required is not known, make the pHmeasurement on a separate sample that will not be analyzed.Introduction of pH paper to an actual sample or sample capmay remove some oil from the sample. To more accuratelycalcul
43、ate the final oil and grease concentration the followingequation can be used:CS5 Ci3 VS1VA!/VS(1)where Ciis the measured concentration, VSis the samplevolume, VAis the volume of acid added to the sample, and CSis the sample concentration before the acid was added.10.3 If the sample is to be shipped
44、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 and1.15 if H2SO4is used (see 40 CFR, Part 136, Table II, Footnote3).NOTE 4For those circumstances requiring the collection of multiplealiquots of one sample, eac
45、h aliquot is to be collected in either of thefollowing ways: (1) collect simultaneously in parallel, if possible, or (2)collect as grab samples in rapid succession, filling13 of each container ata time and continuing until all containers are 9095 % full, consistent withNote 3.11. Preparation of Appa
46、ratus11.1 Hexadecane and Stearic Acid (1+1) Spiking SolutionPlace 400 mg 64 mg hexadecane and 400 mg 64 mg stearicacid in a 100-mL volumetric flask and fill to the bottom of theneck, not to the mark, with acetone.NOTE 5The solution may require warming for complete dissolution ofstearic acid.11.2 Aft
47、er 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 a100150 mL vial with fluoropolymer-lined cap. Mark thesolution level on the vial and store in the dark at roomtemperature.11.3 Immed
48、iately prior to the first use, verify the level onthe vial and bring to volume with acetone, if required. Warm toredissolve all visible precipitate, if required. If there is doubt ofthe concentration, remove 10.0 6 0.1 mL with a volumetricpipet, place in a tared weighing pan, and evaporate to drynes
49、sin a fume hood. The weight must be 80 6 1 mg. If not, preparea fresh solution (11.1).11.4 The spiking solutions should be checked frequently forsigns of degradation or evaporation using the test in 11.3.11.5 If necessary, this solution can be made more or lessconcentrated to suit the concentration needed for the matrixspike (MS). A fresh spiking solution should be preparedweekly or bi-weekly.12. Calibration and Standardization12.1 To ensure analytical values obtained using this testmethod are valid and accurate within the confidence limits ofthe test,
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