ASTM D7575-2010 6875 Standard Test Method for Solvent-Free Membrane Recoverable Oil and Grease by Infrared Determination.pdf

1、Designation: D7575 10Standard 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 of revision, the y

2、ear 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 water extracted with an infrared-amenable membran

3、eand measured by infrared transmission through the membrane.1.2 This method defines oil and grease in water as thatwhich is extractable in the test method and measured byinfrared transmission.1.3 The method detection limit (MDL) and recommendedreporting range are listed in Table 1.1.4 The values sta

4、ted 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, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety an

5、d health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee

6、D19 on WaterD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE178 Practice for Dealing With Outlying Observations2.2 EPA Standards3EPA Method 1664 Revision A: N-Hexane Extracta

7、ble Ma-terial (HEM; Oil and Grease) and Silica Gel TreatedN-Hexane Extractable Material (SGT-HEM; Non-polarMaterial) By Extraction and Gravimetry40 CFR49 CFR3. Terminology3.1 Definitions: For definitions of terms used in this testmethod, refer to Terminology D1129 and Practices E168.3.2 Definitions

8、of Terms Specific to This Standard:3.2.1 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 theprocedure used.3.2.1.1 DiscussionThe nature of the oils or greases (orboth), and the presence o

9、f recoverable non-oily matter in thesample will influence the material measured and interpretationof results.3.2.2 extractor, na device that contains an infrared-amenable oil-and-grease solid-phase-extraction-membrane anddirects water flow through the membrane under applied pres-sure.4. Summary of T

10、est Method4.1 This is a performance-based method and modificationsare allowed to improve performance.4.2 A sample of water is processed through an extractor.4.3 The extractor is then sufficiently dried of water so as toallow infrared analysis.4.4 The extractor is examined by an infrared analyzer for

11、 anoil and grease measurement.4.5 Calibrations and data are processed manually or withappropriate 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, saf

12、ety, andaesthetic effects.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 Jan. 1, 2010. Published January 2010.2For referenced ASTM standar

13、ds, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from United States Environmental Protection Agency (EPA), ArielRios Bldg., 120

14、0 Pennsylvania Ave., NW, Washington, DC 20460, http:/www.epa.gov.TABLE 1 MDL and Reporting RangeAnalyte MDLA(mg/L) Reporting RangeA(mg/L)Oil and Grease 1.0 5200AMDL and recommended reporting range determined by Section 12.4, whichfollows the Code of Federal Regulations, 40 CFR Part 136, Appendix B;

15、limitsshould be determined by each operator.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Regulations and standards have been established thatrequire monitoring of oil and grease in water and wastewater.4NOTE 1Different oil and

16、 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 materials. Caution should be takenwhen testing matrices suspected of containing

17、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 interferences may be caused by contaminants ininstrumentation, reagents, gla

18、ssware 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 from the sample. The extent of matrix inter-ferences can vary considerably fr

19、om 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 deal with processing such samples.NOTE 2It is important to note that the captu

20、re 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 materials (that is, clay orsand) and biological material (that is, algae or cellu

21、lose). 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 measure-ment technique may be necessary.7. Apparatus7.1 ExtractorDevice which

22、 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 themembrane.57.2 Calibration Standard Devices SetCalibration stan-dards have the same or similar outward a

23、ppearance 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 components and connection to attach to the extrac-tor, capable of flowing the

24、sample volume to be processed.7.4 Infrared InstrumentInfrared absorption measurementinstrument; the instrument may be spectroscopic, dispersive,radiometric or filtometric based. The method was validated andthe detection limit was determined with an MB3000 FTIRspectrometer manufactured by ABB accordi

25、ng to 12.4; thedetection limit and reporting range may vary with the instru-ment chosen to perform the analysis; the user should performa detection limit study as described in 12.4 to determine themethod detection limit and reporting range when using thechosen instrument.7.5 HomogenizerA device capa

26、ble 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, such as a syringe pump (optional).7.7 Drying Syst

27、emA 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 shall beused in all tests. Unless otherwise indic

28、ated, 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.7Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit

29、 its use without lessening theaccuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water that meetsthe purity specifications of Type II water, presented in Speci-fication D1193.8.3 Hydrochloric AcidConcentration of 12.1 M

30、.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 % minimum purity.8.7 Stearic Acid98 % minimum purity.9. Hazards9.1 Normal laboratory safety applies to this method. Ana-lysts should wear

31、safety glasses, gloves, and lab coats whenworking with acids.Analysts should review the Material SafetyData Sheets (MSDS) for all reagents used in this method.Additional hazards may be presented by the particular samplebeing tested so proper care must be taken.10. Sampling10.1 Fill the sample contai

32、ner. Do not fill the container tothe brim; sufficient headspace is required to allow vigoroushomogenization. Do not rinse the sample container with thesample to be analyzed. Do not allow the sample to overflow the440 CFR 1365The sole source of supply of the apparatus known to the committee at this t

33、imeis Orono Spectral Solutions, P/N 1018SPE (US Patent Application number12/324,688). If you are aware 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, w

34、hich you mayattend.6The sole source of supply of the apparatus known to the committee at this timeis Orono 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 consideratio

35、n at a meeting of the responsibletechnical committee, which you may attend.7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for Laborator

36、yChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D7575 102container during collection. Preventing overflow may not bepossible in all sampling situations; however, measures shouldbe taken to m

37、inimize overflow at all times.NOTE 3About 510 % of volume headspace has been found to besuitable for homogenization.10.2 Add a sufficient quantity of either sulfuric (see Section8.4) or hydrochloric acid (see Section 8.3)toapHof2.Ifanalysis is to be delayed for more than four hours, refrigerateto 6C

38、 or less, without freezing, from the time of collectionuntil extraction. The amount of acid required will be dependentupon the pH and buffer capacity of the sample at the time ofcollection. If the amount of acid required is not known, makethe pH measurement on a separate sample that will not beanaly

39、zed. Introduction of pH paper to an actual sample orsample cap may remove some oil from the sample. To moreaccurately calculate the final oil and grease concentration thefollowing equation can be used:CS5 Ci3 VS1VA! / VS(1)where Ciis the measured concentration, VSis the samplevolume, VAis the volume

40、 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 by commercial carrier,U.S. Department of Transportation regulations (see 49 CFRpart 172) limit the pH to a minimum of 1.96 if HCl is used and1.15 if H2SO4is used. (see 40 CFR

41、 Part 136, Table II Footnote3).NOTE 4For those circumstances requiring the collection of multiplealiquots of one sample, each 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 o

42、f each container ata time and continuing until all containers are 9095 % full, consistent withNote 3.11. Preparation of Apparatus11.1 Hexadecane and Stearic Acid (1+1) SpikingSolutionPlace 400 mg 64 mg hexadecane and 400 mg 64mg stearic acid in a 100-mL volumetric flask and fill to thebottom of the

43、neck, not to the mark, with acetone.NOTE 5The solution may require warming for complete dissolutionof 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 a100150 m

44、L vial with fluoropolymer-lined cap. Mark thesolution level on the vial and store in the dark at roomtemperature.11.3 Immediately 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 dou

45、bt ofthe concentration, remove 10.0 6 0.1 mL with a volumetricpipet, place in a tared weighing pan, and evaporate to drynessin a fume hood. The weight must be 80 6 1 mg. If not, preparea fresh solution (Section 11.1).11.4 The spiking solutions should be checked frequently forsigns of degradation or

46、evaporation using the test in Section11.3.11.5 If necessary, this solution can be made more or lessconcentrated to suit the concentration needed for the matrixspike. A fresh spiking solution should be prepared weekly orbi-weekly.12. Calibration and Standardization12.1 To ensure analytical values obt

47、ained using this testmethod are valid and accurate within the confidence limits ofthe test, the instrument manufacturers instructions and thefollowing procedures must be followed when performing thetest method.NOTE 6Instruments other than FTIR spectrometers may have differ-ent procedures that should

48、 be followed according to the manufacturersinstructions.12.2 Calibration is carried out using the set of calibrationstandard devices (CSD).12.2.1 Take a background reference file through the CSDlabeled “Background” according to the instrument manufac-turers instructions.12.2.2 Scan each of the other

49、 CSDs according to theinstrument manufacturers instructions.12.2.3 Measure and record the absorbance of the peakcentered near 2920 cm1(3.42 micron) according to PracticesE168. The instrument may include automatic measurementsoftware; if so follow instrument manufacturers instructionsfor using the software.NOTE 7Other peaks associated with the methylene moiety may alsobe used; detection limits will be affected so the operator should followSection 12.4 to determine the detection limit for the absorbance peakschosen.12.2.4 Linear calibration may be