1、Designation: D8193 18Standard Test Method forTotal Oil and Grease (TOG) and Total PetroleumHydrocarbon (TPH) in Water and Wastewater with SolventExtraction Using Non-Dispersive Mid-IR TransmissionSpectroscopy1This standard is issued under the fixed designation D8193; the number immediately following
2、 the designation indicates the year oforiginal adoption or, in the case 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 cove
3、rs the determination of total oiland grease (TOG) that can be extracted from water or waste-water samples by cyclohexane and measured by non-dispersiveIR spectroscopy from 13701380 cm-1. Treating the extractwith Florisil2to remove polar substances prior to the IRmeasurement enables determination of
4、the total petroleum(TPH).1.2 This method also considers the volatile fraction ofpetroleum hydrocarbons which is lost by gravimetric methodsthat require solvent evaporation prior to weighing, as well asby solventless IR methods that require drying of the employedsolid phase material prior to measurem
5、ent. Similarly, a morecomplete fraction of extracted petroleum hydrocarbon is ac-cessible by this method as compared to GC methods that use atime window for quantification, as petroleum hydrocarbonseluting outside these windows are also quantified.1.3 This method defines total oil and grease in wate
6、r asmaterial that can be extracted with cyclohexane and measuredby IR absorption in the region of 13701380 cm-1(7.257.3m). Similarly, total petroleum hydrocarbon in water is definedas material that can be extracted with cyclohexane, remains inthe extract after filtration over Florisil and is measure
7、d by IRabsorption in the region of 13701380 cm-1(7.257.3 m). Theconcentration of total grease is defined as the differencebetween the total oil and grease and total petroleum hydrocar-bon concentrations.1.4 This method covers the range of 0.5 to 1000 mg/L fortotal oil and grease as well as for total
8、 petroleum hydrocarbonsand has a method detection limit (MDL) of 0.5 mg/L. Therange and method detection limit may be extended to higher orlower concentrations by adjusting the water or solvent volumeused in the liquid-liquid extraction.1.5 The values stated in SI units are to be regarded asstandard
9、. No other units of measurement are included in thisstandard.1.6 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, health, and environmental practices and deter-
10、mine the applicability of regulatory limitations prior to use.1.7 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendatio
11、ns issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1141 Practice for the Preparation of Substitute OceanWaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Preci
12、sion and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisD7678 Test Method for Total Oil and Grease (TOG) andTotal Petroleum Hydrocarbon
13、s (TPH) in Water and Waste-water with Solvent Extraction using Mid-IR Laser Spec-troscopyE168 Practices for General Techniques of Infrared Quanti-tative Analysis1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Method
14、s forAnalysis forOrganic Substances in Water.Current edition approved Dec. 15, 2018. Published January 2019. DOI: 10.1520/D8193-18.2Florisil is a trademark by U.S. Silica Company, Frederick, MD.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at s
15、erviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordanc
16、e with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.12.2 ISO Standards:4ISO 9377-2 Determ
17、ination of Hydrocarbon Oil Index2.3 Code of Federal Regulations (CFR) Publications:540 CFR Part 136 Guidelines Establishing Test Proceduresfor the Analysis of Pollutants49 CFR Part 172 Hazardous Materials Table, SpecialProvisions, Hazardous Materials Communications, Emer-gency Response Information,
18、Training Requirements, andSecurity Plans3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method, referto Terminology D1129 and Practices E168.3.1.2 total oil and grease (TOG), nmaterial that can beextracted from water or wastewater by this test method andwhich can be me
19、asured by infrared absorption in the regionfrom 1370 cm-1to 1380 cm-1.3.1.3 total petroleum hydrocarbon (TPH), nnon-polar or-ganic material that can be extracted from water or wastewater,and which can be measured by infrared absorption in the regionfrom 1370 cm-1to 1380 cm-1.3.2 Definitions of Terms
20、 Specific to This Standard:3.2.1 grease, nthe difference between TOG and TPH of asample.4. Summary of Test Method4.1 An acidified 900-mL sample of water or wastewater isextracted with 50 mL of cyclohexane. A part of the extract ismeasured with infrared spectroscopy to quantify the total oiland greas
21、e (TOG) concentration. The remaining part of theextract is treated by Florisil to remove polar substances. Thetreated extract is measured with infrared spectroscopy toquantify the total petroleum hydrocarbon concentration (TPH).The difference between TOG and TPH provides the amount ofgrease extracte
22、d from the sample.5. Significance and Use5.1 The presence and concentration of total petroleumhydrocarbons, as well as total oil and grease, in domestic andindustrial wastewater is of concern to the public because of itsdeleterious aesthetic effect and its impact on aquatic life.5.2 Regulations and
23、standards have been established thatrequire monitoring of total petroleum hydrocarbons as well astotal oil and grease in water and wastewater.6. Interferences6.1 Soaps, detergents, surfactants, and other materials mayform emulsions that could reduce the amount of oil and greaseas well as petroleum h
24、ydrocarbons extracted from a sample.This test method contains procedures that can assist the analystin breaking such emulsions.6.2 Organic compounds and other materials not consideredas oil and grease or petroleum hydrocarbons based on theirchemical structure (for example, halogenated or cyclic hydr
25、o-carbons) may be extracted and measured by the method.7. Apparatus7.1 All glassware that will come in contact with the sampleshall be thoroughly cleaned, rinsed with distilled water, anddried at 130C.7.2 Temperature controlled absorption spectrometer with anautomatic filling system and a transmissi
26、on cell. The spectrom-eter should use a light source and an optical interference filtertransmitting in the range from 13701380 cm-1. The pathlength of the transmission cell shall be between 11.5 mm. Inorder for the spectrometer to qualify, the standard deviation of10 blank measurements should be les
27、s than 0.06 mAU.7.3 Glass wide mouth sample bottle, suggested 1 L, eitherwith screw cap having a fluoropolymer liner or a wide-neckedglass flask with a ground neck with either glass or fluoropo-lymer stopper. The sampling bottle shall allow direct extractionfrom the bottle.7.4 Micro-separator, for e
28、xample see figure in Annex A2 orother suitable device for phase separation (optional).7.5 Solid phase extraction cartridges containing Florisilwith PTFE or stainless steel frits (for TPH).7.6 Beakers 50100 mL.7.7 Magnetic stirrer, with PTFE-fluorocarbon stirring bar(optional).7.8 Volumetric flasks,
29、glass, various (50, 100, and 200 mL).7.9 Teflon spritz bottle, one-piece wash bottle for rinsing.7.10 Volumetric pipettes, glass, various (10, 20, and 40 mL).7.11 Analytical balance.7.12 Graduated glass syringes, 250 L (optional).7.13 Benchtop shaker, (optional).7.14 Glass stirring rod, (optional).8
30、. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals 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 availa
31、ble.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4Available from International Organization for Standardization (ISO), ISOCentral Secretariat, BIBC II, Chemin de Blandonn
32、et 8, CP 401, 1214 Vernier,Geneva, Switzerland, http:/www.iso.org.5Available from U.S. Government Printing Office, Superintendent ofDocuments, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:/www.access.gpo.gov.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical So
33、ciety, Washington, DC, www.chemistry.org. For suggestions on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,Inc. (USPC), Rockville, MD, http:/www.usp.org.D8193 1828.2 Cyclohexane, minimum pur
34、ity 99.5 %, used for extrac-tion.8.3 Purity of WaterUnless otherwise indicated, referencesto laboratory or reagent water shall be understood to meanreagent water conforming to Specification D1193, Type II.8.4 n-Octane, 99.0 % minimum purity, for use in calibra-tion.8.5 2,2,4 Trimethylpentane, 99.0 %
35、 minimum purity, for usein calibration.8.6 1:1 (w/w) Mixture of Mineral Oil Type A (Diesel OilWithout Additives) and Mineral Oil Type B (Lubricating OilWithout Additives), for use as laboratory control sample (LCS).Areadily prepared 1:1 (w:w) mixture of these oils may be used(for example, BAM K0107)
36、.8.7 Florisil, grain size 75 m to 150 m (100 mesh to 200mesh), heated to 140C for 16 h and stored in a desiccator.Florisil is a trade name for a prepared diatomaceous substance,mainly consisting of anhydrous magnesium silicate.8.8 Sodium Sulfate (Na2SO4), anhydrous, granular.8.9 Sulfuric Acid (1+1)S
37、lowly and carefully add 1 vol-ume of sulfuric acid (H2SO4, sp gr 1.84) to 1 volume of water,stirring and cooling the solution during addition.8.10 Hydrochloric acid, ACS, (1 + 1)Mix equal volumesof concentrated HCl and water.8.11 Stearyl stearate (C36H72O2), minimum purity 98.0 %,for qualification o
38、f Florisil used for TPH measurements.9. Hazards9.1 Normal laboratory safety applies to this method. Ana-lysts should wear safety glasses, gloves and lab coats. Analystsshould review the Safety Data Sheets (SDS) for all reagentsused in this method. Additional hazards may be presented bythe particular
39、 sample being tested so proper care must be taken.10. Sampling10.1 Weigh the dried bottle before sample collection. Pre-rinse the sample bottle and cap with the solvent (8.2) and dryit prior to sample collection. Do not rinse the sample bottlewith the sample to be analyzed.10.2 Collect the sample in
40、 accordance with the principlesdescribed in Practices D3370, using a glass bottle as specifiedin 7.3.10.3 Fill the bottle to approximately 80 %. Filling the bottleabove 80 % of total volume or allowing the bottle to overflowwill make extraction more difficult and lead to erroneousresults.10.4 Asampl
41、e volume of about 900 mL is recommended forthis test. Weigh the bottle containing the sample to determinethe actual sampled amount. Alternatively, record the sampledvolume. Use the entire sample because removing a portionwould not apportion the hydrocarbons that adhere to the bottlesurfaces. The hig
42、h probability that extractable matter mayadhere to sampling equipment and result in measurements thathave a low bias precludes the collection of composite samplesfor determination of total oil and grease and total petroleumhydrocarbon. Therefore, samples must be collected as grabsamples. If a compos
43、ite measurement is required, individualgrab samples collected at prescribed time intervals may beanalyzed separately and the concentrations averaged.Alternatively, samples can be collected in the field and com-posited in the laboratory. For example, collect three individual300-mL samples over the co
44、urse of a day. In the laboratory,extract each 300-mL sample with 15 mL and combine theextracts in a 50-mL volumetric flask and fill up to mark withsolvent prior to measurement (12.2 and 12.3).10.5 Preserve the sample with a sufficient quantity ofsulfuric acid (see 8.9) or hydrochloric acid (see 8.10
45、)toapHof 2 or lower and refrigerate at 16C from the time ofcollection until extraction. The amount of acid required will bedependent upon the pH and buffer capacity of the sample at thetime of collection. If the amount of acid required is not known,make the pH measurement on a separate sample that w
46、ill not beanalyzed. Introduction of pH paper to an actual sample orsample cap may remove some oil from the sample. In case thebottle containing the sample cannot be weighed before additionof the acid, the volume of acid added to each sample can berecorded and then subtracted from the final measured
47、sampleamount. If the sample is to be shipped by commercial carrier,U.S. Department of Transportation regulations limit the pH toa minimum of 1.15 if H2SO4is used and 1.96 if HCl is used(see 40 CFR Part 136, Table II Footnote 3 and 49 CFR Part172).10.6 All samples must be refrigerated at 16 C from th
48、etime of collection until extraction. All samples must beanalyzed within 28 days of the date and time of collection (40CFR 136, Table II). Extracted samples can be stored up to twoweeks between 7C and 10C.11. Quality Control11.1 To ensure analytical values obtained using this testmethod are valid an
49、d accurate within the confidence limits ofthe test, the instrument manufacturers instructions and thefollowing procedures must be followed when performing thetest method. Calibrations made by the instrument manufacturermay be used for analysis.11.2 Instrument Calibration:11.2.1 Bring all solutions to 22 6 3C.11.2.2 Calibration Solution S:11.2.2.1 Prepare a stock solution by weighing in 9.00 gn-octane and 1.00 g 2,2,4 Trimethylpentane.NOTE 1A 10 % solution of 2,2,4 Trimethylpentane in n-Octane wasfound to provide representative values for TOG and TPH f
