1、Designation: D7678 11D7678 17Standard Test Method forTotal Oil and Grease (TOG) and Total PetroleumHydrocarbons (TPH) in Water and Wastewater with SolventExtraction using Mid-IR Laser Spectroscopy1This standard is issued under the fixed designation D7678; the number immediately following the designa
2、tion 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 covers the deter
3、mination of total oil and grease (TOG) and total petroleum hydrocarbons (TPH) inwater,water and waste water,water that are extractable by this test method from an acidified sample with a cyclic aliphatichydrocarbon (for example cyclohexane), cyclohexane, cyclopentane) and measured by IR absorption i
4、n the region offrom 1370-1380 cm-1 to 1380 cm-1 (7.25 -7.30 microns). m to 7.30 m) using a mid-IR laser spectrometer. Polar substances are removedby clean-up with Florisil.21.2 The This test method also considers the volatile fraction of petroleum hydrocarbons, which is lost by gravimetric methodsth
5、at require solvent evaporation prior to weighing, as well as by solventlesssolvent-less IR methods that require drying of theemployed solid phase material prior to measurement. Similarly, a more complete fraction of extracted petroleum hydrocarbonishydrocarbons are accessible by this test method as
6、compared to GC methods that use a time window for quantification, aspetroleum hydrocarbons eluting outside these windows are also quantified. quantified too.1.3 This method defines oil and grease in water and wastewater as that which is extractable in the test method and measuredby IR absorption in
7、the region of 1370-1380 cm-1(7.25 7.30 microns).1.3 This test method covers the range of 0.5 0.1 mg/Lto 1000 mg/Land may be extended to a lower or higher level by extractionof a larger or smaller sample volume collected separately.1.4 The values stated in SI units are to be regarded as standard. No
8、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 responsibilityof the user of this standard to establish appropriate safety safety, health and healthenvironmental practices an
9、d determine theapplicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommenda
10、tions issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1141 Practice for the Preparation of Substitute Ocean WaterD1193 Specification for Reagent Water1 This test method is under the juris
11、diction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved Feb. 1, 2011July 15, 2017. Published March 2011September 2017. Originally approved in 2011. Last previous edition approved in
12、 2011 as D7678 11. DOI: 10.1520/D7678-11.10.1520/D7678-17.2 Florisil is a trademark by U.S. Silica Company, Frederick, MD.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refe
13、r to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all cha
14、nges accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. U
15、nited States1D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits (Withdrawn 2003)3D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3921 Test Method For Oil and Grea
16、se and Petroleum Hydrocarbons in Water (Withdrawn 2013)4D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water AnalysisD7575 Test Method for Solvent-Free Membrane Recoverable Oil and Grease by Infrared DeterminationE168 Practices for General Techniques of Infra
17、red Quantitative Analysis2.2 ISO Standards:5ISO 9377-2 Determination of Hydrocarbon Oil Index2.3 Code of Federal Regulations (CFR) Publications:640 CFR Part 136 Guidelines Establishing Test Procedures for the Analysis of Pollutants49 CFR Part 172 Hazardous Materials Table, Special Provisions, Hazard
18、ous Materials Communications, Emergency ResponseInformation, Training Requirements, and Security Plans4 The last approved version of this historical standard is referenced on www.astm.org.5 Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, Case postale 56
19、, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.ISOCentral Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva, Switzerland, http:/www.iso.org.6 Available from U.S. Government Printing Office, Superintendent of Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001,
20、http:/www.access.gpo.gov.D7678 1723. Terminology3.1 DefinitionsDefinitions: For definitions of terms used in this test method, refer to Terminology D1129 and Practices E168.3.1.1 For definitions of terms used in this standard, refer to Terminology D1129 and Practices E168.3.2 Definitions of Terms Sp
21、ecific to This Standard:3.2.1 grease, ndifference between measured value for TOG and TPH of a sample.3.2.2 total oil and grease (TOG), nmaterial that can be extracted from water or wastewater by this test method and which canbe measured by infrared absorption in the region from 1370 cm-1 to 1380 cm-
22、1.3.2.3 Totaltotal petroleum hydrocarbons (TPH), nthe extracted material material that can be extracted from water orwastewater by this test method, which remains in the solventextract after treatment with Na2SO4 and Florisil.Florisil, and whichcan be measured by infrared absorption in the region fr
23、om 1370 cm-1 to 1380 cm-1.4. Summary of Test Method4.1 An acidified 900 mL Hydrocarbons from an acidified 900-mL sample of water or wastewater isare extracted with 50 mLof cyclohexane. The solvent. The material, which is measured directly after extraction by mid-infrared laser spectroscopy isreferre
24、d to as total oil and grease (TOG). The material, which is measured after the extract is treated with sodium sulfate andFlorisil to remove traces of water,water as well as polar substances, and thereby producing a solution containing nonpolar material.The nonpolar material is non-polar material, and
25、 which is measured by mid-infrared laser spectroscopy is referred to as totalpetroleum hydrocarbons (TPH) and is measured by mid-infrared laser spectroscopy.(TPH). The difference between TOG and TPHprovides the amount of grease extracted from the sample.5. Significance and Use5.1 The presence and co
26、ncentration of total petroleum hydrocarbons, oil and grease as well as oil and grease,total petroleumhydrocoarbons, in domestic and industrial wastewater is of concern to the public because of its deleterious aesthetic effect and itsimpact on aquatic life.5.2 Regulations and standards have been esta
27、blished that require monitoring of total petroleum hydrocarbons oil and grease aswell as oil and greasetotal petroleum hydrocarbons in water and wastewater.6. Interferences6.1 Soaps, detergents, surfactants, and other materials may form emulsions that could reduce the amount of total petroleumhydroc
28、arbonsTOG and TPH extracted from a sample. This test method contains procedures that can assist the analyst in breakingsuch emulsions.6.2 Organic compounds and other materials not considered as total oil and grease or petroleum hydrocarbons on the basis ofchemical structure may be extracted, retaine
29、d in the extract after filtration over Florisil and thus measured as total petroleumhydrocarbons (for example, halogenated hydrocarbons).(for example, halogenated hydrocarbons) may be extracted and measuredby this test method.7. Apparatus7.1 All glassware that will come in contact with the sample sh
30、all be thoroughly cleaned, rinsed with distilled water and driedat 130 C. 130C. Prior to starting this procedure, the glassware shall be rinsed with solvent.solvent and dried.7.2 Cell(s), calcium fluoride, two required for double-beam operation, one required for single-beam operation. The path lengt
31、hof the cells should be chosen for optimum signal to noise ratio at the measurement wavelengths. This will be 2-323 mm in caseof quantum cascade laser based spectrometers. However, longer Longer path lengths may be appropriate shouldappropriate, ifmore powerful lasers become available.7.3 Mid-infrar
32、ed laser spectrometer with an optical power 20 mW within the spectral region of 7.25-7.30 m.from 1370 cm-1to 1380 cm-1 (7.25 m to 7.30 m). Either double-beam or single-beam and capable of making measurements measuring in thespectral region from 7.25-7.30 1370 cm-1 to 1380 cm-1m or single beam (7.25
33、m to 7.30 m) or single-beam instrument tunablefrom 7.14 1370 cm-1 to 1400 cm-17.30 m. (7.14 m to 7.30 m).77.4 GlassWide Mouth Sample Bottle,mouth sample bottle, minimum 250 mL,made from glass, suggested 1 L, either with screwcap having a fluoropolymer liner or a wide-necked glass flask with a ground
34、 neck and with either glass or fluoropolymer stopper.The sampling bottle shall allow direct extraction from the bottle.7.5 Micro-separator,Micro-separator for example(for example, see Fig. X1.1,), or other suitable device for phase separation.7 For example: The ERACHECK from Eralytics GmbH has been
35、found to meet these specifications.The sole source of supply of the Oil in Water analyzers known to thecommittee at this time is QuantaRed Technologies GmbH. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters.Yourcomments will receive careful
36、 consideration at a meeting of the responsible technical committee,1 which you may attend.D7678 1737.6 Clean-up columns, made from glass, with frit of sinter porosity 2, for example2 (for example, see Fig. X1.2) or equivalentready-made clean-up column containing Na2SO4 and Florisil (for TPH measurem
37、ents).7.7 Glass bottle, 50-100 mL 50 mL to 100 mL, with glass or fluoropolymer stopper, or crimped cap with lined PTFE septum.7.8 Magnetic stirrer, with PTFE-fluorocarbon stirring bar.PTFE stir bar (optional).7.9 Volumetric flasks, glass, various (50, 100, and 200 mL).7.10 Teflon spritzPTFE bottle,
38、one-piece wash bottle bottle.for rinsing.7.11 Volumetric pipettes, glass, various (20, 30(10, 20, and 4050 mL).7.12 Analytical balance.7.13 Graduated glass syringes, (for example Hamilton) 5 5 L and 25 L.7.14 Benchtop shaker, shaker.(optional).7.15 Glass stirring rod,rod (optional).7.16 A 1.00 mL 1.
39、00-mL serological glass pipet graduated in 0.01-mL increments and a 5.00-mL serological glass pipetgraduated in 0.1-mL increments, or equivalent (optional).8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended th
40、at allreagents shall conform to the specification of the Committee on Analytical Reagents of the American Chemical Society, whereifsuch specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without le
41、ssening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to laboratory or reagent water shall be understood to mean reagentwater conforming to Specification D1193, Type II.8.3 Tetradecane99.0 % minimum purity, for use in calibration.8.4 Petroleum hydrocarbo
42、nsHydrocarbons, similar in composition to petroleum hydrocarbons determined by this test methodfor possible use as calibration material.8.5 Mineral oil typeOil Type A (Diesel oilOil without additives)Additives) and Mineral oil typeOil Type B (Lubricating oilOilwithout additives)Additives)These oil t
43、ypes may be obtained from suppliers of fine chemicals, for example Fluka (mineral oiltype A: Product No. 91975; mineral oil type B: Product No. 78473). Alternatively chemicals and mixed 1:1 (w:w). The mixturecan be stored at 1C to 6C for up to six months. Alternatively, a readily prepared 1:1 (w:w)
44、mixture of these oils may be used(for example, BAM K0108from the German Federal Institute for Materials Research and Testing).).8.6 Florisilgrain size 150 m to 250 m (60 mesh to 100 mesh), heated activated by heating to 140C for 16 h and storedin a desiccators.desiccator. Florisil is a tradetrademar
45、k name for a prepared diatomaceous substance, mainly consisting ofanhydrous magnesium silicate, available for example from Sigma Aldrich (Product Number 03286). Determine the cyclohexanesoluble material content of the Florisil by extracting 10 g of Florisil with 25 mL of cyclohexane and collect the
46、elute in a flask.Filter and fill a calcium fluoride cell for analysis by IR. The cyclohexane soluble material must be less than 0.5 mg/25mL.silicate.8.7 Sodium Sulfate (Na2SO4)anhydrous, granular.8.8 Sulfuric Acid (1+1)Slowly and carefully add 1 volume of sulfuric acid (H2SO4, sp gr 1.84) to 1 volum
47、e of water, stirringand cooling the solution during addition.8.9 Hydrochloric acid,Acid, ACS, (1 + 1)Mix equal volumes of concentrated HCl and water.8.10 SolventCyclohexane (minimum purity 99.5%) 99.5 %) or cyclopentane (minimum purity 98.5%)98.5 %).8.11 Stearic Acid (C18H36O2), minimum purity 98 %.
48、9. Hazards9.1 Normal laboratory safety applies to this test method. Analysts should wear safety glasses, gloves and lab coats whenworking with acids. Analysts should review the materialMaterial Safety Data Sheets (MSDS) for all reagents used in this testmethod. Additional hazards may be presented by
49、 the particular sample being tested so proper care must be taken.8 The sole source of supply of the prepared mixture BAM K010 known to the committee at this time is the German Federal Institute for Materials Research and Testing.If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1 which you may attend.D7678 17410. Sampling10.1 Collect the sample in accordance with the principles d
