1、Designation: D7066 04 (Reapproved 2017)Standard Test Method fordimer/trimer of chlorotrifluoroethylene (S-316) RecoverableOil and Grease and Nonpolar Material by InfraredDetermination1This standard is issued under the fixed designation D7066; the number immediately following the designation indicate
2、s 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 determination of o
3、il andgrease and nonpolar material in water and wastewater by aninfrared (IR) determination of dimer/trimer of chlorotrifluoro-ethylene (S-316)2extractable substances from an acidifiedsample. Included in this estimation of oil and grease are anyother compounds soluble in the solvent.1.2 This test me
4、thod is applicable to measurement of thelight fuel although loss of some light ends during extractioncan be expected.1.3 This test method defines oil and grease in water andwastewater as that which is extractable in the test method andmeasured by IR absorption at 2930 cm-1or 3.4 microns.Similarly, t
5、his test method defines nonpolar material in waterand wastewater as that oil and grease which is not adsorbed bysilica gel in the test method and measured by IR absorption at2930 cm-1.1.4 This test method covers the range of 5 to 100 mg/L andmay be extended to a lower or higher level by extraction o
6、f alarger or smaller sample volume collected separately.1.5 The values stated in SI units are to be regarded asstandard. 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 therespo
7、nsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine (Guide D3856) the applicability of regulatory limitationsprior to use.1.7 This international standard was developed in accor-dance with internationally recognized principles on
8、 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:3D1129 Terminology Relating to WaterD1193
9、 Specification for Reagent WaterD3370 Practices for Sampling Water from Closed ConduitsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD5847 Practice for Writing Qu
10、ality Control Specificationsfor Standard Test Methods for Water AnalysisE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE178 Practice for Dealing With Outlying Observations3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer toTerminology
11、D1129 and Practices E168.3.2 Definitions of Terms Specific to This Standard:3.2.1 nonpolar material, nthe oil and grease remaining insolution after contact with silica gel and measured by this testmethod.3.2.2 oil and grease, nthe organic matter extracted fromwater or wastewater and measured by this
12、 test method.3.2.3 solvent, ndimer/trimer of chlorotrifluoroethylene (S-316).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 Sept. 1, 2017.
13、 Published September 2017. Originallyapproved in 2004. Last previous edition approved in 2011 as D7066 04 (2011).DOI: 10.1520/D7066-04R17.2The sole source of supply of the material S-316 known to the committee at thistime is Horiba Instruments, Irvine, CA. If you are aware of alternative suppliers,p
14、lease provide this information to ASTM International Headquarters. Your com-ments will receive careful consideration at a meeting of the responsible technicalcommittee,1which you may attend.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servi
15、ceastm.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 accordance wi
16、th 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.14. Summary of Test Method4.1 An acidifie
17、d 250-mL sample of water or wastewater isextracted serially with three 15-mL volumes of dimer/trimer ofchlorotrifluoroethylene (S-316). The extract is diluted to 50 mLand a portion is examined by infrared spectroscopy (IR) for anoil and grease measurement.4A portion of the extract iscontacted with s
18、ilica gel to remove polar substances, therebyproducing a solution containing nonpolar material. The non-polar material is measured by infrared spectroscopy.5. Significance and Use5.1 The presence and concentration of oil and grease indomestic and industrial wastewater is of concern to the publicbeca
19、use of its deleterious aesthetic effect and its impact onaquatic life.5.2 Regulations and standards have been established thatrequire monitoring of oil and grease in water and wastewater.6. Interferences6.1 Soaps, detergents, surfactants, and other materials mayform emulsions that may reduce the amo
20、unt of oil and greaseextracted from a sample. This test method contains proceduresthat can assist the analyst in breaking such emulsions.6.2 Organic compounds and other materials not consideredas oil and grease on the basis of chemical structure may beextracted and measured as oil and grease. Of tho
21、se measured,certain ones may be adsorbed by silica gel while others maynot. Those not adsorbed are measured as nonpolar material.7. Apparatus7.1 All glassware that will come in contact with the samplemust be rinsed with dimer/trimer of chlorotrifluoroethylene(S-316) prior to beginning this procedure
22、.7.2 Cell(s), quartz, 10-mm path length (lower concentra-tions may require a longer pathlength), two required fordouble-beam operation, one required for single-beamoperation, or built-in or drop-in cell for infrared filtometeranalyzer operation.7.3 Filter paper, ashless, quantitative, general-purpos
23、e, 11-cm, Whatman #40 or equivalent.7.4 Glass funnel.7.5 Glass wide mouth sample bottle, minimum 250-mL,with screw cap having a fluoropolymer liner.7.6 Glass graduated cylinder, 100-mL7.7 Infrared spectrometer, double-beam dispersive, single-beam dispersive, Fourier transform, filtometers or other c
24、a-pable of making measurements at 2930 cm-1.7.8 Magnetic stirrer, with small TFE-fluorocarbon stirringbar.7.9 Glass separatory-funnel, 500mL, with fluoropolymerstopcock and stopper.7.10 Volumetric flasks, glass, various (10, 25, 50, 100, and200-mL).7.11 TFE-fluorocarbon spritz bottle, one-piece wash
25、 bottlefor rinsing.7.12 Repeating pipetter, glass, 15-mL, (optional).7.13 Volumetric pipettes, glass, various (0.50, 1.00, 5.00,10.0 and 25.0-mL, including a 1.00 serological pipet graduatedin 0.01-mL increments and a 5.00-mL serological pipet gradu-ated in 0.1-mL increments, or equivalent).7.14 Ben
26、chtop shaker, (optional).7.15 Glass stirring rod, (optional).7.16 Analytical balance.7.17 Syringes, 50 and 500 mL.8. Reagents8.1 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
27、Committeeon Analytical Reagents of the American Chemical Society,where such specifications are available. Other 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.8.2 Purity of WaterU
28、nless otherwise indicated, referencesto laboratory or reagent water shall be understood to meanreagent water conforming to Specification D1193, Type II.8.3 Isooctane (2,2,4-trimethylpentane) 98 % minimumpurity, for use in calibration.8.4 Octanoic Acid 98 % minimum purity, for use in calibra-tion.8.5
29、 Silica Gel, Anhydrous, 75150 micrometres, DavisilGrade 923 (Supelco 21447-7A, or equivalent). Dry at200250C for 24 hour minimum and store in a desiccator ortightly sealed container. Determine the dimer/trimer of chloro-trifluoroethylene (S-316) soluble material content of the silicagel by extractin
30、g 10 g of silica gel with 25 mL of dimer/trimerof chlorotrifluoroethylene (S-316) and collect the elute in aflask. Filter and fill a quartz cell for analysis by IR. Thedimer/trimer of chlorotrifluoroethylene (S-316) soluble mate-rial must be less than 5 mg/L.8.6 Sodium Sulfate (Na2SO4), ACS, granula
31、r anhydrous.Dry at 200250C for 24 hours minimum and store in a tightlysealed container until use.NOTE 1Powdered sodium sulfate should not be used because watermay cause it to solidify.8.7 Solventdimer/trimer of chlorotrifluoroethylene,IRspectroscopy grade.58.8 Sulfuric Acid (1 + 1)Slowly and careful
32、ly add 1volume of sulfuric acid (H2SO4, sp gr 1.84) to 1 volume ofwater, stirring and cooling the solution during the addition(optional HCl replacement).4Consult the manufacturers operation manual for the specific instructionsrelated to the infrared spectrometer or analyzer to be used.5The material
33、S-316, available from Horiba Instruments, Irvine, CA, orequivalent, has been found suitable for use.D7066 04 (2017)28.9 Hydrochloric acid, ACS,1+1.Mixequal volumes ofconcentrated HCl and water8.10 Sodium Chloride (NaCl), crystalline, ACS, or use inbreaking emulsions, if needed. Wet thoroughly with s
34、olventbefore using.9. Sampling9.1 Collect the sample in accordance with the principlesdescribed in Practices D3370, using a glass bottle equippedwith a screw cap having a fluoropolymer liner. Prerinse thesample bottle and cap with the solvent prior to samplecollection. Do not rinse the sample bottle
35、 with the sample to beanalyzed. Fill bottle with minimal headspace to prevent loss ofvolatile constituants. Do not allow the sample to overflow thebottle during collection. Preventing overflow may not bepossible in all sampling situations, however, measures shouldbe taken to minimize overflow at all
36、 times.9.2 A sample of about 250 mL is required for this test. Usethe entire sample because removing a portion would notapportion the oil and grease that adheres to the bottle surfaces.The high probability that extractable matter may adhere tosampling equipment and result in measurements that are bi
37、asedlow precludes the collection of composite samples for deter-mination of oil and grease. Therefore, samples must becollected as grab samples. If a composite measurement isrequired, individual grab samples collected at prescribed timeintervals may be analyzed separately and the concentrationsavera
38、ged. Alternatively, samples can be collected in the fieldand composited in the laboratory. For example, collect fourindividual 63-mL samples over the course of a day. In thelaboratory, pour each 63-mL sample into the separatory funnel,rinse each of the four bottles (and caps) sequentially with 10mL
39、of solvent, and use the solvent for the extraction (12.2.2).Do not exceed 50 mL of total solvent during the extraction andrinse procedure.9.3 Preserve the sample with a sufficient quantity of eithersulfuric (see 8.8) or hydrochloric acid (see 8.9)toapHof2orlower and refrigerate at 04C from the time
40、of collection untilextraction. 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 beanalyzed. Introduction of pH paper to an actual
41、 sample orsample cap may remove some oil from the sample. To moreaccurately calculate the final oil concentration of the extract,the volume of acid added to each sample can be recorded, thensubtracted from the final measured sample volume.If the sample is to be shipped by commercial carrier, U.S.Dep
42、artment of Transportation regulations limit the pH to aminimum (see 40 CFR, Part 136, Table II, Footnote 3) of 1.96if HCl is used and 1.15 if H2SO4is used (see 49 CFR, Part172). Collect an additional 1 or 2 sample aliquots for the matrixspike and matrix spike duplicate (14.1.5) and preserve withacid
43、.9.4 Refrigerate the sample at D7066 04 (2017)415 %, a calibration curve must be used or the calibrationstandards must be adjusted to bound the linear range (seeSection 11, Note 4). Either the average calibration factor (CFm)or the calibration curve is used, not both. Verification is doneon the chos
44、en calibration.11.13 Verify calibration after each 10 analyses using cali-bration solution C or D, or alternating the calibration solutions.Calibration is verified if CFXis within 615 % of CFmor itsrespective point on the calibration curve.11.14 If calibration is not verified, prepare a fresh calibr
45、a-tion solution and repeat the calibration verification test (11.13).If calibration is not verified with the fresh calibration standard,recalibrate and reanalyze all extracts of all samples analyzedsince the last calibration or verification, whichever is mostrecent.12. Procedure12.1 Sample Pretreatm
46、ent:12.1.1 Bring the sample and QC (that is, MS/MSD) aliquotsto room temperature.12.1.2 Either mark the sample bottle at the water meniscusor weigh the bottle for later determination of the samplevolume. Weighing will be more accurate.12.2 Extraction:12.2.1 Transfer the sample from the sample bottle
47、 to a cleanseparatory funnel via a clean transfer funnel.12.2.2 Place a filter paper in a filter funnel, add approxi-mately1gofNa2SO4, rinse with a small portion of solvent anddiscard the rinsate.NOTE 6Use of the sodium sulfate is necessary to prevent water frominterfering in the determination. Beca
48、use the sample is extracted threetimes, it is not necessary to remove all of the solvent from the separatoryfunnel; it is better to preclude water from reaching the sodium sulfate. Ifthe sodium sulfate cakes when contacted with the extract, flush once with2 mL of solvent into the 50-mL volumetric fl
49、ask. Remove the solid witha clean spatula, and add about1goffresh sodium sulfate to the filter.Rewet sodium sulfate with solvent before use.12.2.3 Add 15 mL of solvent to the sample bottle. Cap withthe original cap and shake the sample bottle to rinse all interiorsurfaces. Pour the solvent into the separatory funnel, rinsingdown the sides of the transfer funnel.12.2.4 Extract the sample by shaking the separatory funnelvigorously for 2 minutes with periodic venting into a hood torelease excess pressure. Vent the funnel slowly to prevent lossof sample.12.2.5 Allow t
