1、Designation: D7066 04 (Reapproved 2011)An American National StandardStandard 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 follo
2、wing 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
3、covers the determination of oil andgrease and nonpolar material in water and wastewater by aninfrared (IR) determination of dimer/trimer of chlorotrifluoro-ethylene (S-316) extractable substances from an acidifiedsample. Included in this estimation of oil and grease are anyother compounds soluble in
4、 the solvent.1.2 The method is applicable to measurement of the lightfuel although loss of some light ends during extraction can beexpected.1.3 This method defines oil and grease in water and waste-water as that which is extractable in the test method andmeasured by IR absorption at 2930 cm-1or 3.4
5、microns.Similarly, this 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 method covers the range of 5 to 100 mg/L and maybe extended to a lower or higher level
6、by extraction of a largeror 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 problems, if any, associated with its use.
7、 It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine (D3856 Guidefor Good Laboratory Practices2) the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:D1129 Terminology Relating to WaterD
8、1193 Specification for Reagent WaterD3370 Practices for Sampling Water from Closed ConduitsD3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD58
9、10 Guide for Spiking into Aqueous SamplesD5847 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 Observations3. Terminology3.1 DefinitionsFor d
10、efinitions of terms used in this testmethod, refer to Terminology D1129 and Practices E168.3.2 Definitions of Terms Specific to This Standard:3.2.1 oil and greasethe organic matter extracted fromwater or wastewater and measured by this test method.3.2.2 nonpolar materialthe oil and grease remaining
11、insolution after contact with silica gel and measured by this testmethod.3.2.3 solventdimer/trimer of chlorotrifluoroethylene (S-316)4. Summary of Test Method4.1 An acidified 250-mL sample of water or wastewater isextracted serially with three 15-mL volumes of dimer/trimer ofchlorotrifluoroethylene
12、(S-316). The extract is diluted to 50mLand a portion is examined by infrared spectroscopy (IR) for anoil and grease measurement.3A portion of the extract iscontacted with silica gel to remove polar substances, thereby1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is th
13、e direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved May 1, 2011. Published June 2011. Originallyapproved in 2004. Last previous edition approved in 2004 as D7066 041. DOI:10.1520/D7066-04R11.2For referenced ASTM standards, vis
14、it 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.3Consult the manufacturers operation manual for the specific instructionsrelated to the infrared
15、 spectrometer or analyzer to be used.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.producing a solution containing nonpolar material. The non-polar material is measured by infrared spectroscopy.5. Significance and Use5.1 The presen
16、ce and concentration of oil and grease indomestic and industrial wastewater is of concern to the publicbecause 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. Int
17、erferences6.1 Soaps, detergents, surfactants and other materials mayform emulsions that may reduce the amount 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 considereda
18、s oil and grease on the basis of chemical structure may beextracted and measured as oil and grease. Of those measured,certain ones may be adsorbed by silica gel while others maynot. Those not adsorbed are measured as nonpolar material.7. ApparatusAll glassware that will come in contact with the samp
19、le mustbe rinsed with dimer/trimer of chlorotrifluoroethylene (S-316)prior to beginning this procedure.7.1 Cell(s), quartz, 10-mm path length (lower concentra-tions may require a longer pathlength), two required fordouble-beam operation, one required for single-beam opera-tion, or built-in or drop-i
20、n cell for infrared filtometer analyzeroperation.7.2 Filter Paper, ashless, quantitative, general-purpose, 11-cm, Whatman #40 or equivalent.7.3 Glass Funnel7.4 Glass Wide Mouth Sample Bottle, minimum 250-mL,with screw cap having a fluoropolymer liner.7.5 Glass Graduated Cylinder, 100-mL7.6 Infrared
21、Spectrometer, double-beam dispersive, single-beam dispersive, Fourier transform, filtometers or other ca-pable of making measurements at 2930 cm-1.7.7 Magnetic Stirrer, with small TFE-fluorocarbon stirringbar.7.8 Glass Separatory-Funnel, 500mL, with fluoropolymerstopcock and stopper.7.9 Volumetric F
22、lasks, glass, various (10, 25, 50, 100, and200-mL)7.10 Teflon spritz bottle, one-piece wash bottle for rinsing7.11 Repeating pipetter, glass, 15-mL, (optional)7.12 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 increment
23、s and a 5.00-mL serological pipet gradu-ated in 0.1-mL increments, or equivalent)7.13 Benchtop shaker, (optional)7.14 Glass Stirring Rod, (optional)7.15 Analytical Balance,7.16 Syringes, 50 and 500 mL8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise
24、 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. Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to
25、permit its use without lessening theaccuracy of the determination.8.2 Purity of WaterUnless 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 % minimum pu-rity, f
26、or use in calibration.8.4 Octanoic acid 98 % minimum purity, for use in calibra-tion.8.5 Silica Gel, Anhydrous, 75 - 150 micrometers, 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
27、 of chloro-trifluoroethylene (S-316) soluble material content of the silicagel by extracting 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 (
28、S-316) soluble mate-rial must be less than 5 mg/L.8.6 Sodium Sulfate (Na2SO4), ACS, granular anhydrous.Dry at 200-250 C for 24 hours minimum and store in a tightlysealed container until use. (Note: Powdered sodium sulfateshould not be used because water may cause it to solidify.)8.7 Solvent - dimer/
29、trimer of chlorotrifluoroethylene,IRspectroscopy grade, for example S-316 manufactured byHoriba Instruments, Irvine CA, 800-446-7422 (ASTM does notadvocate the use of one vendor over another)8.8 Sulfuric Acid (1 + 1)Slowly and carefully add 1volume of sulfuric acid (H2SO4, sp gr 1.84) to 1 volume of
30、water, stirring and cooling the solution during the addition(optional HCl replacement).8.9 Hydrochloric acid, ACS, 1 + 1. Mix equal volumes ofconcentrated HCl and water8.10 Sodium Chloride (NaCl), crystalline, ACSor use inbreaking emulsions, if needed. Wet thoroughly with solventbefore using.9. Samp
31、ling9.1 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 with the sample to beanal
32、yzed. 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 times.9.2 A sample of abo
33、ut 250mL is required for this test. Usethe entire sample because removing a portion would notapportion the oil and grease that adheres to the bottle surfaces.D7066 04 (2011)2The high probability that extractable matter may adhere tosampling equipment and result in measurements that are biasedlow pre
34、cludes 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 concentrationsaveraged. Altern
35、atively, 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 with10mLof solvent, a
36、nd use the solvent for the extraction (Section12.2.2). Do not exceed 50 mL of total solvent during theextraction and rinse procedure.9.3 Preserve the sample with a sufficient quantity of eithersulfuric (see Section 8.8) or hydrochloric acid (see Section 8.9)to a pH of 2 or lower and refrigerate at 0
37、-4 C from the timeof collection until extraction. The amount of acid required willbe dependent upon the pH and buffer capacity of the sample atthe time of collection. If the amount of acid required is notknown, make the pH measurement on a separate sample thatwill not be analyzed. Introduction of pH
38、 paper to an actualsample or sample cap may remove some oil from the sample.To more accurately calculate the final oil concentration of theextract, the volume of acid added to each sample can berecorded, then subtracted from the final measured samplevolume.If the sample is to be shipped by commercia
39、l carrier, U.S.Department of Transportation regulations limit the pH to aminimum (see 40CFR Part 136, Table II Footnote 3) of 1.96 ifHCl is used and 1.15 if H2SO4is used (see 49 CFR part 172).Collect an additional 1 or 2 sample aliquots for the matrix spikeand matrix spike duplicate (Section 14.5) a
40、nd preserve withacid.9.4 Refrigerate the sample at 15 %, a calibration curve must be used or the calibrationstandards must be adjusted to bound the linear range (seeSection 11 note). Either the average calibration factor (CFm)orthe calibration curve is used, not both. Verification is done onthe chos
41、en calibration.11.12 Verify calibration after each 10 analyses using cali-bration solution C or D, or alternating the calibration solutions.Calibration is verified if CFXis within +/- 15 % of CFmor itsrespective point on the calibration curve.11.13 If calibration is not verified, prepare a fresh cal
42、ibra-tion solution and repeat the calibration verification test (Section11.12). If calibration is not verified with the fresh calibrationstandard, recalibrate and reanalyze all extracts of all samplesanalyzed since the last calibration or verification, whichever ismost recent.D7066 04 (2011)412. Pro
43、cedure12.1 Sample pretreatment12.1.1 Bring the sample and QC (i.e., MS/MSD) aliquots toroom 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
44、 from the sample bottle 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 5Use of the sodium sulfate is necessary to prevent water frominterfering in
45、the determination. Because 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
46、the 50-mL volumetric flask. 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. Pou
47、r 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 the phas
48、es to separate.12.2.6 Drain the solvent (lower) layer from the separatoryfunnel through the sodium sulfate into a pre-cleaned 50-mLvolumetric flask.NOTE 6Certain types of samples, such as those containing a largeamount of detergent, may form an emulsion during the extraction. Ifemulsion forms betwee
49、n the phases and the emulsion is greater thanone-third the volume of the solvent layer, the laboratory should employemulsion-breaking techniques to complete the phase separation. Theoptimum technique depends upon the sample, but may include stirring,filtration through glass wool, use of solvent phase separation paper,centrifugation, use of an ultrasonic bath with ice, addition of NaCl,increasing the temperature, lowering the pH, or other physical methods.Alternatively, solid-phase extraction (SPE), continuous liquid-liquid ex-traction, or other extraction techniques
