ASTM D2580-2006(2012) Standard Test Method for Phenols in Water by Gas-Liquid Chromatography 《气相-液相色谱法测定水中苯酚的标准试验方法》.pdf

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1、Designation: D2580 06 (Reapproved 2012)Standard Test Method forPhenols in Water by Gas-Liquid Chromatography1This standard is issued under the fixed designation D2580; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las

2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers a direct aqueous

3、 injectionprocedure for the gas-liquid chromatographic determination ofphenols, cresols, and mono- and di-chlorophenols in water.21.2 The precision and bias of the test method has beencalculated from the results of interlaboratory analyses of threemaster solutions, each containing phenol, p-cresol,p

4、-chlorophenol, 3,5-dichlorophenol.1.3 The test method may be applied to waste water orconcentrates that contain more than 1 mg/L of phenoliccompounds. Therefore, for a comparison with Test MethodsD1783, see Appendix X1.1.4 The analyst should recognize that precision statementsprovided in 16.1 and 16

5、.2 may not apply to waters of othermatrices.1.5 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are provided forinformation only.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is therespons

6、ibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Note 3.2. Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1193 Specificat

7、ion for Reagent WaterD1783 Test Methods for Phenolic Compounds in WaterD3370 Practices for Sampling Water from Closed ConduitsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low

8、-Level Data4E260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Rela-tionships3. Terminology3.1 Definitions:3.1.1 Definitions and terms are presented in Practice E355and Terminology D1129.3.1.2 The following terms used in this test method aredefined in Te

9、rminology D1129 as follows:3.1.3 ghosting a gas-chromatographic interference, show-ing as a peak, which appears at the same elution time as acomponent from previous injection.3.1.4 internal standarda material present in or added tosamples in known amount to serve as a reference measurement.3.1.5 noi

10、sean extraneous electronic signal that affectsbaseline stability.3.1.6 phenolic compoundshydroxy derivatives of ben-zene and its condensed nuclei.3.1.7 retention timethe time that elapses from the intro-duction of the sample until the component peak maximum isreached.4. Summary of Test Method4.1 Thi

11、s test method uses a single gas-liquid chromato-graphic column for the separation of phenolic compounds anda flame-ionization detector for their measurement. The peakarea of each component is measured and compared with that ofa known standard to obtain quantitative results.Adiscussion ofgas chromato

12、graphy is presented in Practice E260.4.2 In this test method, elution of characteristic phenolsoccurs in the following order: (1) o-chlorophenol, (2) phenoland o-cresol, (3) m- and p-cresol, (4) 2,3-, 2,4-, 2,5- and2,6-dichlorophenols, (5) m- and p-chlorophenol, and (6) 3,4-dichlorophenol.4.2.1 For

13、comparison purposes, see Appendix X1.1This 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 June 15, 2012. Published August 2012. Originallyapprov

14、ed in 1967. Last previous edition approved in 2006 as D2580 94 (2006).DOI: 10.1520/D2580-12.2Baker, R. A., “Phenolic Analyses by Direct Aqueous Injection Gas Chroma-tography,” Journal American Water Works Association, Vol 58, No. 6, 1966, pp.751760.3For referenced ASTM standards, visit the ASTM webs

15、ite, 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.4Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM I

16、nternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Phenolic compounds are sometimes found in surfacewaters from natural and industrial sources. Chlorination ofsuch waters may produce odoriferous, objectionable tastingchlorophe

17、nols. These compounds may include o-chlorophenol,p-chlorophenol, 2,6-dichlorophenol, and 2,4-dichlorophenol.56. Interferences6.1 Particulate MatterParticulate or suspended mattermay, unless very finely subdivided, plug the needle used forsample injection. Such matter may be removed by centrifuga-tio

18、n or filtration, provided it is ascertained that compounds ofinterest are not removed also. A colloid mill may be used, ifnecessary, to prepare a colloidal solution or suspension suitablefor injection. Particulate matter may serve as condensationnuclei for samples; acid treatment may often dissolve

19、suchinterfering solids.6.2 Nonphenolic OrganicsCompounds which have thesame retention value as the phenolic compounds will interferewith the test. Such compounds may be eliminated by a suitablepreliminary separation technique.NOTE 1Refer to Test Methods D1783.6.3 Alkaline CompoundsUnder strongly alk

20、aline condi-tions, some chlorophenols may form salts which reduce theirvolatility in the test. Also, some nonphenolic organics, forexample, tar bases, may be more volatile in basic solution.Simple pH adjustment to near neutral or slightly acid willeliminate these interferences.6.4 GhostsElimination

21、of ghosts or memory peaks isrequisite before chromatographic analyses are possible. In thistest method, ghosts are minimized or eliminated by injecting 3L of water between all sample injections. This water washusually clears the injection port, column, and detector ofartifacts; however, repeated was

22、h injections may be necessaryto clear the system. The electrometer should be set at maximumsensitivity during the wash injections to facilitate detection ofghosts.NOTE 2Glass injector inserts are recommended. Inserts are easy toclean or replace and minimize clean-up difficulties.6.5 Other Interferen

23、cesIt is beyond the scope of this testmethod to describe procedures for eliminating all possibleinterferences which might occur, particularly with highlycontaminated industrial waste water.6In addition, the chro-matographic resolution of this test method is insufficient todifferentiate among some is

24、omeric alkyl phenols.7. Apparatus7.1 Chromatographic ColumnsColumns may be pur-chased or prepared by the analyst. Variations of columnloading, length, diameter, support size, treatment, etc., arepossible. Any column, for example, packed, wide bore (mega-bore) open tubular, analytical capillary, etc.

25、, may be used if itis shown to give precision and bias comparable to thoseobtained in the interlaboratory study of this test method. Thethree columns cited in this procedure may be modified with theunderstanding that the elution time and sensitivity may bealtered.7.1.1 Carbowax 20-M7A 3-mm by 3-m (1

26、8-in. by 10-ft)stainless steel column packed with 60/80 mesh ChromosorbW7,8(acid washed and hexamethyldisilazane, (HMDS)-treated) coated with 20 weight % of Carbowax 20M-TPA(terephthalic acid).7.1.2 Free Fatty Acid Phase, 1.5 mA 3-mm by 1.5-m(18-in. by 5-ft) stainless steel column packed with 70/80

27、meshChromosorb W (acid washed) coated with 5 weight % freefatty acid phase.7.1.3 Free Fatty Acid Phase, 3-mA 3-mm by 3-m (18-in.by 10-ft) stainless steel column packed with 60/80 meshChromosorb T coated with 10 % free fatty acid phase. Chro-mosorb T is a TFE-fluorocarbon 6 product which melts at327C

28、 and may begin to fuse above 250C. It is available fromsuppliers of gas chromatographic materials.7.2 Gas ChromatographA commercial or custom de-signed gas chromatograph with a column oven capable ofisothermal temperature control to at least 210 6 0.2C. A unitequipped for temperature programming wil

29、l facilitate elutionof a mixture of phenolics of wide boiling-point range. This testmethod describes an isothermal analysis using a single column-type gas chromatograph. Temperature programming is anoption of the analyst.7.3 Hydrogen Flame Ionization Detector.7.4 RecorderTo measure chromatographic o

30、utput at afull-scale range of 1 mV with a response time of 1 s.7.5 Syringe, 10-L.8. 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 specifications of the Commit-tee on Anal

31、ytical Reagents of the American Chemical Society,where such specifications are available.9Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determinations.8.2 Unless otherwise indicated, ref

32、erences to water shall beunderstood to mean reagent water that meets the purityspecifications of Type I or Type II water presented in Specifi-cation D1193.5Burttschell, R. H., et al., “Chlorine Derivatives of Phenol Causing Taste andOdor,” Journal American Water Works Association, Vol 51, No. 2, 195

33、9.6Baker, Robert A., “Trace Organic Analyses by Aqueous Gas-Liquid Chroma-tography,” Air and Water Pollution Institute Journal, Pergamon Press, Vol 10, 1966,pp. 591602.7The sole source of Carbowax known to the committee at this time is UnionCarbide, P.O. Box 4393, Houston, TX 77210. If you are aware

34、 of alternativesuppliers, please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.8The sole source of supply of Chromosorb known to the committee at this timeis Johns

35、Manville, P.O. Box 5108, Denver, CO 80217.9Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dors

36、et, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D2580 06 (2012)28.3 Carrier Gases Research grade nitrogen or helium ofhighest purity are used as carrier gases.8.4 Hydrogen (H) For use with the flame ionizationdetector; may

37、 be obtained using a hydrogen generator, or froma high-purity tank supply.8.5 Phenolic CompoundsResearch grades of high purityare required. Highest purity compounds may be prepared byredistillation, recrystallization, or by using a preparatory gaschromatographic instrument.NOTE 3WarningPhenolic comp

38、ounds are skin irritants. Appropri-ate safety measures should be taken to preclude contact with or inhalationof phenolic compounds.The following phenolic compounds are suggested:8.5.1 o-Chlorophenol,8.5.2 m-Chlorophenol,8.5.3 p-Chlorophenol,8.5.4 o-Cresol,8.5.5 m-Cresol,8.5.6 p-Cresol,8.5.7 2,3-Dich

39、lorophenol,8.5.8 2,4-Dichlorophenol,8.5.9 2,5-Dichlorophenol,8.5.10 2,6-Dichlorophenol,8.5.11 3,4-Dichlorophenol, and8.5.12 Phenol.9. Sampling9.1 Collect the sample in accordance with Practices D3370.9.2 Because of the possibility of oxidation or bacterialdecomposition of phenols in the sample, the

40、lapse of timebefore analyses should be kept to a minimum. In addition, keepthe sample cool and protected from atmospheric oxygen.10. Preparation of Chromatograph10.1 Install the packed column in the chromatograph usingsuitable fittings. The use of antigalling thread lubricant isadvisable.10.2 Conduc

41、t a leak test at approximately 103 kPa (15 psi)above the operating pressure by shutting off the downstreamend of the system and pressurizing from the carrier gas supply.Shut off the cylinder valve and observe the pressure gage. If nodrop is noted in 10 to 15 min, the system may be consideredtight. A

42、queous soap solutions may be used to locate minorleaks but this should be done with caution. If soap solutionenters the system, it may prove difficult to eliminate extraneouspeaks or stabilize the system. Do not use the soap method forleak testing near the ionization detector.10.3 Column Conditionin

43、g:10.3.1 Condition columns for at least 24 h at temperatures30 to 50C above the expected operating temperature beforeuse. Exercise caution to avoid exceeding the maximum allow-able temperature for both the packing and substrate.10.3.2 Disconnect the column at the end near the detectorbase to avoid d

44、eposition of volatiles on the detector duringconditioning.10.3.3 Adjust carrier gas flow to about 20 to 40 mL/min fora 3-mm (18-in.) diameter column.10.3.4 Occasional injection of 3 to 5 L of water duringconditioning facilitates elution of impurities.10.3.5 After conditioning, connect the column to

45、the flameionization detector.10.3.6 Adjust the hydrogen flow to the detector to about 25mL/min for a 3-mm (18-in.) diameter column. Adjust the airflow as specified in the instrument being used. Ignite thedetector.10.3.7 Adjust the column temperature to the desired level.10.3.8 Adjust the carrier gas

46、 flow rate to 20 to 40 mL/min.10.3.9 Observe the recorder base line. When a base line driftis no longer apparent, the column is ready for use.10.3.10 When the series of analyses are completed and thecolumn is to be moved and stored, it is advisable to seal or capthe ends.11. Operating Conditions for

47、 Analysis11.1 Typical operating conditions are summarized in Table1. These operating parameters may be varied but analytical andcalibration test variations must be reconciled in calculatingresults. For example, either nitrogen or helium may be used asthe carrier gas; recorder chart speeds of approxi

48、mately 30 in./hTABLE 1 Typical Operating Conditions for Chromatographic ColumnsColumn and PackingColumn Number1(see 7.1.1)3-mby3-mm(10-ftby18-in.)SS, 20 % Carbowax20M-TPA, 60/80 Chromo-sorb W-HMDS2(see 7.1.2)1.5-m by 3-mm(5-ft by18-in.)SS, 5 % FFAP, 70/80 Chromosorb W3(see 7.1.3)3-mby3-mm(10-ftby18-

49、in.) SS, 10 %FFAP Chromosorb TCarrier gas helium helium nitrogenCarrier gas flow, mL/min 25 35 60Temperature, C:Injection port 250 205 250Column 210 147 188Hydrogen for detector, mL/min 25 25 30Chart speed, in. (mm)/h 12 (305) 12 12Sensitivity, mV 1 1 1Electrometer range 1 0.1 1Attenuation 1 1 1Sample vol, L 1 1 1Figure reference Figs. 1 and 2 Fig. 5 Figs. 3 and 4D2580 06 (2012)3are commonly employed; sample sizes of 3 to 5 L are usuallyinjected (see Figs. 1-5).12. Method of Compound Identification12.1 Compound identification is based up