VOC蘇碼罐采樣和GC分析方法

1、 VOLATILE ORGANIC COMPOUNDS (VOCs) in Ambient AirUsing Summa Canister Sampling and Gas Chromatography (GC) AnalysisTable 1A.Summary of Holding Times and PreservationAnalytical ParameterTechnical and Contract Holding TimesPreservationaTechnical: 14 days from collection;Contract: 12 days from receipt

2、atlaboratoryAmbient temperature; atnear atmospheric pressubTechnical: 48 hours from collection;Contract: 36 hours from receipt atlaboratoryAmbient temperature; atnear atmospheric pressuIndividual target compounds are listed in Table 1B.abThe laboratory must provide clean and certified 6-liter SUMMA

3、canisterswith the manufacturers serial number, or a unique permanent identificationnumber attached. For cleaning and certification of SUMMA canisters, followthe requirements specified in Sections 7.3 and 11 of EPA Method TO-14.cleaning and certification, the SUMMA canisters will be shipped to the fi

4、eldAfterwith a vacuum of 50 mm TORR.blank for each SDG.One canister shall be designated as the tripData Calculations and Reporting Units:Calculate and report the sample results as specified in the EPA Method TO-14.Perform sample quantitation using the response factor (RF) from the averageresponse fa

5、ctors of the calibrated range. Report results for all targetanalytes in concentration units of parts per billion by volume (ppbv).Report tentatively identified compounds (TICs) with a response of 10% of thenearest internal standard.TIC values should be estimated in ppbv based on the response of thec

6、orresponding internal standard. EPA Method TO-14Table 1B.Target Compound List and Contract Required Quantitation Limits forVOCs by EPA Method TO-14AnalyteCRQL(ppbv)Acetone5555252555222222222225522252Benzyl chlorideBromodichloromethaneBromomethane2-ButanoneCarbon tetrachlorideChlorobenzeneChlorodiflu

7、oromethaneChloroethane0Chloroform67-66-374-87-3Chloromethane3-Chloro-1-propeneCyclohexaneDibromochloromethane1,2-Dibromoethane1,2-Dichlorobenzene1,3-Dichlorobenzene1,4-DichlorobenzeneDichlorodifluoromethane1,1-Dichloroethane1,2-Dichloroethane1,1-Dichloroethenecis-1,2-Dichloroethene75-35-4156-59-2 Di

8、chlorofluoromethanet-1,2-Dichloropropenecis-1,2-DichloropropeneHeptaneHexachlorobutadieneHexaneMethylene chlorideMethyl methacrylate4-Methyl-2-pentanonealpha-Methyl styreneOctanen-PentanePropyleneStyrene75-69-42252Vinyl chloride27397 Xylenes (m- and p-)Xylene (o-)55 EPA Method TO-14Table 2.Summary o

9、f Calibration ProceduresAcceptance CriteriaCorrectiveGC/MS Tuning with 4bromofluorobenzene(BFB)Beginning of each 12 Ion abundance criteria 1. Identifyhour period during which in Table 4 of Method TO 2. MS tune14met before1. Terminat2. Recalibrbefore sampa, b, cContinuing Calibration Following ICV, a

10、fterevery 10 samples, andend of run%D between RF of CCV and 1. Recalibraavg. RRFs from ICAL #25% 2. Reanalyzelast good CVerification (CCV)(middle of thecalibration range)The ICAL low standard must be at concentrations equivalent to the CRQL.ICAL and CCV standards must contain all target analytes lis

11、ted in Table 1B.Report the retention time (RT) window for each analyte. Determine RTabcwindows as 3 x the standard deviation (SD) of the average initial calibrationRT for each analyte.Follow the tuning and calibration procedures in Section 10.2.2 and 10.2.3 ofEPA Method TO-14 and in SOP #1705, Secti

12、on 3.7.1 and 3.7.2 of OSWER Directive9360.4-05, May 1992.The standards must be traceable to a known certified source. EPA Method TO-14Table 3. Summary of Internal Quality Control ProceduresAcceptance CriteriaCorrective AcMethod Blank (MB) One for each day,minimum of one per SDG CRQL for each compoun

13、d 1. Investigatcontamination2. Reanalyzeprocessed witout of controOne per day or for each 80-120% of expected value 1. Reanalyze aassociated wicompliant PEaSurrogate Spikes Every sample, standardband method blank70-130% of expected value 1. Reanalyze anon-compliantrecoveries.LaboratoryDuplicatesOne

14、of every 10 samples RPD #20 between duplicate 1. Reanalyze aor one per day,whichever is greaterresults $5 times CRQL;CRQL for duplicateresults #5 times CRQLnon-compliantPE samples - The National Institute of Standards and Technology (NIST)standard reference materials (SRM) that are traceable to know

15、n concentrations.aSurrogates - The laboratory must demonstrate that the selected threesurrogates do not interfere with any target analytes.bDilute and reanalyze samples which contain one or more target analytes atconcentrations above the initial calibration range. Results for suchreanalyses should f

16、all within the mid-range of the calibration curve. Reportresults and submit documentation for both analyses. EPA Method TO-15 (January 1999)VOLATILE ORGANIC COMPOUNDS (VOCs) in Air(Ambient Air/Soil Vapor/Stack Gas) Samples Collected in Specially-PreparedCanistersand Analyzed by Gas Chromatography/Ma

17、ss Spectrometry (GC/MS)Table 1A.Summary of Holding Times and PreservationAnalytical ParameterTechnical and Contract Holding TimesPreservationaAmbient temperatubTechnical: 48 hours from collection;Contract: 36 hours from receipt atlaboratoryAmbient temperatuIndividual target compounds are listed in T

18、able 1B.abThe laboratory must provide the following equipment certified as clean:Cleaned and evacuated 6-liter SUMMA canisters with the manufacturersserial number, or a unique permanent identification number attached.For cleaning and certification of SUMMA canisters, follow therequirements specified

19、 in Section 8.4 of EPA Method TO-15 (January1999).Cleaned and preset ultra-low flow orifices for each ambient air samplepreset by the laboratory at a flow rate of 3.2 mL/min 10% and digitalflow meters capable of accurate measurements in the 3.2 mL/min range.Leak test all canisters prior to sample co

20、llection according to Section8.4 of Method TO-15 (January 1999).Data Calculations and Reporting Units:Calculate and report the sample results as specified in Section 10.8.4 of EPAMethod TO-15 (January 1999). EPA Method TO-15 (January 1999)Perform sample quantitation using the relative response facto

21、r (RRF) from thedaily continuing calibration standard.in concentration units of parts per billion by volume (ppbv).tentatively identified compounds(TICs) with a response of 10% of the nearestinternal standard. TIC values should be estimated in ppbv based on theresponse of the corresponding internal

22、standard.Report results for all target analytesReport EPA Method TO-15 (January 1999)Target Compound List, CAS Numbers, and Contract RequiredTable 1B.Quantitation LimitsAnalyteBenzeneBromomethaneCarbon TetrachlorideChlorobenzeneChloroethaneCAS Number71-43-274-83-9p-Xylene &m- Xyleneo-Xylene106-42-3

23、&108-38-395-47-62.01.00950.00470.40.2EPA Method TO-15 (January 1999)Table 2.Summary of Calibration ProceduresFrequencyAcceptance CriteriaCorrectiveBeginning of each 12hour period duringwhich standards andsamples are analyzedIon abundance criteria inTable 3 of Method TO-151. Identify2. MS tu

24、nemet beforeInitial Calibration(minimum blank + 5points for eachInitially; wheneverrequired, due tofailure of CCVRRFs $0.05 for eachanalyte; RSD for RRFs #30%1. Terminate2. Recalibrbefore sampanalyte) (ICAL) a, b, c Continuing CalibrationVerification (CCV)(middle of theFollowing ICV, every12-hour, a

25、nd end ofrun1. Recalibra2. Reanalyzelast good C65-135% of the expectedvalue1. Recalibra2. Reanalyzelast good CInternal Standards1. Investiga2. Re-analyzanalyzed dumalfunctiondRetention timeevaluation0.50 minute of the ISretention time in theassociated CCV1. Re-calibr2. Re-analyzto last gooThe ICAL l

26、ow standard must be at concentrations equivalent to the CRQL.ICAL and CCV standards must contain all target analytes listed in Table 1B.Report the retention time (RT) window for each analyte. Determine RT windows as 3 xabcthe standard deviation (SD) of the average initial calibration RT for each ana

27、lyte.Internal standards: Bromochloromethane, 1,4-Difluorobenzene, and Chlorobenzene-d5.dThe standards must be traceable to known certified source. Humidify calibrationstandards when used.EPA Method TO-15 (January 1999)Table 3.Summary of Internal Quality Control ProceduresAcceptance CriteriaCorrectiv

28、e AcMethod Blank (MB) CRQL for each compound1. Investigatcontamination2. Reanalyzeprocessed witout of controOne BS/BSD set per batchor SDG (1 MS/MSD set per20 samples minimum)65-135% of expectedvalue; #35% RPD betweenBS and BSD1. Report inSurrogate Spikes80-120% of expected value1. Reanalyzenon-comp

29、liantrecoveriesaLaboratoryDuplicatesOne per SDGRPD #20 between duplicateresults $5 times CRQL;CRQL for duplicate1. Reanalyzenon-compliantresults #5 times CRQL1,2-dichloroethane-d, Toluene-d , and 4-Bromofluorobenzene. If other surrogates are8a4used the laboratory must demonstrate that the surrogates do not interfere with anytarget analytes. The laboratory must also notify the Region in advance.Reanalyze samples containing target analytes at concentrations gr