PAHs - Thermo Scientific

Application Note:ANCCSGCPAHWTRAnalysis of Polynuclear Aromatic Hydrocarbons(PAHs) in Wastewater by GC/MSAnila I Khan, Rob Bunn, Tony Edge, Thermo Fisher Scientific, Runcorn, Cheshire, UKKey Words• US EPA 610• US EPA 8100• Polynucleararomatichydrocarbons• PAH’s• waste water• TG-5SilMS• 5% PhenylIntroductionUS EPA method 610 is an analytical GC/MS method usedfor determining a range of polynuclear aromatic hydrocarbons(PAHs) in municipal and industrial wastewater.This method was developed by the US EnvironmentalProtection Agency to monitor industrial and municipaldischarges under 40 CFR 136.1.EPA method 610 was performed using a splitlessinjection mode on a Thermo Scientific TRACE GC coupledto a Thermo Scientific Ion Trap mass spectrometer.The Thermo Scientific TraceGOLD TG-5SilMS columnprovides excellent performance for the analysis of PAHs, inaccordance with EPA method 610. It can also be used forthe analysis of PAHS for EPA method 8100.GoalTo demonstrate the suitability and performance ofTraceGOLD TG-5SilMS for the analysis of EPA method610; PAHs in wastewater.Experimental detailsThe PAHs stated in the EPA method 610 were run on aTRACE GC fitted with a TriPlus autosampler. The Iontrap mass spectrometer was used in a segmented mode toallow precise control of groups of ions for improved ionstatistics and ion ratios. The column used for analysis ofthe series of PAHs was a low polarity silarylene phase,with selectivity comparable to a 5% diphenyl/95% dimethylpolysiloxane phase. The data was acquired andprocessed using Thermo Scientific Xcalibur data handlingsoftware.Sample preparationA pre-mixed 1 ng/µL of PAHs standard solution prepared in dichloromethaneand benzene was used for the analysis.ColumnPart NumberTraceGOLD TG-5SilMS, 30 m × 0.25 mm × 0.25 µm, 26096-1420Guard Column 2 m × 0.32 mm260RG497Press-Fit Union 64000-001Thermo Scientific TriPlus AutosamplerSample volume 1 µLTRACE GC UltraOven Program60 °C (5 min), 8 °C/min, 300 °C (10 min)Equilibration Time0.5 minInjector275 °C, Splitless (1 min)Split Flow30 mL/minColumn FlowHelium, 1.5 mL/min (constant flow)Transfer Line Temperature 300 °CThermo Scientific Ion Trap MSMS TypeITD 230LT (250 L turbo pump)MS Source Temperature 225 °CMS Source Current 250 µAElectron Energy70 eVFilament Delay5 minMS Aquisition ModeEI+, 45-450 amu Segmented ScanConsumablesPart NumberBTO 17 mm septa 313032113 mm ID Focus Liner, 105 mm long 45350032Liner graphite seal 2903340610 µL, 80 mm Syringe 36502019Graphite ferrules to fit 0.32 mm id columns 29053487Graphite/vespel 0.25 mm ID ferrules for GC/MS interface 290334962 mL clear vial and Si/PTFE seal 60180-599

ResultsThe requirements for the EPA method 610 were achievedwith separation of all of the sixteen PAHs using theTraceGOLD TG-5SilMS on a GC/MS system. Thestationary phase in the TraceGOLD TG-5SilMS providesexcellent performance due to minimal interaction of activecompounds with active sites on the column, therefore nosignificant peak tailing was observed. The excellentseparation achieved using this column makes it applicableto the analysis of EPA method 8100. Figure 1 shows theTIC chromatogram for a 1 ng/µL of PAHs in a mixture ofdichloromethane and benzene obtained using aTraceGOLD TG-5SilMS column. Table 1 shows the peakidentification of compounds according to the retentiontimes on a TraceGOLD TG-5SilMS.ConclusionsThe TraceGOLD TG-5SilMS column demonstratedexcellent performance for the analysis of PAHs displayingFigure 1: TIC chromatogram of 1 ng/µL of PAHs separated on a TG-5SilMS columnPAHsIS132ISPeak No.Internal StandardISNaphthalene 1Acenaphthylene 2Internal StandardISAcenaphthene 3Fluorene 4Internal StandardISPhenanthrene 5Internal StandardISAnthracene 6Fluoranthene 74PAHIS 5 IS 6excellent selectivity. The chromatogram illustrates thesuperior performance of the TraceGOLD TG-5SilMS forthe analysis of PAHs in accordance with EPA methods610 and 8100.References1. EPA method 610:www.epa.gov/waterscience/methods/method/organics/610.pdf2. EPA method 8100:www.epa.gov/osw/hazard/testmethods/sw846/pdfs/8100.pdfAcknowledgementMany thanks to the dedicated team at Cromlab S.L.,Barcelona, Spain for all of their help providing the data forthis application.7 8Time (min)Peak No.Pyrene 8Benz(a)anthracene 9Chrysene 10Benzo(b)fluoranthene 11Benzo(k)fluoranthene 12Benzo(a)pyrene 13Internal StandardISIndeno(1,2,3-cd)pyrene 14Dibenz(a,h)anthracene 15Benzo(g,h,i)perylene 1610911 12 13IS151614In addition to theseoffices, Thermo FisherScientific maintainsa network of representativeorganizationsthroughout the world.North AmericaUSA and Canada+1 800 332 3331EuropeFrance+33 (0)1 60 92 48 34Germany+49 (0) 2423 9431 -20or -21Switzerland+41 56 618 41 11United Kingdom+44 1928 534110AsiaJapan+81 3 5826 1615China+86-21-68654588or +86-10-84193588800-810-5118India1800 22 8374 (toll-free)+91 22 6716 2200Thermo FisherScientific AustraliaPty Ltd1300 735 292 (free calldomestic)Thermo FisherScientific NewZealand Ltd0800 933 966 (free calldomestic)All Other Enquiries+44 (0) 1928 534 050TechnicalSupportNorth America800 332 3331Outside NorthAmerica+44 (0) 1928 534 440Table 1: List of Polynuclear Aromatic Hydrocarbons (PAHs) compounds according to retention timeswww.thermoscientific.com/chromatography©2011 Thermo Fisher Scientific Inc. All rights reserved. All trademarks are the property of Thermo Fisher Scientific Inc. and its subsidiaries.Specifications, terms and pricing are subject to change. Not all products are available in all countries. Please consult your local sales representative for details.ANCCSGCPAHWTR 0311Part of Thermo Fisher Scientific