FASTGCWITHPID&FUVDETECTORSINFIELD ENVIRONMENTALANALY ENVIRONMENTAL ANALYSES IRONMENTALANAL Dr.JackDriscoll PIDAnalyzers,LLC,Sandwich,MA & Dr.

PhilipSmith , p , USDOL USDOL OSHA,HealthResponseTeam, SaltLakeCity,UT PittsburghConferencePaper#180 20P PittsburghConferencePaper#180 March2011 March 2011

TypesofSamples yp f p
BTEX ChlorinatedHC(TCA,TCE,PERC,MeCl2) Chlorinated HC (TCA TCE PERC MeCl2 ) GasolineHCs Solvents

=============================== Columnsselected ThickfilmMSCap(0.53mm)&aGasPro Columnsselected PLOT(0.32mm) 0.32mm) =============================== Pesticides&PCBs notconsideredhere Pesticides&PCBs Betterwithshort(5 ( ) p y Betterwithshort(510M)thinfilmcapillarycolumn

DETECTORS PID & FUV DETECTORS PID&FUV

Photoionization FarUVAbsorbance Far UV Absorbance

ComparisonofPLOT&ThickFilm Columns l
Compare PLOT to Thick Film columns for ComparePLOTtoThickFilmcolumnsfor speedforC1C6anes &enes speedforC1C6anes &enes What are the advantages/disadvantages of Whataretheadvantages/disadvantagesof each? A Anyadvantagesofresistivelyheated d f i i l h d columns? Heatup/cooldown?Powerutilized? Heatup/cooldown?Powerutilized? g g p y Advantagese.g comparisonofsensitiviity Advantagese.g comparisonofsensitiviity

GC312
PortableGC PortableGC Portable GC312 Features Batteryoperated Batteryoperated 8hours Has external charger or Hasexternalchargeror powerfromcarbattery Carriergassupply Carriergassupply >25 hours hours 1or2Detectors PID FID TCD Far UV FPD (S PID,FID,TCD,FarUV,FPD(S orP) TemperatureProgramming TemperatureProgramming NEW

GCSchematic GC Schematic

Focus is on the column/oven Small or no oven (direct heating of column) provides rapid temperature p g programming and faster analyses g y

OurDefinitions Our Definitions

#1 What is a FAST GC? A FAST GC has a low mass or resistively heated column that h l i ti l h t d l th t can be heated and/or cooled faster than a conventional oven ConditionsConditionsImproved heating efficiency is a must for battery operated GCs Fast GC run times in 5- 10 minutes instead of 20-30 minutes 520#2 What is a FAST GC column? Depends on the application; two examples are: 1. A 15m x 0.32 mm ID, PLOT that is resistively heated & can be cooled faster since it has a very small thermal mass 2. A thick film (5-10 ) 7.5-30 M capillary column that can (57.5separate gases & Solvents

PowerConsiderationsforaPortableGC Power Considerations for a Portable GC

Clearly,we do not need a heating rale like y we donotneedaheatingrale like 8000C/min;wearemoreconcernedwith powerutilization power utilization

FASTGC FAST GCAdvantages FASTGC

AdvantagesofFASTGC g Reducedruntimes Increasedsamplethroughput Fasterturnaroundofresults Improvedsignaltonoiseratio Improveddetectionlimits Widerrangeofanalytes Widerrangeofanalytes More samples means a more accurate assessment of the site Moresamplesmeansamoreaccurateassessmentofthesite DisadvantagesofFASTGC MoreExpensive More Expensive Minimal

ResistivelyHeatedColumnorLow MassOven

AgilentLowMassColumn(?)Oven Agilent Low Mass Column (?)Oven

The Agilent cap column is wound with Pt wire TheAgilentcapcolumniswoundwithPtwire thatprovidestheResistancevs Tfunctionthat isusedtoaccuratelydeterminethe is used to accurately determine the temperatureofthecolumnandanadditional wirewitharesistanceofapp8?Ohms.A wire with a resistance of app 8? Ohms A proportionalvoltagesource(48V)canbeused torapidlyheatthecolumnattemperaturesof to rapidly heat the column at temperatures of >1000C/mininsteadof100C/min.

Valco Low Mass Column (?) Oven LowMassColumn(?)Oven

VICI takes polyimidecoated fused silica (FST) and VICItakespolyimide coatedfusedsilica(FST)and removesthepolyimidelayer.Thenthe(FST)is electroplatedwithnickel.Theresultingnickelplated FSTtubingprovidesexcellentheattransfertothe FSTlining.TheNitubingiscoatedwithpolyimide whichprovidesflexibilityandelectricalinsulation. hi h id fl ibilit d l t i l i l ti Thepowerisappliedtoacentertapandtheendsare groundedsothatthecolumncanberapidlyheated grounded so that the column can be rapidly heated atratesupto8000C/min insteadof10200C/min 800 10

ComparisonofOvenCoolDown times
120

Cooldowntimes(Agilent)resistive(blue)&Lowmass(red)ovens

100

80 Oven nTemperatureC

60 Series1 Series2 40

20

0 0 1 2 3 Cooldownmin. Cool down min 4 5 6

C1toC6Alkanes wFUVon0.32mm C1toC6Alkanes (5 f l ) Capillary film ll

C1toC3HC(15ppm)on0.32mmcapat lowflowrate(1.5ccc/min) lowflowrate(1.5ccc/min) l fl ( / i )

PLOT Column (15M 00.32 mm)with TP PLOTColumn(15M00.32mm)withTP

PLOTColumn (30M00.32 (30M 00 32 mm)withTP )

Alkanes & BTEX on 7u MXT1 w PID &BTEXon7uMXT1wPID

DifferencesBetweenTFCapandPLOTfor C1C6 HC
Main differences are for C1C3HC MaindifferencesareforC1C3 HC C1
SeparationofCH4 &C2H6 betteronPLOT SeparationofC2H6 &C2H4 better on PLOT Separation of C &C betteronPLOT SeparationofC3H8 &C3H6 betteronPLOT El ti ElutionofC4 t C6 HC muchshorteronTFC f C toC HC HC h h t TFC

ComparisonofPLOTtoWideBoreThick FilmCapsensitivity il ii i
WCOTSensitivityThickFilm7ux0.53mmx7.5M;15cc&35C;PID0.2ccinj.X100 Compound Run PH C2H425ppm Avg pp H2S25ppm Avg g 3306 cts/ppm 1453cts/ppm /pp

Gaspro Sensitivity30Mx0.32mm;5cc&35C:PID 0.2ccinj.X100 C2H425ppm Avg. 1519 cts/ppm H2S25ppm Avg. 1739cts/ppm

SUMMARY
Thethickfilmcapscanprovidefasteranalyseswithexcellentseparations forawidevarietyofHC&solventsthanPLOTcolumns Thesensitivityforthethickfilmcolumnforgases(C2H4&H2S)issimilarto thePLOT AResistivelyheatedcolumncanprovidefasteranalysesthanasmallGC ovenbecauseofitslowmass Ifweprogramfrom30Cto100C,thetotaltimefortheRHCis10min., whereas,asmalloven(fancooled)willtake>20mintorunthisprogram. ThesetwodetectorsFUV&PIDcanprovidesubppmorppbdetectionof CH4,TCAtothexylenes ordecane inair,waterorsoil(headspaceforthe lattertwo) Ifweuseathickfilm30Mx0.32mmcolumnthatisresistivelyheated,we candomostanalysesin1012minandnearlydoublethevolumeof samplesdoneinanormalworkday.