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Chromatography Techniques
Newtechnologiesaremakingiteasier,fasterandmore
reliabletodetectexplosivesorhighlyenergeticmaterials
beforetheycanbeused.
Thereareanumberoftechniquesthatareusedto
detectexplosives.Someofthesehavebeeninusefor
severalyears,othershaverecentlybeendevelopedor
enhanced.Thesedetectionsystemsincludeelectrochemical,
photoluminescence,massspectroscopy,gas
chromatography,laserinducedbreakdownspectroscopy
(LIBS),surfaceenhancedRamanscattering(SERS),
terahertz(THz)detection,ionmobilityspectroscopy(IMS),
colormetric,infrared(IR),Xrayandothers.Whilemanyof
thesesystemsworkwellonspecificexplosives,theyoften
aretimeconsuming,largeandnotportable,expensiveand
generallydontworkwellonothercompoundslikeillicit
drugsandinsecticides.
ResearchersatLawrenceLivermoreNationalLaboratory,
California,incollaborationwithFieldForensics,Inc.,St.
Petersburg,Fla.,recentlydevelopedthemicroTLC,a
miniaturized,fieldportabledetectionsystembasedonthin
layerchromatography(TLC)technologiesthatcanbeused
todetectandidentifyunknowns.Originallydevelopedto
identifymilitaryexplosives,themicroTLChasbeenmodified
toidentifyanddeterminethepurityofothercompoundsas
well.TheprincipleapplicationofthemicroTLCisforthe
militarymonitoringofbulkandresidualexplosivesandfor
lawenforcementmonitoringofillicitsubstances,suchas
explosivesanddrugs.
Thephysicaldetectionplatformis1.5by2.0"insizeand
comespackedinasmallpaddedsuitcasewithchemicals,
standardsandabatterypowersupply.Thedevicerequires
about3minutestoidentifyasamplewitheasystepbystep
onscreeninstructionsnocalculationsoroperator
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interpretationneeded,makingitusableforforensics,first
respondersandmilitarydiagnostics.
ThemicroTLCexplosivesdetectiondevicewasthewinnerof
a2014R&D100Awardfromoursisterpublication,R&D
Magazine,earlierthisyear.TheR&D100Awardsnowin
their52ndyeararegivenouttocommercialproducts
havingtechnologicalsignificanceandintroducedintothe
marketplaceoverthepastyear.
Operation
Ingeneral,TLCisusedtoseparatemixturesofsubstances
intotheircomponents.Itisananalyticaltoolwidelyused
becauseofitssimplicity,relativelylowcostandhigh
sensitivity.Itfunctionsonthesameprincipleasall
chromatographytechniquesacomponentwillhave
differentaffinitiesforthemobileandstationaryphases,and
thisaffectsthespeedatwhichitmigrates.Thisapproachis
usedtoidentifyacompoundinasamplebycomparingthe
distancethecompoundtraveledwiththedistancetraveled
ofaknowncompound(standard)runonthesameTLC
plate.Thisratioisreferredtoastheretentionfactor(Rf).
Whencomparingtwodifferentcompoundsunderthesame
conditions,thecompoundwiththelargerRfislesspolar
becauseitdoesnotsticktothestationaryphaseaslongas
thepolarcompound,whichwouldhavealowerRf.Because
ofitsuniquesize,separationformatandsolventapplication,
themicroTLCissuitableforrapididentificationofunknowns
forbothfieldandlaboratoryapplications.
ThemicroTLCusesaluminumbackedreversephaseC18
TLCplateschromatoplate(RP18)toidentifycommon
militaryexplosives(i.e.,TNT,tetryl,picricacid,ExplosiveD,
RXandHMX)allononeplate.Thedeviceusessmallerpre
cutplatesthatareprespottedwithexplosivestandards,
therebyeliminatingtheneedtoapplythestandardsinthe
field.Thestandardsremainviableformorethanayear.By
employingtheprespottedstandards,theentiresampling,
unknownspotting,developingandidentificationprocesscan
becompletedinlessthan3minutesinthefield.This
enhancedidentificationspeedassistsfirstrespondersand
lawenforcementpersonneltorapidlyassesssuspect
materials.
Samplesarequicklyextractedwithsolventsandthen
efficientlyspottedwithpipettesontotheplates.Theplates
arethenplacedinthedevelopingchamberwiththe
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developingsolventsuspendedinCabOSil.Afteradrying
timeof10to15sec,theplatescanbeexaminedunderUV
lighttoidentifythesuspectmaterialscomparedtothepre
spottedstandards.Abatterypacksuppliespowerforthefan
todrytheplatesafterdevelopmentandfortheUVlampto
readthedevelopedplatesothattheimagecanbedisplayed.
Allmaterialsarecontainedinthesuitcase.
Theuseofreversephaseplateshastheaddedadvantageof
beingabletochangetheelutionsolventandobtaina
differentseparationpattern.Thisfeatureprovidesamethod
toconfirmtheidentityofasuspectedexplosivewithout
changingtheidentityoftheTLCplate.Thisisimportantin
thosesituationswhentheremaybeanonexplosive
materialthathasthesameretentionfactorasoneofthe
standardexplosivecompounds.Asecondelutionsolvent
couldallowconfirmatoryevidencethatthesuspectedspot
ontheTLCplateisindeedtheexplosiveinquestion.
Advantages
ThemicroTLCanalyzesforensicandenvironmental
samplestodetectandidentifyexplosives,illicitdrugs,
insecticides,pesticidesandothertargetsinsamples
takenfromsurfaces,liquidsandsolids.
ThemicroTLCanalyzesforensicandenvironmentalsamplesto
detectandidentifyexplosives,illicitdrugs,insecticides,pesticides
andothertargetsinsamplestakenfromsurfaces,liquidsand
solids.
Thespeedwithwhichthissystemoperatesandthesolvent
handlingsystemaretwouniquefeatures.Thespeed
dependsontwodesignfeaturesthesignificantlysmaller
sizeoftheseparationplatformandtheslurrysolvent
handlingsystem.Thesmallerplateshavetheadvantageof
rapidelution,therebydrasticallyreducingseparationtimes
aswellastheamountofelutionsolvent.Theinclusionof
theprespottedstandardsreducesidentificationtimeofthe
unknownsamplesbecauseoftheircloseproximitytothe
unknownontheseparationplate.
ThesolventhandlingsystemforthemicroTLCis
significantlydifferentfromcompetingTLCtechnologies
becausethesolventisboundasanonliquidslurrywiththe
CabOSil.Thisadvantageisaresultofhavingasmall
overallsystem.Theslurryiseasytomanipulatebecauseits
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notaliquid.Also,itcanbedisposedofinanenvironmental
friendlymanner,unlikebulkTLCmethods.
Thisdevicefillsinthegapsofcompetingtechnologies,like
IMSandcolormetricsystems.Itprovidessample
specifications,wheretheothersystemsdonot.microTLC
canalsobeusedasafirststepforfurtherlabanalyses.
Competitivesystemsalsotendtobedestructiveofthe
sample,whilethemicroTLCisnot.ThemicroTLCprovides
preseparationforfollowuplabanalyses,forexample,by
massspectrometry.Thedeviceseparatesandidentifies
insteadofonlyidentifyingbygroup,likethatfor
colorimetricsystems.Italsohasbettersensitivitythan
similaranalysesbyRamanandIRtechnologies.IMS
detectionsystemsmaybemoresensitivethanthe
microTLC,buttheIMShasclearancelimitationsitcanbe
overwhelmedbyhighsignals.
ThemicroTLCisalsofasterinthatitdoesnotrequireany
warmuptimelikethatrequiredforIMS,Raman,IRandX
raysystems.Theseparationsarefastandidentifiable.IMS,
Raman,IRandXraysystemsalsohavesignificantlylarger
powerrequirementsthanthemicroTLC,whichisespecially
importantforitsportabilityrequirements.
Competitivetechnologies
IMSandcolorimetricdevicesaretheprimarycompetitive
devicesusedtodetectexplosives.Technologiesbasedon
IMS,alsoincludeiontrapmobilityspectrometry(IRMS)and
differentialmobilityspectrometry(DMS).LikethemicroTLC,
manyoftheIMSsystemsarealsoportablethesehandheld
devicesweighabout7lb.Theyarealsomoreexpensive
(about3x)thanthemicroTLC,andlikethecompetitive
colorimetricdetectiondevices,theyaresubjecttofalse
positives.IMSdevicesarealsosubjecttooverrange
problemstheydonottoleratehighsampleconcentrations.
Colorimetricbasedexplosivedetectionsystemsemploya
combinationofproprietarysolutionsandheatthatare
appliedtoasampleswipematerialthatcausescolorless
explosivestobecomecoloreddyes.Anycolorchangetothe
swipeindicatesthepresenceofexplosivesorenergetic
materials.Ifnocolorchangeoccurs,thereareno
explosivespresent,astestedbygovernmentagenices.
Colorimetricdetectiondevicesarealsosubjecttofalse
positivesduetotheirreactionwithnitritesandnitrates.
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Theyarelimitedbytheavailablecolorimetricchemistriesfor
thetargetanalyses.
Avariationonthecolorimetricexplosivedetectoristhe
aerosolbasedfieldtestkits.Thesespraysystemscanbe
usedasapreblastanalyticaltoolandpostblast
investigativetooltoscreenagainstpotentialterrorist
elements,andasatechnicalevaluationtestinsoil
remediationonhazardousmaterialcleanupsites.These
systemsareextremelyfastwithoneaerosolsprayproviding
resultswithinoneminute.Theyrealsoinexpensiveless
than$3pertest.Inthesetests,samplesareswipedonto
teststripsthatarethensprayedwiththereactivematerials
apinkblushappearingontheteststripsindicatesthe
presencesofanexplosiveorenergeticmaterial.
SpeciallydesignedXraydetectionsystemscanalsobeused
todetectexplosivesbyanalyzingthedensityoftheitems
beingexamined.Useofenhancedcomputedaxial
tomographysystemswithenhancedsoftware(containinga
libraryofexplosivematerialthreats)andfalsecolorcoding
allowoperatorstouseandevaluatethesespecialized
systems.
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