Chromatography. TLC Thin layer chromatography Stationary phase Mobile phase.
Thin-Layer Chromatography a Field Technique for Propellant … · 2017-05-19 · Thin-Layer...
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ThinThin--Layer ChromatographyLayer Chromatographya Field Technique for a Field Technique for Propellant Stabilizers and Propellant Stabilizers and
Explosives AnalysisExplosives Analysis
Lawrence Livermore National LaboratoryLawrence Livermore National Laboratory
Rich Whipple, Greg Klunder, Leslie Carman, Peter Nunes, Rich Whipple, Greg Klunder, Leslie Carman, Peter Nunes, Marina ChiarappaMarina Chiarappa--Zucca, Jeanne Bazan (Ret.)Zucca, Jeanne Bazan (Ret.)
Global Demilitarization Symposium Global Demilitarization Symposium Reno, NVReno, NVMay, 2007May, 2007
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AgendaAgenda
Propellant Stability Analysis in the Field with TLCPropellant Stability Analysis in the Field with TLC
TLC Explosives ModuleTLC Explosives Module
Future DevelopmentsFuture Developments
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TLC Project TLC Project –– How We Got HereHow We Got Here
Project Inception Project Inception ---- 1996 1996
•• R & D Effort to Develop TLC for R & D Effort to Develop TLC for
Propellant StabilityPropellant Stability
•• From Screening to QuantificationFrom Screening to Quantification
•• FieldableFieldable Kit DevelopmentKit Development
•• Validation Trips Validation Trips –– 2000, 20022000, 2002
•• Validation testing Validation testing –– 2004 2004
•• PSSB Endorsement PSSB Endorsement –– 7/067/06
•• Fielding & Commercialization Fielding & Commercialization -- 20062006
2NNNODPA
2,42,2’2,4’
44,4’
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Propellant Stability Analysis in the Field with Propellant Stability Analysis in the Field with ThinThin--Layer ChromatographyLayer Chromatography
Commercialized to:Commercialized to:
Pelatron Inc. Pelatron Inc. –– Honolulu, HI Honolulu, HI (808) 543(808) 543--52905290
TLC Sales and SupportTLC Sales and Support(866) 460(866) 460--13561356www.pelatron.com/tlcwww.pelatron.com/tlc
PIKA International PIKA International –– Houston, TXHouston, TX(281) 340(281) 340--55235523
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Explosive Analysis ModuleExplosive Analysis Module
•• Typical Military ExplosivesTypical Military Explosives
TNT, NG, RDX, Picric Acid, Exp. D, CLTNT, NG, RDX, Picric Acid, Exp. D, CL--20, HMX, 20, HMX, TetrylTetryl, & , & PETNPETN
•• Other ExplosivesOther ExplosivesUrea, Urea NitrateUrea, Urea NitrateAmmonium Ammonium perchlorateperchlorate & nitrate, Sodium nitrate, chlorate, & nitrate, Sodium nitrate, chlorate, & & bromatebromate
•• Areas of UseAreas of UseTrace & Bulk analysis, Environmental CleanTrace & Bulk analysis, Environmental Clean--up, etc.up, etc.
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The TLC KitThe TLC Kit
TLC systemTLC system
Imaging Imaging
FiltrationFiltration
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Chromatography Solution #1Chromatography Solution #1
••View with UV lightView with UV light
••ColorColor
••View with white lightView with white light
••Develop and view with UV lightDevelop and view with UV light
Viewed under UV light after elution
TNT
RDX
Picricacid
Solvent front
Tetryl
HMXCL-20
Exp D
Viewed under UV light after elution
TNT
RDX
Picricacid
Solvent front
Tetryl
HMXCL-20
Exp D
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Chromatography Solution #2Chromatography Solution #2
1 2 3 4 5 6 7 8
Solvent front
Picric Acid
RDX
TNT
Exp D
HMX
Tetryl
CL-201 2 3 4 5 6 7 8
Solvent front
Picric Acid
RDX
TNT
Exp D
HMX
Tetryl
CL-20
••Order of explosives reversedOrder of explosives reversed
••Same type plate used with both solventsSame type plate used with both solvents
••Not all explosives appear in each viewNot all explosives appear in each view
••Second method confirms resultsSecond method confirms results
Picric acid
RDX
NGTNT
Exp D
HMX
TetrylPETNCL-20
Picric acid
RDX
NGTNT
Exp D
HMX
TetrylPETNCL-20
Exp D
HMX
TetrylPETNCL-20
Picric acid
RDX
NGTNT
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RF RF valuesvalues Syst. #1 Syst. #2
Explosive RP plate* RP plate**
picric acid 0.09 0.76
Exp D 0.09 0.76
HMX 0.31 0.41
RDX 0.39 0.44
Tetryl 0.61 0.16
NG 0.73 0.28
CL-20 0.28 0.01
PETN 0.78 0.08
TNT 0.86 0.23
* Non-Polar
** Polar
100++TNT
100+PETN
50+++CL-20
100+NG
50++Tetryl
50++RDX
50++HMX
25++Exp D
25++picric acid
DL (ng)Coloring
+ UVColoring
Sol’nUVExplosive
Visualization
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Urea and Urea Nitrate TLCUrea and Urea Nitrate TLC
Lane1 urea nitrate, 0.2 μg 2 urea nitrate, 0.5 μg3 urea nitrate, 1.0 μg4 urea nitrate, 2.0 μg5 urea, 0.2 μg6 urea, 0.5 μg7 urea, 1.0 μg8 urea, 2.0 μg
Solvent frontRf = 0.6
1 2 3 4 5 6 7 8
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Ions of interestIons of interest
Lane1 NH4 perchlorate, 2 μg2 NH4 perchlorate, 5 μg3 Na nitrite, 2 μg4 Na nitrite, 5 μg5 NH4 nitrate, 2 μg6 NH4 nitrate, 5 μg7 Na chlorate, 2 μg8 Na chlorate, 5 μg9 Na bromate, 2 μg10 Na bromate, 5 μg
1 2 3 4 5 6 7 8 9 10
NH4+
Na+
Solvent front
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Common ToolsCommon Tools
Sampling ToolsSampling Tools
Filtration SyringeFiltration Syringe
Light Box Light Box
TLC Process Tank TLC Process Tank
Dip TankDip Tank
TLC Plate TLC Plate –– Explosives and Urea NitrateExplosives and Urea Nitrate
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Expanding Capabilities Expanding Capabilities
Add quantification to explosives moduleAdd quantification to explosives module
Additional modules Additional modules –– CW, TIC, Street DrugsCW, TIC, Street Drugs
High Throughput Screening for Propellant StabilityHigh Throughput Screening for Propellant Stability
PrePre--Screen for strong Cat AScreen for strong Cat AUnknownsUnknowns
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4 4 10 10 16 16 22
0
1 2 3 4 5 6 7 8 91
2
3
4
5
6
High Throughput Screening for Propellant StabilityHigh Throughput Screening for Propellant Stability
Rapidly screen 50 propellant Rapidly screen 50 propellant samplessamplesEach spot contains all the Each spot contains all the components in the standardcomponents in the standardDetermine strong Category A’sDetermine strong Category A’sSamples prepared for TLC analysisSamples prepared for TLC analysisSpotted and colored with no Spotted and colored with no separation separation Uses same software and cameraUses same software and camera
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Conclusion Conclusion
Propellant analysis with TLC is commercialized Propellant analysis with TLC is commercialized
Fielded at TEAD, HWAD, APG, YPGFielded at TEAD, HWAD, APG, YPG
Explosive Module being addedExplosive Module being added
Expand propellant analysisExpand propellant analysis
Expand kit capabilitiesExpand kit capabilities
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AcknowledgementsAcknowledgements
Defense Ammunition CenterDefense Ammunition Center
Pelatron Inc.Pelatron Inc.
PIKA International Inc.PIKA International Inc.
Picatinny ArsenalPicatinny Arsenal