IP Library Granted Patent US 8,815,606
Granted Patent B2
US 8,815,606 · App. 12/106,400 · Granted Aug 26, 2014

Thin-layer chromatography and colorimetric analysis of multi-component explosive mixtures

Inventors: Philip F. Pagoria (Livermore, CA); Alexander R. Mitchell (Livermore, CA); Richard E. Whipple (Livermore, CA); M. Leslie Carman (San Ramon, CA)
Assignee: Lawrence Livermore National Security, LLC.
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Quick Facts
Patent No.
US 8,815,606
App. No.
12/106,400
Granted
Aug 26, 2014
Kind
B2
Abstract

A thin-layer chromatography method for detection and identification of common military and peroxide explosives in samples includes the steps of provide a reverse-phase thin-layer chromatography plate; prepare the plate by marking spots on which to deposit the samples by touching the plate with a marker; spot one micro liter of a first standard onto one of the spots, spot one micro liter of a second standard onto another of the spots, and spot samples onto other of spots producing a spotted plate; add eluent to a developing chamber; add the spotted plate to the developing chamber; remove the spotted plate from the developing chamber producing a developed plate; place the developed plate in an ultraviolet light box; add a visualization agent to a dip tank; dip the developed plate in the dip tank and remove the developed plate quickly; and detect explosives by viewing said developed plate.

Claims (43)

1. A thin-layer chromatography method using a single thin-layer chromatography plate and a single colorimetric reagent for detection and identification of both military explosives and peroxide explosives in samples using the single thin-layer chromatography plate and using the single colorimetric reagent, consisting of the steps of:

providing a single reverse-phase thin-layer chromatography plate for detection and identification of both military explosives and peroxide explosives in samples;

preparing said single reverse-phase thin-layer chromatography plate for detection and identification of both military explosives and peroxide explosives in sample by marking spots on which to deposit the samples;

spotting one micro liter of a first standard onto one of said spots wherein said first standard is a standard for military explosives, spotting one micro liter of a second standard onto another of said spots wherein said second standard is a standard for peroxide explosives, and spotting samples onto other of said spots producing a spotted single reverse-phase thin-layer chromatography plate for detection and identification of both military explosives and peroxide explosives in sample;

adding eluent to a developing chamber;

adding said spotted single reverse-phase thin-layer chromatography plate to said developing chamber;

removing said spotted single reverse-phase thin-layer chromatography plate from said developing chamber producing a developed single reverse-phase thin-layer chromatography plate;

placing said developed single reverse-phase thin-layer chromatography plate in an ultraviolet light box;

adding a single colorimetric visualization reagent to a dip tank, wherein said single colorimetric visualization reagent is diphenylbenzidine in EtOH;

dipping said developed single reverse-phase thin-layer chromatography plate in said dip tank and remove said developed single reverse-phase thin-layer chromatography plate; and

detecting the military explosives and detecting the peroxide explosives by viewing said developed single reverse-phase thin-layer chromatography plate.

2. The thin-layer chromatography method for detection and identification of both military explosives and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of preparing said single reverse-phase thin-layer chromatography plate by marking spots on which to deposit the samples comprises touching said single reverse-phase thin-layer chromatography plate with a pencil to mark spots on which to deposit the samples.

3. The thin-layer chromatography method for detection and identification of both military explosives and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of spotting samples onto other of said spots producing a spotted single reverse-phase thin-layer chromatography plate comprises spotting one micro liter of one of said samples onto another of said spots and waiting for said one micro liter of one of said samples to dry before spotting another of said samples onto other of said spots.

4. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of adding eluent to a developing chamber comprises pipeting ten milliliter of toluene:propan-2-ol into said developing chamber.

5. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of adding eluent to a developing chamber comprises pipeting ten milliliter of water:methanol:acetonitrile into said developing chamber.

6. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of add said spotted single reverse-phase thin-layer chromatography plate to said developing chamber includes allowing said spotted single reverse-phase thin-layer chromatography plate to develop for between fourteen minutes and thirty-five minutes.

7. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said developing chamber contains solvent and wherein said step of removing said spotted single reverse-phase thin-layer chromatography plate from said developing chamber producing a developed single reverse-phase thin-layer chromatography plate includes allowing said solvent to evaporate.

8. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said developing chamber contains solvent and wherein said step of removing said spotted single reverse-phase thin-layer chromatography plate from said developing chamber producing a developed single reverse-phase thin-layer chromatography plate includes allowing said solvent to evaporate for five minutes.

9. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of placing said developed single reverse-phase thin-layer chromatography plate in an ultraviolet light box includes photographing said developed single reverse-phase thin-layer chromatography plate.

10. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of adding a visualization agent to a dip tank comprises adding fifty milliliters of two one hundredths of a percent diphenylbenzidine in ethanol to a dip tank.

11. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatography plate of claim 1 wherein said step of detecting explosives by viewing said developed single reverse-phase thin-layer chromatography plate includes photographing said developed single reverse-phase thin-layer chromatography plate.

12. A thin-layer chromatography method using a single thin-layer chromatography plate and a single colorimetric reagent for detection and identification of both common military and peroxide explosives in samples using the single thin-layer chromatography plate and using the single colorimetric reagent, consisting of the steps of:

providing a single reverse-phase thin-layer chromatography plate for detection and identification of both military explosives and peroxide explosives in samples;

preparing said single reverse-phase thin-layer chromatography plate for detection and identification of both military explosives and peroxide explosives in sample by marking spots on which to deposit the samples by touching said single reverse-phase thin-layer chromatography plate with a marker;

spotting one micro liter of a first standard onto one of said spots wherein said first standard is a standard for military explosives, spotting one micro liter of a second standard onto another of said spots wherein said second standard is a standard for peroxide explosives, and spotting samples onto other of said spots producing a spotted single reverse-phase thin-layer chromatography plate for detection and identification of both military explosives and peroxide explosives in sample;

adding eluent to a developing chamber;

add said spotted single reverse-phase thin-layer chromatography plate to said developing chamber;

removing said spotted single reverse-phase thin-layer chromatography plate from said developing chamber producing a developed single reverse-phase thin-layer chromatography plate;

placing said developed single reverse-phase thin-layer chromatography plate in an ultraviolet light box;

adding a single colorimetric visualization reagent to a dip tank;

dipping said developed single reverse-phase thin-layer chromatography plate in said dip tank and remove said developed single reverse-phase thin-layer chromatography plate quickly; and

detecting the military explosives and detecting the peroxide explosives by viewing said developed single reverse-phase thin-layer chromatography plate.

13. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of preparing said single reverse-phase thin-layer chromatography plate by marking spots on which to deposit the samples by touching said single reverse-phase thin-layer chromatography plate with a marker comprises touching said single reverse-phase thin-layer chromatography plate with a pencil.

14. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of spotting samples onto other of said spots producing a spotted single reverse-phase thin-layer chromatography plate comprises spotting one micro liter of one of said samples onto another of said spots and waiting for said one micro liter of one of said samples to dry before spotting another of said samples onto other of said spots.

15. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 14 wherein said step of spotting samples onto other of said spots producing a spotted single reverse-phase thin-layer chromatography plate comprises spotting one micro liter of one of said samples onto another of said spots and waiting for said one micro liter of one of said samples to dry before spotting another of said samples onto other of said spots and repeating said step of spotting one micro liter of one of said samples onto another of said spots and waiting for said one micro liter of one of said samples to dry before spotting another of said samples onto other of said spots.

16. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of adding eluent to a developing chamber comprises pipeting ten milliliter of toluene:propan-2-ol into said developing chamber.

17. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of adding eluent to a developing chamber comprises pipeting ten milliliter of water:methanol:acetonitrile into said developing chamber.

18. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of adding said spotted single reverse-phase thin-layer chromatography plate to said developing chamber includes allowing said spotted single reverse-phase thin-layer chromatography plate to develop for between fourteen minutes and thirty-five minutes.

19. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said developing chamber contains solvent and wherein said step of removing said spotted single reverse-phase thin-layer chromatography plate from said developing chamber producing a developed single reverse-phase thin-layer chromatography plate includes allowing said solvent to evaporate.

20. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said developing chamber contains solvent and wherein said step of removing said spotted single reverse-phase thin-layer chromatography plate from said developing chamber producing a developed single reverse-phase thin-layer chromatography plate includes allowing said solvent to evaporate for five minutes.

21. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of placing said developed single reverse-phase thin-layer chromatography plate in an ultraviolet light box includes photographing said developed single reverse-phase thin-layer chromatography plate.

22. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of adding a visualization agent to a dip tank comprises adding fifty milliliters of two one hundreths of a percent diphenylbenzidine in ethanol to a dip tank.

23. The thin-layer chromatography method for detection and identification of both common military and peroxide explosives in samples using a single thin-layer chromatograph plate of claim 12 wherein said step of detecting explosives by viewing said developed plate includes photographing said developed single reverse-phase thin-layer chromatography plate.

Assignments (3)
CONFIRMATORY LICENSE (SEE DOCUMENT FOR DETAILS) Recorded May 19, 2020
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 052701/0089 →
CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNORS NAME NEEDS TO BE CORRECTED. (PHILLIP F. PAGORIA SHOULD BE PHILIP F. PAGORIA)CORRESPONDENCE INFORMATION CHANGED. PREVIOUSLY RECORDED ON REEL 021045 FRAME 0870. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT OF ASSIGNOR'S INTEREST. Recorded Jun 17, 2008
From: PAGORIA, PHILIP F.; MITCHELL, ALEXANDER R.; WHIPPLE, RICHARD E.; CARMAN, M. LESLIE
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 021108/0533 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 29, 2008
From: PAGORIA, PHILLIP F.; MITCHELL, ALEXANDER R.; WHIPPLE, RICHARD E.; CARMAN, M. LESLIE
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 021045/0870 →
Continuity (2)
Provisional Application 60930781 · May 17, 2007
Related Publication 20090221085A1 · Sep 3, 2009