HYDROGEN PEROXIDE DETECTOR AND METHODS

• US 20100144050A1
• Filed: 08/24/2007
• Published: 06/10/2010
• Est. Priority Date: 03/19/2007
• Status: Active Grant

• Current Assignee: Teledyne FLIR Defense Incorporated (Teledyne Technologies Incorporated)
• Original Assignee: Flir Detection, Inc. (Teledyne Technologies Incorporated)
• Inventors: La Grone, Marcus
• Granted Patent: US 8,647,579 B2
• Time in Patent Office: Days
• US Class Current: 436/135
• CPC Class Codes: G01N 21/766 of gases
• CPC Class Codes: G01N 2201/0221 Portable; cableless; compact; hand-held
• CPC Class Codes: G01N 33/0057 for warfare agents or explosives properties of explosives G01N33/227
• CPC Class Codes: Y10T 436/206664 Ozone or peroxide

Abstract

The current invention provides a detector and method suitable for sensing vapor-phase hydrogen peroxide. The detector utilizes a chemiluminescent material comprising a peroxide reactive compound, a dye and a solvent. Upon reaction with hydrogen peroxide, the chemiluminescent material will generate detectible light.

Claims

1. An apparatus for detecting vapor-phase hydrogen peroxide, said apparatus comprising:

a housing having at least one passageway therethrough, said passageway having an inlet and an outlet;

a pump in fluid communication with said passageway, said pump suitable for drawing gases from the exterior of said housing into said passageway;

a sensing assembly in fluid communication with said passageway, said sensing assembly comprising a chemiluminescent material and an optical light detector, said chemiluminescent material having at least one peroxide reactive component.

2. The apparatus of claim 1, further comprising a tip carried by said inlet, said tip designed to substantially preclude penetration of ambient light into said passageway.

3. The apparatus of claim 2, wherein said tip contains a fluid passageway comprising at least two ninety degree bends.

4. The apparatus of claim 2, wherein said tip contains a fluid passageway comprising at least four ninety degree bends.

5. The apparatus of claim 2, wherein said apparatus further comprises a heater suitable for heating said tip.

6. The apparatus of claim 1, wherein said sensing assembly further comprises a heater suitable for heating said chemiluminescent material.

7. The apparatus of claim 2, wherein said sensing assembly further comprises a single heater suitable for heating said chemiluminescent material and said tip.

8. The apparatus of claim 1, wherein said sensing assembly further comprises a solid support defining a reaction zone.

9. The apparatus of claim 8, wherein said solid support is a glass capillary with said chemiluminescent material carried by the interior walls of a capillary.

10. The apparatus of claim 9, wherein said chemiluminescent material is carried as a layer having a thickness of about 2 μ

m to about 10 μ

m.

11. The apparatus of claim 8, wherein said solid support is a plurality of glass beads positioned within a capillary, said glass beads carrying said chemiluminescent material.

12. The apparatus of claim 1, wherein said chemiluminescent material comprises a light-emitting material, a peroxide-reactive material and a carrier.

13. The apparatus of claim 12, wherein said light-emitting compound is selected from the group consisting of:

iptycene compounds, anthracenes, diphenylanthracenes, 9,10-bis(phenylethynyl) anthracene, benzanthracenes, phenanthrenes, naphthacenes, pentacenes, poly(arylene)s, poly(phenylene vinylene)s, poly(phenylene ethynylene)s, 5-amino-2,3-dihydrophthalazine-1,4-dione, 3-aminophthalhydrazide, 2,4,5-triphenylimidazole, 10,10′

-dialkyl-9,9′

-biacridinium salts, and 9-chlorocarbonyl-10-methylacridinium chloride.

14. The apparatus of claim 12, wherein said peroxide reactive compound is selected from the group consisting of bis(2,4,6-trichlorophenyl) oxalate, bis(2-carbopentyloxy-3,5,6-trichlorophenyl)oxalate, or oxalic acid bis[2,4,5-trichloro-6-(pentyloxycarbonyl)phenyl]ester, bis(2-nitrophenyl) oxalate, bis(2,4-dinitrophenyl) oxalate, bis(2,6-dichloro-4-nitrophenyl) oxalate, bis(2,4,6-trichlorophenyl) oxalate, bis(3-trifluoromethyl-4-nitrophenyl) oxalate, bis(2-methyl 4,6-dinitrophenyl) oxalate, bis(1,2-dimethyl-4,6-dinitrophenyl) oxalate, bis(2,4-dichlorophenyl) oxalate, bis(2,5-dinitrophenyl) oxalate, bis(2-formyl-4-nitrophenyl) oxalate, bis(pentachlorophenyl) oxalate, bis(pentafluorophenyl) oxalate, bis(1,2-dihydro-2-oxo-1-pyridyl) glyoxal, bis-N-phthalmidyl oxalate, bis(2,4,5 trichloro-6-carbopentoxyphenyl) oxalate, bis(2,4,5-trichloro-6-carbobutoxyphenyl) oxalate, bis(2,4,6-trichlorophenyl) oxalate, and phthalimido 3,6,6-trisulfo-2-naphthyl oxalate.

15. The apparatus of claim 12, wherein said peroxide reactive compound is an oxamide having the following formula

wherein R′

is selected from the group consisting of trifluoromethane sulfonyl, 2,4,5-trichlorophenyl, 2,3,4,5,6-pentafluorophenyl, 2,4-dinitrophenyl and phenyl and wherein R″

is selected from the group consisting of 2,4,5-trichlorophenyl, 2,3,4,5,6-pentafluorophenyl, 2,4-dinitrophenyl, phenyl.

16. The apparatus of claim 15, wherein R′

has an electron withdrawing group, selected from the group consisting of nitro, cyano, carbonyl, sulfonyl and trifluoromethyl.

17. The apparatus of claim 15, wherein R″

has an electron withdrawing group, selected from the group consisting of nitro, cyano, carbonyl, sulfonyl and trifluoromethyl.

18. The apparatus of claim 12, wherein said carrier is selected from the group consisting of:

ethylene glycol ethers, diethyl ether, diamyl ether, diphenyl ether, anisole, tetrahydrofuran, dioxane, ethyl acetate, propyl formate, amyl acetate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate, methyl formate, triacetin, diethyl oxalate, dioctyl terphthalate, citric acid ester, methyl benzoate, ethyl benzoate, butyl benzoate, benzene, ethyl benzene, butyl benzene, toluene, xylene, chlorobenzene, o-dichlorobenzene, m-dichlorobenzene, chloroform, carbon tetrachloride, hexachloroethylene, tetrachlorotetrafluoropropane, or combinations thereof.

19. The apparatus of claim 12, wherein said chemiluminescent material further comprises a catalyst is selected from the group consisting of:

sodium salicylate, tetrabutylammonium salicylate, potassium salicylate, lithium salicylate, tetrahexylammonium benzoate, benzyltrimethylammonium m-chlorobenzoate, tetraethyl ammonium stearate, calcium stearate, magnesium stearate, lithium stearate, triethylamine, pyridine, piperidine, imidazole, potassium trichlorophenoxide.

20. The apparatus of claim 1, further comprising a reservoir housing additional chemiluminescent material, said reservoir in fluid communication with said sensing assembly.

21. The apparatus of claim 12, wherein said light-emitting material and said peroxide-reactive material are a single compound.

23. The apparatus of claim 19 further comprising a tip carried by said inlet, said tip designed to substantially preclude penetration of ambient light into said passageway.

24. The apparatus of claim 20, wherein said apparatus further comprises a heater suitable for heating said tip.

25. The apparatus of claim 19, wherein said sensing assembly further comprises a heater suitable for heating said chemiluminescent material.

26. The apparatus of claim 19, wherein said solid support is a glass capillary with said chemiluminescent material carried by the interior walls of a capillary.

27. The apparatus of claim 23, wherein said chemiluminescent material is a layer having a thickness of about 2 μ

m to about 10 μ

m on said solid support.

28. The apparatus of claim 19, wherein said solid support is a plurality of glass beads positioned within a capillary, said glass beads carrying said chemiluminescent material.

29. The apparatus of claim 19, further comprising a reservoir housing additional chemiluminescent material, said reservoir in fluid communication with said sensing assembly.

31. The method of claim 27, wherein said chemiluminescent material is heated to a temperature between about 25°

C. and about 150°

C.

32. The method of claim 28, wherein said chemiluminescent material is heated to a temperature between about 45°

C. and about 65°

C.

33. The method of claim 27, wherein said step of contacting said chemiluminescent material with a vapor-phase hydrogen peroxide comprises passing said vapor-phase hydrogen peroxide over said chemiluminescent material at a flow rate between about 20 cm³/min to about 200 cm³/min.

34. The method of claim 27, wherein said step of contacting said chemiluminescent material with a vapor-phase hydrogen peroxide comprises passing said vapor-phase hydrogen peroxide over said chemiluminescent material at a flow rate between about 100 cm³/min to about 140 cm³/min.

35. The method of claim 27, wherein said vapor-phase hydrogen peroxide detector carries a tip and further comprising the step of heating said tip to a temperature between about 25°

C. and about 100°

C.

36. The method of claim 27, wherein said vapor-phase hydrogen peroxide detector carries a tip and further comprising the step of heating said tip to a temperature between about 45°

C. and about 85°

C.

37. The method of claim 27, wherein said chemiluminescent material reacts with said vapor-phase hydrogen peroxide, thereby generating visible light, within at least 10 seconds.

38. The method of claim 27, wherein said chemiluminescent material reacts with said vapor-phase hydrogen peroxide, thereby generating visible light, within at least 5 seconds.

39. The method of claim 27, wherein following said reaction of said chemiluminescent material with said vapor-phase hydrogen peroxide, said visible light fades and said chemiluminescent material is ready to react with another vapor-phase hydrogen peroxide within at least 10 seconds.

40. The method of claim 27, wherein following said reaction of said chemiluminescent material with said vapor-phase hydrogen peroxide, said visible light fades and said chemiluminescent material is ready to react with another vapor-phase hydrogen peroxide within at least 5 seconds.

41. The method of claim 27, wherein said gas carrying said vapor-phase hydrogen peroxide comprises at least 30 ppb vapor-phase hydrogen peroxide.

42. The method of claim 27, wherein said gas carrying said vapor-phase hydrogen peroxide comprises at least 10 ppb vapor-phase hydrogen peroxide.

43. The method of claim 27, wherein said vapor-phase hydrogen peroxide detector further comprises a reservoir containing said chemiluminescent material and further comprises the step of pumping said chemiluminescent material to said solid support.

44. The method of claim 27, further comprising the step of waiting sixty seconds or less following detection of vapor-phase hydrogen peroxide and subsequently contacting with said chemiluminescent material again with gas carrying a vapor-phase hydrogen peroxide for a period of time sufficient to permit said vapor-phase hydrogen peroxide to react with said chemiluminescent material wherein said reaction generates visible light.

46. The method of claim 42, further comprising heating said tip to a temperature between about 25°

C. and about 100°

C.

47. The method of claim 42, further comprising heating said tip to a temperature between about 45°

C. and about 85°

C.

48. The method of claim 42, wherein said chemiluminescent material is heated to a temperature between about 25°

C. and about 150°

C.

49. The method of claim 42, wherein said chemiluminescent material is heated to a temperature between about 45°

C. and about 65°

C.

50. The method of claim 42, wherein said step of flowing a gas carrying a vapor-phase hydrogen peroxide through said detector occurs at a flow rate between about 100 cm³/min to about 140 cm³/min.

51. The method of claim 42, wherein said vapor-phase hydrogen peroxide detector further comprises a reservoir containing said chemiluminescent material and further comprises the step of pumping said chemiluminescent material to said solid support.

52. The method of claim 42, further comprising the step of waiting sixty seconds or less following detection of vapor-phase hydrogen peroxide and subsequently contacting with said chemiluminescent material again with gas carrying a vapor-phase hydrogen peroxide for a period of time sufficient to permit said vapor-phase hydrogen peroxide to react with said chemiluminescent material wherein said reaction generates visible light.

53. The method of claim 42, wherein said chemiluminescent material reacts with said vapor-phase hydrogen peroxide, thereby generating visible light, within at least 10 seconds.

54. The method of claim 42, wherein said chemiluminescent material reacts with said vapor-phase hydrogen peroxide, thereby generating visible light, within at least 5 seconds.

55. The method of claim 42, wherein following said reaction of said chemiluminescent material with said vapor-phase hydrogen peroxide, said visible light fades and said chemiluminescent material is ready to react with another vapor-phase hydrogen peroxide within at least 10 seconds.

56. The method of claim 42, wherein following said reaction of said chemiluminescent material with said vapor-phase hydrogen peroxide, said visible light fades and said chemiluminescent material is ready to react with another vapor-phase hydrogen peroxide within at least 5 seconds.

57. The method of claim 42, wherein said gas carrying said vapor-phase hydrogen peroxide comprises at least 30 ppb vapor-phase hydrogen peroxide.

58. The method of claim 42, wherein said gas carrying said vapor-phase hydrogen peroxide comprises at least 10 ppb vapor-phase hydrogen peroxide.

22. An apparatus for detecting vapor-phase hydrogen peroxide, said apparatus comprising:

a housing having at least one passageway therethrough, said passageway having an inlet and an outlet;

a pump in fluid communication with said passageway, said pump suitable for drawing gases from the exterior of said housing into said passageway;

a sensing assembly in fluid communication with said passageway, said sensing assembly comprising a solid support carrying a liquid chemiluminescent material and an optical light detector positioned to detect light generated by said chemiluminescent material, said chemiluminescent material having at least one peroxide reactive component.

30. A method of detecting vapor-phase hydrogen peroxide comprising:

providing a vapor-phase hydrogen peroxide detector comprising a sensing assembly, said sensing assembly comprising a solid support carrying a liquid chemiluminescent material and an optical light detector positioned to detect light generated by said chemiluminescent material;

contacting with said chemiluminescent material with a gas carrying a vapor-phase hydrogen peroxide for a period of time sufficient to permit said vapor-phase hydrogen peroxide to react with said chemiluminescent material wherein said reaction generates visible light; and

,

detecting said visible light with said optical light detector.

45. A method of detecting vapor-phase hydrogen peroxide comprising:

providing a vapor-phase hydrogen peroxide detector comprising a tip and a sensing assembly in fluid communication with said tip, said sensing assembly comprising a solid support carrying a liquid chemiluminescent material and an optical light detector positioned to detect light generated by said chemiluminescent material;

heating said chemiluminescent material;

flowing a gas carrying a vapor-phase hydrogen peroxide through said detector at a flow rate between about 20 cm³/min to about 200 cm³/min;

contacting with said chemiluminescent material with said gas carrying a vapor-phase hydrogen peroxide for a period of time sufficient to permit said vapor-phase hydrogen peroxide to react with said chemiluminescent material wherein said reaction generates visible light; and

,

detecting said visible light with said optical light detector.