USRE36811EExpiredUtility

Solid phase extraction medium

57
Assignee: MINNESOTA MINING & MFGPriority: Feb 7, 1991Filed: Oct 24, 1994Granted: Aug 8, 2000
Est. expiryFeb 7, 2011(expired)· nominal 20-yr term from priority
Inventors:Craig G. MarkellDonald F. HagenJames D. Luedtke
G01N 2030/527B01J 20/28033B01D 15/00B01J 20/28052B01J 20/28028G01N 2030/528B01D 15/08
57
PatentIndex Score
21
Cited by
31
References
37
Claims

Abstract

A method for isolating an environmentally hazardous organic contaminant from a fluid utilizes a solid phase extraction medium comprises a PTFE fibril matrix, and sorptive particles enmeshed in said matrix comprising more than 30 and up to 100 weight percent of porous organic particles, and less than 70 to 0 weight percent of porous (organic-coated or uncoated) inorganic particles, the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight. The extraction medium is useful in pesticide, phenolics, and residue of explosives separations. The separations can be efficiently performed in a stacked disk format.

Claims

exact text as granted — not AI-modified
We claim: 
     
       1. A method of isolating at least one organic contaminant from a fluid comprising the step of: passing a fluid containing at least one contaminant through at least one solid phase extraction medium comprising (a) a PTFE fibril matrix, and   (b) sorptive particles .Iadd.that are essentially non-water-swellable .Iaddend.enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight.     
     
     
       2. The method according to claim 1 further comprising the step of eluting said at least one contaminant from said extraction medium with an appropriate solvent. 
     
     
       3. The method according to claim 1 wherein said organic-coated inorganic particles comprise at least one of silica, alumina, titania, or zirconia to which is bonded an aliphatic or aromatic organic group. 
     
     
       4. The method according to claim 3 wherein said particle is silica and wherein said organic group is selected from the group consisting of amino, hydroxyl, chiral, cyano, cyclohexyl, phenyl, ethyl, butyl, octyl, and octadecyl. 
     
     
       5. The method according to claim 1 wherein the ratio of organic to inorganic particles by weight is 35 to 100:0 to 65. 
     
     
       6. The method according to claim 1 wherein the ratio of organic to inorganic particles by weight is 50 to 100:0 to 50. 
     
     
       7. The method according to claim 1 wherein said medium is a sheet material. 
     
     
       8. The method according to claim 1 wherein said contaminant is a pesticide. 
     
     
       9. The method according to claim 1 wherein said contaminant is a residue of an explosive. 
     
     
       10. The method according to claim 1 wherein said contaminant is a phenolic compound. 
     
     
       11. The method according to claim 1 wherein said organic particulate is a copolymer of styrene divinylbenzene and said inorganic particulate is C 18  -covalently bonded silica. 
     
     
       12. The method according to claim 1 wherein said contaminant is a polar or semi-polar substance. 
     
     
       13. The method according to claim 1 wherein said organic particles are a copolymer of styrene divinylbenzene or a derivative thereof. 
     
     
       14. The method according to claim 1 wherein said organic particles are a poly(meth)acrylic acid ester or a derivative thereof. 
     
     
       15. The method according to claim 1 wherein said organic particles are a polydivinylbenzene or a derivative thereof. 
     
     
       16. A solid phase extraction medium comprising (a) a PTFE fibril matrix, and   (b) sorptive particles .Iadd.that are essentially non-water-swellable .Iaddend.enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight.   
     
     
       17. The medium according to claim 16 wherein said organic particles are present in the range of 35 to 100 weight percent and said coated or uncoated inorganic particles are present in the range of 0 to 65 weight percent. 
     
     
       18. The medium according to claim 16 wherein in said medium said organic particles are present in the range of 50 to 100 weight percent and said coated or uncoated inorganic particles are present in the range of 0 to 50 weight percent. 
     
     
       19. The medium according to claim 16 wherein said organic particles are present in the range of 35 to 100 weight percent and said coated or uncoated inorganic particles are present in the range of 0 to 65 weight percent. 
     
     
       20. The medium according to claim 16 wherein said organic particles are present in the range of 50 to 100 weight percent and said coated or uncoated inorganic particles are present in the range of 0 to 50 weight percent. 
     
     
       21. The medium according to claim 16 wherein said contaminant is a polar or semi-polar substance. 
     
     
       22. The medium according to claim 16 wherein said organic particles are a copolymer of styrene divinylbenzene or a derivative thereof. 
     
     
       23. The medium according to claim 16 wherein said organic particles are a poly(meth)acrylic acid ester or a derivative thereof. 
     
     
       24. The medium according to claim 16 wherein said organic particles are a polydivinylbenzene or a derivative thereof. 
     
     
       25. The medium according to claim 16 wherein said organic-coated inorganic particles comprise at least one of silica, alumina, titania, or zirconia to which is bonded an aliphatic or aromatic organic group. 
     
     
       26. The medium according to claim 25 wherein said particle is silica and wherein said organic group is selected from the group consisting of amino, hydroxyl, cyano, cyclohexyl, phenyl, ethyl, butyl, octyl, and octadecyl. .[. 
     
     
       27.  The medium according to claim 16 wherein said sorptive particles are non-swellable..]. 
     
     
       28. A stack of at least 2 disks wherein at least one disk is a solid phase extraction .[.medium.]. .Iadd.material .Iaddend.comprising (a) a PTFE fibril matrix, and   (b) essentially non-water-swellable .[.and non-organic liquid swellable.]. sorptive particles enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight, and wherein in at least one of said disks said organic particles are selected from the group consisting of a copolymer of styrene divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing.   
     
     
       29. The stack of disks according to claim 28 wherein the media of said disks are of the same composition. 
     
     
       30. The stack of disks according to claim 28 wherein the media of at least two of said disks differ from each other in composition. 
     
     
       31. The stack of disks according to claim 28 wherein at least one disk comprises at least one of C 2  -C 8 , and C 18  -covalently bonded silica particles. 
     
     
       32. The stack of disks according to claim 28 wherein at least one disk comprises inorganic particles to which are bonded organic groups selected from the group consisting of amino, cyano, hydroxyl, cyclohexyl, phenyl, ethyl, butyl, octyl, octadecyl, and chiral groups. 
     
     
       33. A method of isolating at least one organic contaminant from a liquid comprising the step of: passing a liquid containing at least one contaminant through at least one solid phase extraction medium comprising (a) a PTFE fibril matrix, and   (b) sorptive particles .Iadd.that are essentially non-water-swellable .Iaddend.enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight.     
     
     
       34. The method according to claim 33 further comprising the step of eluting said at least one contaminant from said extraction medium with an appropriate solvent. 
     
     
       35. A method of isolating at least one organic contaminant from a fluid comprising the step of: passing a fluid containing at least one contaminant through at least one solid phase extraction medium comprising (a) a PTFE fibril matrix, and   (b) sorptive particles .Iadd.that are essentially non-water-swellable .Iaddend.enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight, and      eluting said at least one contaminant from said extraction medium with an appropriate solvent.   
     
     
       36. The medium according to claim 16 wherein the molecules of said organic coating of said inorganic particles are chiral. .Iadd. 
     
     
       37.  An extraction medium comprising (a) a PTFE fibril matrix, and   (b) sorptive particles enmeshed in said matrix having a change in volume of less than 0.5 when swollen in water, said sorptive particles comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene and divinylbenzene, a poly(metha)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles, the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight,      said medium being a solid phase extraction medium..Iaddend..Iadd.38. The extraction medium according to claim 37 wherein said sorptive particles have a change in volume of less than 0.1 when swollen..Iaddend..Iadd.39. The extraction medium according to claim 37 wherein said sorptive particles have a change in volume of less than 0.01 when swollen..Iaddend..Iadd.40. The extraction medium according to claim 37 wherein said porous organic particles have an average size in the range of 0.1 to 30 micrometers..Iaddend..Iadd.41. An extraction medium comprising   (a) a PTFE fibril matrix, and   (b) sorptive particles having a water sorptive capacity of less than 25 weight percent enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene and divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight,   
     
     
        said medium being a solid phase extraction medium..Iaddend..Iadd.42.  The extraction medium according to claim 41 wherein said sorptive particles have a water sorptive capacity of less than 5% by weight..Iaddend..Iadd.43. An extraction medium comprising (a) a PTFE fibril matrix, and   (b) highly crosslinked sorptive particles enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles selected from the group consisting of a copolymer of styrene and divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or a derivative of any of the foregoing, and   (2) less than 70 to 0 weight percent of porous, organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight,    said medium being a solid phase extraction medium..Iaddend..Iadd.44. The extraction medium according to claim 43 wherein said porous organic particles having an average size in the range of 0.1 to 30   
     
     
        micrometers..Iaddend..Iadd.45.  A disk comprising a solid phase extraction medium including (a) a PTFE fibril matrix, and   (b) sorptive particles that are essentially non-water-swellable enmeshed in said matrix comprising (1) more than 30 and up to 100 weight percent of porous organic particles, and   (2) less than 70 to 0 weight percent of porous organic-coated or uncoated, inorganic particles,      the ratio of sorptive particles to PTFE being in the range of 40:1 to 1:4 by weight, and wherein in said disk said organic particles are selected from the group consisting of a copolymer of styrene and divinylbenzene, a poly(meth)acrylic acid ester, a polydivinylbenzene, or derivative of any of the forgoing..Iaddend..Iadd.46. The method according to claim 1 wherein said fluid passes through said solid phase extraction medium at an angle of 90 degrees to the surface of said medium..Iaddend..Iadd.47. The method according to claim 1 wherein said method further comprises the step of chromatographically analyzing said at least one contaminant after isolation from said fluid..Iaddend.

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