US4741830A
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Separation materials for thin layer chromatography
Assignee: Merck Patent GmbH
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Filing: 1987-02-11
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Granted: 1988-05-03
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Expires: 2007-02-11
Abstract
Abstract New separation materials for thin layer chromatography are based on carrier materials coated with an adsorbent silica gel layer which has been surface-modified by a silanizing agent after the coating step. The degree of covering of the modifying reagent can be adjusted in a defined and controllable manner, e.g., from 0.15 to 0.8 μmol/m 2 in the case of reversed phase materials and 1.2 to 2.5 μmil/m 2 in the case of hydrophilic materials. A process for the preparation of these separation materials is also provided.
Inventors
- 👤 Heinz E. Hauck
- 👤 Willi Jost
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 23:03
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/281; B01J20/02; B01J20/10; B01J20/103; B01J20/28; B01J20/28054; B01J20/28057; B01J20/286; B01J20/287; B01J20/30; B01J20/32; B01J20/3202; B01J20/3204; B01J20/3231; B01J20/3242; B01J20/3244; B01J20/3246; B01J20/3257; B01J20/3263; B01J20/3285; G; G01; G01N; G01N30/00; G01N30/90; B01J2220/00; B01J2220/50; B01J2220/54
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
175 words
A process for controlling water wettability from easily wettable to just wettable of a separation material sized and dimensioned for thin layer chromatography and comprising a carrier material coated with an absorbent silica gel layer whose surface has been modified by reaction with a silanizing agent, comprising, prior to the silanization step, homogeneously doping the silica gel surface by completely impregnating it with a solvent solution of a catalyst effective for catalyzing the silanization reaction of the silica gel surface with the silianization agent, said silica gel surface being doped to a preselected extent, solvent washing the resultant doped silica gel layer of excess catalyst prior to the silanization reaction, and adjusting the water wettability of the separation material by adjusting said impregnation step to achieve a degree of covering of the silica gel surface with an amount of catalyst effective to produce a degree of silanization of 0.15-0.8 μmol/m 2 for reversed phase materials or 1.2-2.5 μmol/m 2 for hydrophilic materials, the less the extent of covering the higher the degree of water wettability.
Claim 2
Dependent Claim
175 words
A process for controlling water wettability from easily wettable to just wettable of a separation material sized and dimensioned for thin layer chromatography and comprising a carrier material coated with an absorbent silica gel layer whose surface has been modified by reaction with a silanizing agent, comprising, prior to the silanization step, homogeneously doping the silica gel surface by completely impregnating it with a solvent solution of a catalyst effective for catalyzing the silanization reaction of the silica gel surface with the silianization agent, said silica gel surface being doped to a preselected extent, solvent washing the resultant doped silica gel layer of excess catalyst prior to the silanization reaction, and adjusting the water wettability of the separation material by adjusting said impregnation step to achieve a degree of covering of the silica gel surface with an amount of catalyst effective to produce a degree of silanization of 0.15-0.8 μmol/m 2 for reversed phase materials or 1.2-2.5 μmol/m 2 for hydrophilic materials, the less the extent of covering the higher the degree of water wettability.
Claim 3
Dependent Claim
20 words
A process according to claim 1, wherein the doping and silanization steps are carried out without the exclusion of moisture.
Claim 4
Dependent Claim
19 words
A process of claim 2, wherein the doping and silanization steps are carried out in the presence of moisture.
Claim 5
Dependent Claim
49 words
A process of claim 1, wherein the extent of the silanization of the silica gel surface is controlled by preselection of at least one of: (a) the composition of the catalyst, (b) the concentration of said solution, (c) the composition of the solvent, or (d) the time of impregnation.
Claim 6
Dependent Claim
19 words
A process of claim 4, wherein the catalyst concentration in the impregnating solution is 0.01 to 20% by weight.
Claim 7
Dependent Claim
25 words
A process of claim 4, wherein at least one intermediate washing is included between the doping and silanization steps to eliminate excess amounts of catalyst.
Claim 8
Dependent Claim
17 words
A process of claim 1, wherein the silanization step renders the silica gel surface hydrophobic but water-wettable.
Claim 9
Dependent Claim
81 words
A process according to claim 7, wherein the resultant modifying separation material has a degree of covering of 0.15 to 0.80 μmol/m 2 , and the silanization agent is a silane of the R--SiX 3 type, wherein Ris unsubstituted alkyl, aryl, or aralkyl of 1 to 20 C atoms in the alkyl chain and X is alkoxy or alkyl with 1 to 20 C atoms in the alkyl chain, with the proviso that at least one X is alkoxy or aralkoxy.
Claim 10
Dependent Claim
21 words
A process according to claim 8, wherein a mixture of acetyl chloride and glacial acetic acid is used as the catalyst.
Claim 11
Dependent Claim
19 words
A process according to claim 8, wherein tri, di- or mono-chloro- or -fluoro-acetic acid is used as the catalyst.
Claim 12
Dependent Claim
82 words
A process of claim 1, wherein the silanization renders the silica gel surface hydrophililc, the degree of covering thereof is 1.2 to 2.5 μmol/m 2 , and the silanization agent is a silane of the R--Six 3 type, wherein R is alkyl, aryl or aralkyl, in each case containing at least one epoxy or amino group, and X is alkoxy or alkyl of 1-20 C atoms in the alkyl chain, with the proviso that at least one X is alkoxy or aralkoxy.
Claim 13
Dependent Claim
27 words
A process according to claim 9, wherein the epoxy groups are additionally converted into diol groups by treatment with dilute acid after the modification of the surface.
Claim 14
Dependent Claim
18 words
A process according to claim 1, wherein the solvent washing step is performed directly before the silanizing reaction.
Claim 15
Dependent Claim
25 words
A process according to claim 1, wherein the amount of said catalyst is effective to produce a degree of silanization of 0.15-0.8 μmol/m 2 .
Claim 16
Dependent Claim
25 words
A process according to claim 1, wherein the amount of said catalyst is effective to produce a degree of silanization of 1.2-2.5 μmol/m 2 .
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-05-03 | 1991-11-02 | 1992-05-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-05-03 | 1995-11-02 | 1996-05-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-05-03 | 1999-11-02 | 2000-05-03 | $7700.00 | Window Closed / Lapsed |