Claims
- 1. A process for the X-ray diffraction analysis of a compound comprising:
a) preparing a sample of the compound to be analyzed in slurry form; b) transferring the slurry to an assembly for a X-ray diffraction analysis, the assembly including a housing with an opening and an insert received in the housing opening, the insert having a recess for receiving the sample and a filter situated in the recess such that the filter supports the sample; c) creating a pressure differential across the filter to remove the liquid portion of the slurry while the insert is in the housing opening and thereby obtain the sample to be analyzed in powder form in the insert recess; d) transferring the assembly into a X-ray diffractometer; and e) performing X-ray diffraction analysis on the sample in the insert recess.
- 2. The process of claim 1 wherein the step of transferring the slurry comprises introducing the slurry into the insert recess.
- 3. The process of claim 1 wherein the step of creating a pressure differential comprises applying a vacuum to the filter through the insert recess.
- 4. The process of claim 1 wherein the step of creating a pressure differential comprises applying pressure to the filter through the insert recess.
- 5. The process of claim 1 wherein the step of receiving the insert in the housing opening comprises placing the insert into the housing opening from above the upper surface of the housing.
- 6. The process of claim 5 wherein the step of placing the insert comprises seating the insert within the housing opening.
- 7. An automated process for the X-ray diffraction analysis of multiple compounds comprising:
a) preparing samples of the compounds to be analyzed in slurry form; b) transferring each slurry to an assembly for retaining a X-ray diffraction analysis sample, the assembly including a housing with an array of openings and multiple inserts, one insert for each sample, each insert being received in a different housing opening, each insert having a recess for receiving the sample and a filter situated in the recess such that the filter supports the sample; c) while the inserts are in the housing, creating a pressure differential across each filter to remove the liquid portion of the slurry, leaving each sample to be analyzed in powder form in the insert recess; d) transferring the assembly into a X-ray diffractometer; and e) performing X-ray diffraction analysis in sequence on each of the samples situated in the insert recesses.
- 8. The process of claim 7 wherein the step of preparing the compounds to be analyzed comprises preparing an array of samples in a multi-well reactor.
- 9. The process of claim 7 wherein the step of transferring the compounds comprises introducing each sample in slurry form into the recess of a different insert.
- 10. The process of claim 9 wherein the step of introducing each sample in slurry form comprises depositing said sample with an automated liquid handler.
- 11. The process of claim 7 wherein the step of creating a pressure differential comprises simultaneously applying a vacuum to each filter through the recess in each insert.
- 12. The process of claim 7 wherein the step of creating a pressure differential comprises simultaneously applying pressure to each filter through the recess in each insert.
- 13. The process of claim 7 further comprising the steps of generating laboratory information data for each of the multiple samples to be analyzed and utilizing the data in the X-ray diffraction analysis.
- 14. An insert for use in an X-ray diffraction sample housing with an opening for receiving said insert, said insert comprising a recess extending through said insert and a filter, said recess being formed to receive a sample of the compound to be analyzed in slurry form; and means for retaining the filter in the recess.
- 15. The insert of claim 14 wherein the recess comprises a section for receiving the sample and a second section within which the filter is retained.
- 16. The insert of claim 14 wherein the filter-retaining means comprises a channel providing access to the filter through the recess.
- 17. The insert of claim 14 for use with means for creating a pressure differential across the filter.
- 18. The insert of claim 14 wherein said insert is cylindrical in shape.
- 19. The insert of claim 14 wherein said insert is disc-shaped.
- 20. An X-ray diffraction analysis filtration sample assembly comprising an insert; a housing with an opening for receiving the insert, the insert having a recess extending therethrough and means for cooperating with the housing, said recess being formed to receive a sample of the compound to be analyzed in slurry form, and a filter; and means for retaining the filter in the recess.
- 21. The assembly of claim 20 wherein the means for cooperating with the housing comprises a flange on said insert and additional means on the housing to support the flange.
- 22. The assembly of claim 20 wherein said housing comprises means for interacting with a X-ray diffractometer.
- 23. Apparatus for automated X-ray diffraction analysis of multiple compounds, comprising multiple inserts and a housing with an array of openings into which said inserts are received; each insert comprising a recess extending therethrough, each of said recesses being formed to receive a sample of the compound to be analyzed in slurry form, a filter, and means for retaining the filter in the recess to support the sample; said housing being adapted to be received in an X-ray diffractometer.
- 24. The apparatus of claim 23 wherein the inserts are removable from the housing.
- 25. The apparatus of claim 23 wherein the inserts are integrally formed in the housing.
- 26. The apparatus of claim 23 wherein the recess comprises a section for receiving the sample in slurry form and a second section within which the filter is retained.
- 27. The apparatus of claim 23 further comprising automated liquid handler means for introducing the samples in slurry form into the recess of each of the inserts.
- 28. The apparatus of claim 23 further comprising funnel means for facilitating introduction of the samples into the insert recesses.
- 29. The apparatus of claim 23 wherein the filter retaining means comprises a channel providing access to said filter through the recess.
- 30. The apparatus of claim 23 further comprising X-ray diffractometer means for analyzing the structure of the sample in the recess of each insert in the housing.
- 31. The apparatus of claim 30 wherein the X-ray diffractometer means comprises means for moving the housing relative to said X-ray diffractometer means to align each of the inserts, in sequence, with the X-ray diffractometer means.
- 32. The apparatus of claim 30 further comprising means for generating electronic data representative of each sample and for transferring the data to the X-ray diffractometer means.
- 33. The apparatus of claim 30 wherein the alignment means positions the inserts in relation to the X-ray diffractometer means according to two-dimensional coordinates.
- 34. The apparatus of claim 30 wherein the alignment means detects the presence of the inserts in the housing via a magnetic sensing means.
- 35. Apparatus for introduction and filtration of an array of samples of multiple compounds onto an array of X-ray diffraction analysis filter sample inserts, each insert including a recess which extends through the insert for receiving a sample of a compound in slurry form and a filter situated in the recess that supports the sample, said apparatus comprising a housing adapted to be received in a X-ray diffractometer, the housing comprising a plurality of openings into which the inserts are received, a funnel plate situated above said housing comprising a plurality of funnel shaped recesses each of which is aligned with the recess of a different one of the inserts and a vacuum plate located below said housing comprising a plurality of ports each of which is aligned with the recess of a different one of the inserts and means for connecting said ports to a vacuum source.
Parent Case Info
[0001] This application claims a benefit of priority from U.S. Provisional Application No. 60/371550, filed Apr. 10, 2002, the entire disclosure of which is herein incorporated by reference.
Provisional Applications (1)
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Number |
Date |
Country |
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60371550 |
Apr 2002 |
US |