Process of parallel sample preparation

• US 20020016006A1
• Filed: 10/03/2001
• Published: 02/07/2002
• Est. Priority Date: 07/18/2000
• Status: Active Grant

• Current Assignee: UOP Llc (Honeywell International Inc.)
• Original Assignee: UOP Llc (Honeywell International Inc.)
• Inventors: Murray, Richard C. Jr., Bem, David S., Surman, Cheryl M., Karlsson, Arne, Dahl, Ivar M., Lewis, Gregory J., Akporiaye, Duncan E., Ringwelski, Andrzej Z., Wendelbo, Rune
• Granted Patent: US 6,806,093 B2
• Time in Patent Office: Days
• US Class Current: 436/174
• CPC Class Codes: B01J 19/0046 Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays synthesis methods per se C40B50/00
• CPC Class Codes: B01J 2219/00313 the reactor vessels being formed by arrays of wells in blocks
• CPC Class Codes: B01J 2219/00333 Closures attached to the reactor vessels
• CPC Class Codes: B01J 2219/00351 Means for dispensing and evacuation of reagents
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/00659 Two-dimensional arrays
• CPC Class Codes: B01J 2219/00702 Processes involving means for analysing and characterising the products
• CPC Class Codes: B01J 2219/00707 separated from the reactor apparatus
• CPC Class Codes: B01J 2219/00745 Inorganic compounds
• CPC Class Codes: B01J 2219/00747 Catalysts
• CPC Class Codes: B01J 2219/00756 Compositions, e.g. coatings, crystals, formulations
• CPC Class Codes: B01L 2200/0657 Pipetting powder
• CPC Class Codes: B01L 2300/0829 Multi-well plates; Microtitration plates
• CPC Class Codes: B01L 3/0289 Apparatus for withdrawing or distributing predetermined quantities of fluid B01L3/02 takes precedence; sample taking G01N1/00; sample taking within automatic analysers G01N35/00; volume measuring in general G01F
• CPC Class Codes: B01L 3/50255 Multi-well filtration
• CPC Class Codes: B01L 3/5085 for multiple samples, e.g. microtitration plates
• CPC Class Codes: B02C 2017/065 with several compartments in the form of multiwell blocks
• CPC Class Codes: C40B 30/08 by measuring catalytic activity
• CPC Class Codes: C40B 40/18 Libraries containing only inorganic compounds or inorganic materials
• CPC Class Codes: C40B 60/14 for creating libraries
• CPC Class Codes: G01N 23/20 : by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
• CPC Class Codes: G01N 23/20025 : Sample holders or supports therefor
• CPC Class Codes: Y10T 436/25 : including sample preparation

Abstract

An apparatus and process for forming an array of powder samples arranged in predefined locations where all samples have a flat surface in a common plane has been developed. A monolithic block having a main support section having at least N perforations from a first surface of the main support through a second surface of the main support in predefined locations, where N is the number of samples in the array is provided. The monolithic block also has a flat support section covering the perforations of the main support section. All N samples are loaded simultaneously with sample X in perforation X of the main support where X is an integer from 1 to N. A flat surface of each sample where the flat surfaces are a common plane is formed by forcing the samples within the perforations against the flat support. The samples are retained in position within the perforations against the flat support, and are made ready for analysis since the flat surfaces of the samples are in predefined locations and are all in a common plane.

Claims

1. A method of forming an array of powder samples arranged in predefined locations where all samples have a flat surface in a common plane comprising:

(a) providing a monolithic block defining a main support section and a flat support section, said main support section having at least N depressions providing openings in a first surface of the main support section in predefined locations, where N is the number of samples in the array and N is at least two, said depressions in the form of perforations extending from a first surface of the main support section to a second surface defined by the main support section or the flat support section;

(b) loading sample X in depression X of the main support section where X is an integer from 1 to N;

(c) forming a flat surface of each sample where the flat surfaces are in a common plane by forcing the samples within the depressions against the flat support section;

(d) retaining the samples in position within the depressions using retaining means; and

(e) sufficiently exposing the flat surfaces of the samples in the predefined locations for testing over a common plane by limiting the thickness of the flat support section.

2. The method of claim 1 wherein the flat support section has a thickness of from 0.01 to 10 microns.

3. The method of claim 1 wherein the flat support section comprises a material that allows for the transmission of X-rays for testing of the sample.

4. The method of claim 1 wherein the flat support section comprises a planer portion of the monolithic block extending beyond the depressions with one surface of the planar section forming the flat surface contacted by the samples and the flat surfaces contacting the samples comprising a material with sufficient permeability to permit testing of the samples through the flat support section.

5. The method of claim 1 wherein the retaining means is selected from a group consisting of a mechanical device and a retaining material added to the depressions to fill additional volume.

6. The method of claim 1 further comprising at least partially covering a surface of the monolithic block with a layer of material where the material is selected to minimize any interference of the monolithic block in an analytical analysis of the samples.

7. The method of claim 6 wherein the layer of material is in the form of a film or a deposited layer of material.

8. The method of claim 6 wherein the analytical analysis is X-ray powder diffraction and the layer of material is selected from the group consisting of silver, gold, copper, zinc, nickel, and aluminum.

9. The method of claim 1 wherein the samples X are simultaneously loaded into depressions X of the main support section.

10. The method of claim 1 further comprising, after loading the samples in step (b) of claim 1, adding a wash solution to each depression, washing the samples, and removing the wash solution from each depression.

11. The method of claim 1 further comprising, after loading the samples in step (b) of claim 1, adding a grinding tool to each depression;

agitating the main support section and flat support section to simultaneously grind the samples in the depressions; and

removing the grinding tool from each depression.

12. The method of claim 1 wherein the forcing of the samples within the depressions of step (c) of claim 1 is accomplished by a technique comprising, adding a wash liquid and a grinding tool to each depression;

agitating the main support section and flat support section to simultaneously wash and grind the samples in the depressions; and

removing the wash liquid and grinding tool from each depression wherein said technique also washes and grinds the samples.

13. The method of claim 12 wherein the wash liquid is removed by a technique selected from the group consisting of, evaporating, drying, decanting, centrifuging, pipetting, freeze-drying, and adding sponging adsorbents.

14. The method of claim 1 further comprising mounting the monolithic block in an X-ray powder diffraction instrument so that the X-ray beam is directed at the flat surfaces of the samples to obtain an X-ray powder diffraction pattern of at least one sample.

15. The method of claim 1 further comprising synthesizing the array of samples in a set of synthesis cells prior to loading the samples as in step (b) of claim 1.

17. The sample holder of claim 16 wherein the flat support section allows for the transmission of X-rays for testing of samples retained in the depressions.

18. The sample holder of claim 16 further comprising a layer of material attached to a portion of a surface of the flat support section where the layer of material is selected to minimize any interference of the sample holder in an analytical analysis of the samples.

19. The sample holder of claim 18 wherein the layer of material is in the form of a film or deposited layer of material.

20. The sample holder of claim 18 wherein the layer of material is selected from the group consisting of silver, gold, zinc, copper, nickel, and aluminum.

21. The sample holder of claim 16 wherein said depressions are in the form of perforations that extend through the main support section and have cross sections, A, at the first surface greater than cross sections, B, adjacent the flat support section.

16. A sample holder comprising a monolithic block having a main support section having at least N depressions providing openings in a first surface of the main support section in predefined locations, where N is at least 2;

said monolithic block additionally having a flat support section covering at least one end of the openings of the main support section, having a thickness of from 0.01 to 10 microns, and comprising a material that permits testing of samples retained in the depressions through the flat support section.