Apparatus and method for characterizing libraries of different materials using x-ray scattering

• US 20040017896A1
• Filed: 05/22/2003
• Published: 01/29/2004
• Est. Priority Date: 12/18/1998
• Status: Abandoned Application

• Current Assignee: Freeslate Inc. (Unchained Labs Inc.)
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Bennett, James, Jain, Rakesh, Hajduk, Damian
• Application Number:
  US10/448,039
• Publication Number:
  US 20040017896A1
• Time in Patent Office: Days
• US Class Current: 378/208
• 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 2219/00315 Microtiter plates
• CPC Class Codes: B01J 2219/00511 Walls of reactor vessels
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/00596 Solid-phase processes
• CPC Class Codes: B01J 2219/00659 Two-dimensional arrays
• CPC Class Codes: B01J 2219/00704 integrated with the reactor apparatus
• CPC Class Codes: B01J 2219/00707 separated from the reactor apparatus
• CPC Class Codes: B01J 2219/00745 Inorganic compounds
• CPC Class Codes: C40B 40/18 Libraries containing only inorganic compounds or inorganic materials
• 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: Y10T 436/25 including sample preparation

Abstract

An apparatus for characterizing a library containing an array of samples. The apparatus includes an x-ray beam directed at the library, a chamber housing the library and a beamline for directing the x-ray beam onto the library in the chamber. The chamber may include a translation stage that holds the library and that is programmable to change the position of the library relative to the x-ray beam and a controller that controls the movement of the translation stage to expose an element to the x-ray beam in order to rapidly characterize the element in the library. During the characterization, the x-ray beam diffracts upon impinging the element and a detector detects the diffracted x-ray beam in order to generate characterization data for the element.

Claims

1. Apparatus for characterizing a library containing a plurality of samples, said apparatus comprising:

an x-ray source for producing an x-ray beam;

a chamber positioned in the x-ray beam having an interior sized and shaped for holding said library of samples;

a stage connected to the chamber for moving the library containing the plurality of samples relative to the x-ray beam to align a pre-selected sample of said plurality of samples with the x-ray beam to expose the pre-selected sample to the x-ray beam thereby causing the x-ray beam to diffract and form a diffraction pattern characteristic of materials present in the pre-selected sample; and

a detector mounted adjacent the stage for detecting the diffraction pattern resulting from the diffracted x-ray beam thereby permitting characterization of the pre-selected sample of said plurality of samples in the library.

2. Apparatus as set forth in claim 1 further comprising a beamline positioned along the x-ray beam for directing the x-ray beam toward the library containing the plurality of samples when the library is positioned in the interior of the chamber.

3. Apparatus as set forth in claim 2 wherein at least one of the detector and the beamline are moveable with respect to the stage so as to permit changes in an angle between a first line extending from the beamline to the preselected sample of said plurality of samples and a second line extending from the pre-selected sample and the detector.

4. Apparatus as set forth in claim 1 further comprising a controller operatively connected to the stage for controlling movement of the stage thereby determining which sample of said plurality of samples in the library is exposed to the x-ray beam.

5. Apparatus as set forth in claim 4 wherein the controller includes a computer system having a user interface permitting independent user selection of which sample of said plurality of samples in the library is exposed to the x-ray beam and of an order in which said samples are selected for exposure to the x-ray beam.

6. Apparatus as set forth in claim 1 wherein the stage comprises a first positioning mechanism for moving the library containing the plurality of samples in a first direction relative to the x-ray beam and a second positioning mechanism for moving the library containing the plurality of samples in a second direction relative to the x-ray beam different than said first direction.

7. Apparatus as set forth in claim 6 wherein said second direction extends normal to said first direction.

8. Apparatus as set forth in claim 6 wherein each of said first and second positioning mechanisms includes a stepper motor.

9. Apparatus as set forth in claim 1 in combination with a library containing a plurality of samples.

10. A method for operating an x-ray characterization apparatus for characterizing a library containing a plurality of samples arranged in a predetermined pattern, said apparatus comprising an x-ray source for producing an x-ray beam, a stage for moving the library to align a pre-selected sample of said plurality of samples with the x-ray beam, and a detector for detecting a diffraction pattern, said method comprising the steps of:

loading a library into the apparatus;

activating the x-ray source to produce an x-ray beam traveling along a beampath;

zeroing the stage when the library is in a predetermined position relative to the beampath to establish an reference origin for stage movement;

actuating the stage to move the library to a first position in which a first pre-selected sample of said plurality of samples in the library is aligned with the beampath along which the x-ray beam travels;

exposing the first pre-selected sample of said plurality of samples in the library to the x-ray beam thereby causing the x-ray beam to diffract and form a diffraction pattern characteristic of materials present in the first pre-selected sample;

detecting with the apparatus detector the diffraction pattern resulting from exposure of the first pre-selected sample to the x-ray beam;

recording the diffraction pattern resulting from exposure of the first pre-selected sample to the x-ray beam;

activating the stage to move the library to a second position in which a second pre-selected sample of said plurality of samples in the library is aligned with the beampath along which the x-ray beam travels;

exposing the second pre-selected sample of said plurality of samples in the library to the x-ray beam thereby causing the x-ray beam to diffract and form a diffraction pattern characteristic of materials present in the second pre-selected sample;

detecting with the apparatus detector the diffraction pattern resulting from exposure of the second pre-selected sample to the x-ray beam; and

recording the diffraction pattern resulting from exposure of the second pre-selected sample to the x-ray beam.

11. A method as set forth in claim 10 further comprising the steps of:

processing the diffraction pattern resulting from exposure of the first pre-selected sample to the x-ray beam to determine the materials present in said first pre-selected sample of said plurality of samples in the library; and

processing the diffraction pattern resulting from exposure of the second pre-selected sample to the x-ray beam to determine the materials present in said second pre-selected sample of said plurality of samples in the library.

12. A method as set forth in claim 11 wherein the steps of processing the diffraction pattern resulting from exposure of said first pre-selected sample to the x-ray beam and activating the stage to move the library to the second position occur during overlapping time intervals.

13. A method as set forth in claim 10 wherein the library is in said first position when the stage is zeroed.

14. A method as set forth in claim 10 wherein the apparatus comprises a safety shutter and the method comprises the step of opening the safety shutter.

15. A method as set forth in claim 10 wherein the stage includes a stepper motor and the step of activating the stage to move the library to said second position includes signaling the stepper motor to take a predetermined number of steps.

16. A method as set forth in claim 10 wherein the step of activating the x-ray source occurs before the step of actuating the stage to move the library to the first position.

17. A method as set forth in claim 10 wherein the step of activating the x-ray source occurs before the step of zeroing the stage.

18. A method as set forth in claim 10 further comprising the step of adjusting environmental conditions surrounding the library.

19. Apparatus for characterizing a library containing an array of material members comprising:

an x-ray beam source;

a beamline being adapted to direct, with a predefined beam cross-section, the x-ray beam onto the library;

a chamber adapted to hold the library;

library positioning means adapted to position the library relative to the x-ray beam so as to make each member exposable to the x-ray beam; and

a detector allowing the detection of a photon scattered by one of the members exposed to the x-ray beam in order to generate characterization data for said one member.

20. A method for characterizing a library containing an array of members, comprising the steps of:

adjusting environmental characteristics surrounding the library;

directing an x-ray beam generated by an x-ray source and having a predefined beam cross-section onto the library by means of a beamline;

moving the library by a library positioning means in a predetermined manner to expose a member of the library to the x-ray beam in order to rapidly characterize each member in the library; and

detecting photons scattered by the member in order to characterize the member.