XRD sample handling apparatus

Patent metadata

Field	Value
Publication number	US-9683950-B2
Application number	US-201514877995-A
Country	US
Kind code	B2
Filing date	Oct 8, 2015
Priority date	Oct 31, 2014
Publication date	Jun 20, 2017
Grant date	Jun 20, 2017

Abstract

Disclosed is a sample handling assembly facilitating a sample holding cell used for XRD analysis. The assembly holds the sample cell upright during sample loading and analysis phases. The sample handling assembly is vibrated, partly by a tuning fork, to allow the powder to flow into the sample cell. After the XRD analysis, a rotating arm holding the sample cell is rotated 180° to orient the sample cell completely upside down so that the sample can be emptied. Also disclosed are jets of air that are pulsed onto the sample cell, and/or into the sample cell funnel-tube assembly, to shake and clean the components.

First claim

What is claimed is:

1. A sample handling assembly configured to hold at least one sample cell for undergoing an X-ray Diffraction (XRD) analysis operation on a sample in the form of powder or grains contained in the sample cell during the analysis operation, the operation including a sample feeding phase, analysis phase and sample removing phase,
the assembly comprises,
at least one sample cell having a sample cell opening and a sample cell window,
a sample transfer funnel configured to be on top of the sample cell opening and to guide and transport the sample into the sample cell via the sample cell opening during the sample feeding phase,
a tuning fork base, a tuning fork sample arm to which the sample cell is attached, a tuning fork balancing arm, and a tuning fork actuator, wherein the tuning fork sample arm and the balancing arm are both attached to the fork base,
a rotating arm to which the tuning fork base is attached,
wherein the rotating arm is in a first position causing the cell opening to be facing upward during the feeding and the analysis phases, and rotates upside down to a second position causing the cell opening to be facing downward to allow sample flow out from the sample cell onto a sample tray during the sample removing phase.

2. The sample handling assembly of claim 1 , wherein the tuning fork actuator is configured to cause the tuning fork sample arm and the balancing arm to vibrate, thereby causing the sample cell to vibrate to generate convection in the sample during the analysis phase.

3. The sample handling assembly of claim 1 , wherein the tuning fork actuator is configured to cause the tuning fork sample arm to vibrate, thereby causing the sample cell to vibrate to shake down the sample during the removing phase.

4. The sample handling assembly of claim 1 further comprising a rotating shaft around which the rotating arm and consequently the sample cell are rotated 180 degrees between the feeding and analysis phase and the removing phase.

5. The sample handling assembly of claim 1 , wherein the actuator is attached to, and sandwiched between the fork sample arm and the balancing arm.

6. The sample handling assembly of claim 1 further comprising a sample loading funnel and a filling tube, the filling tube having a higher end attached to a sample loading funnel and a lower end.

7. The sample handling assembly of claim 6 wherein the lower end of the filling tube is positioned right above, yet detached from the sample transfer funnel during the sample feeding and analysis phases.

8. The sample handling assembly of claim 6 further comprising a shaking means configured to shake the filling tube and the loading funnel to assist the sample motion down the filling tube.

9. The sample handling assembly of claim 8 , wherein the shaking means is a non-concentric shaker including a stator and a non-concentric rotor.

10. The sample handling assembly of claim 8 , wherein the shaking means is a thwacker device including a rotor and a thwacker arm.

11. The sample handling assembly of claim 1 further comprising an air suction means to remove the sample from the sample tray.

12. The sample handling assembly of claim 1 further comprising a first air bursting means to burst air into the sample transfer funnel and consequently into the sample cell during the removing phase.

13. The sample handling assembly of claim 1 further comprising a second air bursting means to burst air onto the sample cell window during the removing phase.

14. The sample handling assembly of claim 1 further comprising a computerized controller module configured to control and actuate at least one of the following:
a) the tuning fork actuator,
b) the rotating arm between the first and the second positions.

15. A method of facilitating at least one sample cell for undergoing an X-ray Diffraction (XRD) analysis operation on a sample in the form of powder or grains and contained in the sample cell during the analysis operation, the operation including a sample feeding phase, analysis phase and sample removing phase, the at least one sample cell is attached to a prong of a tuning fork,
the method comprises the steps of,
holding the at least one sample cell in an upright position, with a sample cell opening open and facing upward to receive the sample during the sample feeding phase,
actuating the tuning fork to cause vibration of the sample cell,
feeding the sample via a sample transfer funnel configured to guide the sample into the sample cell via the sample cell opening while the tuning fork is in vibration,
performing XRD analysis on the sample, keeping the tuning fork in vibration,
rotating the sample cell upside-down so that the sample cell opening is facing downward in the direction of gravity,
allowing the sample to fall down during the sample removing phase, keeping the tuning fork in vibration,
returning the sample cell back to the upright position for another cycle of analysis operation.

16. The method of claim 15 wherein the step of actuating the tuning fork is done by an actuator which is attached to, and sandwiched between a fork sample arm and a balancing arm of the tuning fork.

17. The method of claim 15 further including the steps of,
a) filling the sample into a sample loading funnel,
b) allowing the sample to move down through a filling tube by a shaking means, and
c) transferring the sample into the sample transfer funnel.

18. An X-ray Diffraction (XRD) device comprising an X-ray source, an X-ray detector and a data processor and analyzer and at least one sample cell to be exposed to the X-ray source,
the XRD device further comprises,
a sample handling assembly configured to hold at least one sample cell for an XRD analysis operation on a sample in the form of powder or grains contained in the sample cell during the analysis operation, the operation including a sample feeding phase, analysis phase and sample removing phase,
the assembly comprises,
a sample transfer funnel configured to be on top of a sample cell opening and to guide and transport the sample into the sample cell via the sample cell opening during the sample feeding phase,
a tuning fork base, a tuning fork sample arm to which the sample cell is attached, a tuning fork balancing arm, and a tuning fork actuator, wherein the tuning fork sample arm and the balancing arm are both attached to the fork base,
a rotating arm to which the tuning fork base is attached,
wherein the rotating arm is in a first position causing the sample cell opening to be facing upward during the feeding and the analysis phases, and rotates upside down to a second position causing the cell opening to be facing downward to allow sample flow out from the sample cell during the sample removing phase.

Assignees

• Sarrazin Philippe Christian
• Baensch Aaron Troy
• Brunner Will M
• Olympus Scient Solutions Americas Inc

Inventors

• Sarrazin Philippe Christian
• Baensch Aaron Troy
• Brunner Will M

Classifications

• G01N2223/056

  diffraction · CPC title

• G01N23/207

  Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions · CPC title

• G01N23/20025 Primary

  Sample holders or supports therefor · CPC title