Method for high-throughput micro-sampling analysis of electrochemical process salts

Patent metadata

Field	Value
Publication number	US-10416045-B2
Application number	US-201615237430-A
Country	US
Kind code	B2
Filing date	Aug 15, 2016
Priority date	Aug 14, 2015
Publication date	Sep 17, 2019
Grant date	Sep 17, 2019

Abstract

A method and apparatus for analyzing molten salt electrolyte. The method includes extracting a sample of a molten salt electrolyte from an electrorefiner or other process vessel or conduit; generating droplets from the sample, where the droplets are at a first temperature; transporting the droplets to detectors, where during transport, the droplets attain a second temperature that is lower than the first temperature; analyzing the droplets at or below the second temperature; and returning the droplets to the process. The apparatus includes a droplet generator; a sample transport mechanism; and at least one detector positioned above the sample transport mechanism.

First claim

The embodiment of the invention in which an exclusive property or privilege is claimed is defined as follows:

1. A system for analyzing a molten salt electrolyte comprising:
a) a droplet generator with an aperture surface and a longitudinal axis;
b) a sample transport mechanism comprising:
a substrate having a first surface wherein the first surface opposes the aperture surface, a second surface, and a longitudinal axis extending in a direction substantially perpendicular to the longitudinal axis of the droplet generator;
a plurality of rollers adapted to rotate around their longitudinal axes, wherein the second surface of the substrate is in frictional contact with said rollers, and wherein at least one of said rollers is motorized to cause movement of the substrate in a direction perpendicular to the longitudinal axis of the droplet generator;

c) at least one detector positioned above first surface of the substrate;
d) means to remove droplets generated by the droplet generator from the first surface of the substrate;
e) a heating chamber positioned adjacent to the substrate such that droplets removed from the surface of the substrate are received by said heating chamber; and
f) a first conduit having a first end and a second end wherein the first end is in fluid communication with the heating chamber and the second end is in fluid communication with a process vessel.

2. The system of claim 1 further comprising:
a second conduit having a first end and a second end wherein the first end is in fluid communication with an interior surface of the process vessel and the second end is in fluid communication with the droplet generator;
a first pump coupled to the first conduit intermediate the heating chamber and process vessel; and
a second pump coupled to the second conduit intermediate the process vessel and droplet generator.

3. The system of claim 2 wherein the first pump continuously supplies molten electrolyte salt from the process vessel to the droplet generator.

4. The system as recited in claim 2 wherein the second conduit comprises
a) an upstream region, a mid-stream region defining an aperture and a downstream region, wherein the mid-stream region is positioned between the upstream and the downstream region; and
b) a plurality of fluid passageways defining the downstream region, wherein the passageways have cross section areas that reversibly constrict.

5. The system as recited in claim 4 wherein the upstream region has a cross sectional area that is larger than the cross sectional areas of the passageways combined.

6. The system as recited in claim 4 wherein the constriction of the passageways can be modified in situ.

7. The system of claim 1 wherein the droplet generator generates droplets having a volume between about 1 nL and about 10 mL.

8. The system of claim 1 wherein the at least one detector is a device selected from the group consisting of an alpha particle spectrometer, a beta particle spectrometer, a gamma ray spectrometer, an X-Ray fluorescence analyzer, a laser induced breakdown spectroscopy analyzer and combinations thereof.

9. A system for analyzing a molten salt electrolyte comprising:
a) a droplet generator with an aperture surface and a longitudinal axis;
b) a sample transport mechanism comprising:
a substrate having a first surface wherein the first surface opposes the aperture surface, a second surface, and a longitudinal axis extending in a direction substantially perpendicular to the longitudinal axis of the droplet generator;
a plurality of rollers adapted to rotate around their longitudinal axes, wherein the second surface of the substrate is in frictional contact with said rollers, and wherein at least one of said rollers is motorized to cause movement of the substrate in a direction perpendicular to the longitudinal axis of the droplet generator; and

c) at least one detector positioned above first surface of the substrate, wherein the at least one detector is a device selected from the group consisting of an alpha particle spectrometer, a beta particle spectrometer, a gamma ray spectrometer, an X-Ray fluorescence analyzer, a laser induced breakdown spectroscopy analyzer and combinations thereof.

10. The system of claim 9 further comprising:
means to remove droplets generated by the droplet generator from the first surface of the substrate;
a heating chamber positioned adjacent to the substrate such that droplets removed from the surface of the substrate are received by said heating chamber; and
a first conduit having a first end and a second end wherein the first end is in fluid communication with the heating chamber and the second end is in fluid communication with a process vessel.

11. The system of claim 10 further comprising:
a second conduit having a first end and a second end wherein the first end is in fluid communication with an interior surface of the process vessel and the second end is in fluid communication with the droplet generator;
a first pump coupled to the first conduit intermediate the heating chamber and process vessel; and
a second pump coupled to the second conduit intermediate the process vessel and droplet generator.

12. The system of claim 11 wherein the first pump continuously supplies molten electrolyte salt from the process vessel to the droplet generator.

13. The system as recited in claim 11 wherein the second conduit comprises
a) an upstream region, a mid-stream region defining an aperture and a downstream region, wherein the mid-stream region is positioned between the upstream and the downstream region; and
b) a plurality of fluid passageways defining the downstream region, wherein the passageways have cross section areas that reversibly constrict.

14. The system as recited in claim 13 wherein the upstream region has a cross sectional area that is larger than the cross sectional areas of the passageways combined.

15. The system as recited in claim 13 wherein the constriction of the passageways can be modified in situ.

16. The system of claim 9 wherein the droplet generator generates droplets having a volume between about 1 nL and about 10 mL.

17. A system for analyzing a molten salt electrolyte comprising:
a) a droplet generator with an aperture surface and a longitudinal axis;
b) a sample transport mechanism comprising:
a substrate having a first surface wherein the first surface opposes the aperture surface, a second surface, and a longitudinal axis extending in a direction substantially perpendicular to the longitudinal axis of the droplet generator;
a plurality of rollers adapted to rotate around their longitudinal axes, wherein the second surface of the substrate is in frictional contact with said rollers, and wherein at least one of said rollers is motorized to cause movement of the substrate in a direction perpendicular to the longitudinal axis of the droplet generator;

c) at least one detector positioned above first surface of the substrate;
d) means to remove droplets generated by the droplet generator from the first surface of the substrate;
e) a heating chamber positioned adjacent to the substrate such that droplets removed from the surface of the substrate are received by said heating chamber;
f) a first conduit having a first end and a second end wherein the first end is in fluid communication with the heating chamber and the second end is in fluid communication with a process vessel;
g) a second conduit having a first end and a second end wherein the first end is in fluid communication with an interior surface of the process vesse

Assignees

• Launiere Cari A
• Pereira Candido
• Bailey James L
• Wiedmeyer Stanley G
• Uchicago Argonne Llc

Inventors

• Launiere Cari A
• Pereira Candido
• Bailey James L
• Wiedmeyer Stanley G

Classifications

• G01N23/223

  by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence · CPC title

• G01N33/20

  Metals · CPC title

• G01N1/125 Primary

  adapted for sampling molten metals · CPC title

• C25C7/06

  Operating or servicing · CPC title

• C25C3/34

  of metals not provided for in groups C25C3/02 - C25C3/32 · CPC title