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

Patent metadata

Field	Value
Publication number	US-2017045423-A1
Application number	US-201615237430-A
Country	US
Kind code	A1
Filing date	Aug 15, 2016
Priority date	Aug 14, 2015
Publication date	Feb 16, 2017
Grant date	—

Abstract

Briefly, the invention provides a method for analyzing molten salt electrolyte involving 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. Also provided is a system for analyzing molten salt electrolyte using a droplet generator.

First claim

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

1 . A method for analyzing a process fluid, said method comprising the steps of:
a) extracting fluid from a process stream; b) generating droplets from the extracted fluid, wherein the droplets are at a first temperature; c) transporting the droplets to detectors, wherein during transport, the droplets attain a second temperature that is lower than the first temperature; d) analyzing the droplets at or below the second temperature; and e) returning the droplets to the stream.

2 . The method of claim 1 wherein the step of generating the droplets comprises directing the extracted fluid to a droplet generator comprising:
a first molten salt reservoir and a second molten salt reservoir, where the first molten salt reservoir is positioned above the second molt salt reservoir;
a first molten salt conduit providing fluid communication between the first reservoir and the second reservoir, wherein the first conduit defines an upstream region having a first cross sectional area and a downstream region having a second cross sectional area which is reversibly constricted.
a midstream region of the conduit forming an aperture such that the aperture resides between the upstream region and the downstream region of the first conduit;
and a means of molten salt egress from a depending end of the downstream region of the first molten salt conduit, said egress means positioned between the depending end of the conduit and the second molten salt reservoir.

3 . The method as recited in claim 2 wherein the first molten salt conduit downstream cross sectional area is reversibly constricted.

4 . The method as recited in claim 1 wherein the step of generating droplets comprises subjecting the extracted fluid to a flow cell having an upstream region defining a single fluid conduit and a downstream region defining a plurality of fluid conduits.

5 . The method of claim 1 wherein the droplet generator comprises a second molten salt conduit downstream of the first molten salt conduit and establishing reversible fluid communication between a second reservoir and a first reservoir.

6 . The method of claim 1 wherein the step of generating the droplets comprises channeling the molten salt through a conduit having a first cross section defining an orifice and a second section downstream from the orifice, wherein a feedstock of the process fluid is positioned above the orifice and wherein a portion of the conduit downstream of the orifice has a second cross section that is smaller than the first cross section.

7 . The method of claim 1 wherein each of the droplets has a volume between 1 nL and 10 mL.

8 . The method of claim 1 wherein the detectors operate at ambient temperature.

9 . The method of claim 1 further comprising reheating the droplets before returning the droplets to the process stream.

10 . The method of claim 1 wherein the extracting step further comprises continuously pumping a stream of molten salt electrolyte from the feedstock.

11 . The method of claim 1 wherein between about 10 drops and about 5000 drops are analyzed per hour.

12 . A system for analyzing molten salt electrolyte comprising:
a droplet generator with an aperture surface and a longitudinal axis; 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
at least one detector having a longitudinal axis positioned above or below the first surface of the substrate such that the longitudinal axis of the at least one detector is substantially parallel to the longitudinal axis of the droplet generator.

13 . The system of claim 12 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.

14 . The system of claim 13 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.

15 . The system of claim 14 wherein the first pump continuously supplies molten electrolyte salt from the process vessel to the droplet generator.

16 . The system of claim 12 wherein the droplet generator generates droplets having a volume between about 1 nL and about 10 mL.

17 . The system of claim 12 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.

18 . The system as recited in claim 14 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.

19 . The system as recited in claim 18 wherein the upstream region has a cross sectional area that is larger than the cross sectional areas of the passageways combined.

20 . The system as recited in claim 18 wherein the constriction can be modified in situ.

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

• C25C3/34

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

• C25C7/06

  Operating or servicing · CPC title

• G01N1/125 Primary

  adapted for sampling molten metals · CPC title