Adaptation device for adapting an UV-Vis cuvette to perform In-situ spectroanalytical measurements in a controlled atmosphere

Patent metadata

Field	Value
Publication number	US-10955351-B2
Application number	US-201615751457-A
Country	US
Kind code	B2
Filing date	Jul 28, 2016
Priority date	Aug 11, 2015
Publication date	Mar 23, 2021
Grant date	Mar 23, 2021

Abstract

An adaptation device is provided for adapting an UV-Vis cuvette to perform in-situ spectroanalytical characterization of redox processes using gas species or solutes in a controlled atmosphere, the device configured to fit the open end of a UV-Vis cuvette intended to contain products to be measured during achievement of spectroanalytical measurements. The device comprises a main body configured to form a lid covering the opened end of the cuvette, the main body having a first part and a second part; a working, a counter and a reference electrode with removable parts at the respective ends of three conductors coming from outside and passing through the main body; a gas inlet to allow introduction of a gas the gas inlet having one aperture directed to the working electrode and second aperture directed to the bottom of the cuvette, a gas outlet intended to let the reactive gas in excess to flow out of the cuvette and an solution inlet tube for titration measurements.

First claim

The invention claimed is:

1. An adaptation device for adapting an UV-Vis or Raman cuvette to perform in-situ spectroanalytical characterization of redox processes using gas species or titrated redox active species in a controlled atmosphere, said device being configured so as to fit an open end of a UV-Vis or Raman cuvette intended to contain products to be measured during achievement of spectroanalytical measurements, wherein the device comprises:
a main body configured to form a plug closing the opened end of the cuvette;
a working electrode a counter electrode and a reference electrode with removable parts mounted removably at respective ends of conductors passing through the main body;
a gas inlet tube passing through the main body which terminates in a cavity of the cuvette so as to be partially immersed in a solution contained in the cuvette, said gas inlet tube being intended to allow introduction of a reactive gas in the solution;
a gas outlet tube passing through the main body which terminates in the cavity of the cuvette in an emerged part of the cavity, said gas outlet tube being intended to let the gas in excess to flow out of the cuvette;
the gas inlet tube being configured to have a double opened termination at its end located inside the cavity of the cuvette, a first upper termination directed towards the working electrode and a second lower termination directed towards the bottom of the cuvette, said second termination being arranged at a distance from the bottom of the cuvette such that gas bubbles do not reach a lower part of the cavity in which UV-Vis or Raman measurements are performed.

2. The adaptation device according to claim 1 , wherein the main body having a first part and a second part the first part being intended to make it possible to remove the device from the cuvette easily; the second part being intended to be introduced in the cuvette and having an external size substantially equal to the size of the opened end of the cuvette.

3. The adaptation device according to claim 1 , wherein the main body is made of a material thermally stable and chemically inert.

4. The adaptation device according to claim 3 , wherein the main body is made of Polytetrafluoroethylene, Polyetheretherketon or Polypropylene.

5. The adaptation device of claim 4 , wherein the sealing ring is made of Polytetrafluoroethylene.

6. The adaptation device according to claim 1 , further comprising a sealing ring arranged at the periphery of the second part of the main body intended to be introduced in the opened end of the cuvette.

7. The adaptation device according to claim 1 , further comprising a solution inlet aperture configured to be closed when it is not in use during measurement process.

8. The adaptation device according to claim 1 , wherein a length of the gas inlet tube inside the cuvette is sized in such a way that a first aperture be arranged along the length of the gas inlet so as to be located close to the working electrode whereas a second aperture is located relative to the bottom of the cuvette so as to stir the solution in the whole volume of the cuvette, by bubbling, without affecting a spectrochemical measurement.

9. The adaptation device according to claim 1 , wherein the ends of the gas inlet tube and of the gas outlet tube located outside the cuvette are fitted with shutoff valves in order to allow a complete insulation from open air of the solution contained in the cuvette.

10. The adaptation device according to claim 1 wherein the material of the working electrode and of the counter electrode is chosen such that it promotes an electrochemical active surface towards the precursor species, being gases or solutes.

11. The adaptation device according to claim 10 , wherein the working electrode and the counter electrode are made of gold, platinum or of carbon.

12. The adaptation device according to claim 1 , wherein the reference electrode is made of silver or of platinum.

13. A method for performing an UV-Vis or Raman measurement with a measuring instrument using a standard cuvette and an adaptation device according to claim 1 , comprising:
introducing an empty cuvette inside an enclosure containing inert atmosphere,
filling up the cuvette with the solution to be measured,
fitting the adaptation device to a opened end of the cuvette so as to seal said opened end,
removing the cuvette from the enclosure, and placing the cuvette in an appropriate housing of the measuring instrument.

14. The method of claim 13 further comprising:
connecting the gas inlet to a gas pipe;
connecting the working electrode, the counter electrode and the reference electrode to the corresponding outlets of a workstation of the measuring instrument;
applying an operating voltage or current between the working electrode and the reference electrode,
opening a shutoff valve of said gas inlet to let oxidation gas flowing in the cuvette.

Assignees

• Centre Nat Rech Scient

Inventors

• Lutz Lukas
• Alves Dalla Corte Daniel
• Grimaud Alexis
• Tarascon Jean-Marie

Classifications

• G01N21/05

  Flow-through cuvettes (G01N21/09 takes precedence; handling fluid samples G01N1/10) · CPC title

• G01J3/44

  Raman spectrometry; Scattering spectrometry {; Fluorescence spectrometry} · CPC title

• C08L23/12

  Polypropene · CPC title

• C08L61/16

  of ketones with phenols · CPC title

• G01N2021/0325

  Cells for testing reactions, e.g. containing reagents · CPC title