Electrochemical detector system

• US 4,059,406 A
• Filed: 07/12/1976
• Issued: 11/22/1977
• Est. Priority Date: 07/12/1976
• Status: Expired due to Term

• Current Assignee: E D T Supplies Limited
• Original Assignee: E D T Supplies Limited
• Inventors: Fleet, Bernard
• Primary Examiner(s): Serwin, R.E.
• Application Number:
  US05/704,299
• Time in Patent Office: 498 Days
• Field of Search: 23/230 R, 23/253 R, 23/232 E, 23/254 E, 73/23.1, 73/61.1 C, 204/195 R
• US Class Current: 205/786
• CPC Class Codes: G01N 27/28 Electrolytic cell components
• CPC Class Codes: G01N 27/38 Cleaning of electrodes
• CPC Class Codes: G01N 27/42 Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
• CPC Class Codes: G01N 30/64 Electrical detectors

Abstract

An electrochemical detector has an electrochemical thin-layer flow cell whose operation is based on the so-called wall-jet principle, in combination with a controller unit. The controller unit can apply a periodically changing voltage having a square wave voltage formation to a sensor electrode of the electrochemical cell such that a first potential level of the square wave functions as a detecting potential and a second potential level of the square wave functions as a cleaning potential.

Claims

1. A method for detecting an electroactive species in a flow stream comprising the steps of:

i. forcing a solution containing the electroactive species through a fine nozzle to form a jet,

ii. impringing the jet normally to a surface of a sensor electrode so that the solution spreads radially over the surface in a thin film,

iii. applying a periodically changing voltage to the sensor electrode, so that one part of each cycle of the applied voltage functions as a detecting potential and another part of each cycle functions as a cleaning potential, and

iv. measuring a current at the sensor electrode during that part of each cycle of the applied voltage functioning as a detecting potential.

2. A method for detecting an electroactive species as claimed in claim 1 comprising the further step of:

v. recording the current measured at the sensor electrode.

3. A method for detecting an electroactive species as claimed in claim 1 which consists of applying a square wave voltage to the sensor electrode, a first level of each cycle of the applied square wave functioning as a detecting potential and a second level of each cycle functioning as a cleaning potential.

4. In an electrochemical detector having an electrochemical thin-layer flow cell adapted to operate on the wall-jet principle comprising a solution inlet line terminating in a fine nozzle, a sensor electrode, at least one solution exit line, and at least one other electrode, the improvement comprising means for applying a periodically changing voltage to the sensor electrode so that a first part of each cycle of the applied voltage functions as a detecting potential and a second part of each cycle of the applied voltage functions as a cleaning potential.

5. The improvement claimed in claim 4 wherein the periodically changing voltage applied to the sensor electrode is a square wave voltage.

6. The improvement claimed in claim 5 wherein a first level of each square wave cycle functions as a detecting potential and a second level of each square wave cycle functions as a cleaning potential.

7. The improvement claimed in claim 6 wherein a current is measured for a short period towards the end of each level which functions as a detecting potential.

8. The improvement claimed in claim 7 wherein the short period is equal to the time required for one cycle of mains voltage.

9. The improvement claimed in claim 5 comprising means for altering the amplitude of the square wave voltage.

10. The improvement claimed in claim 6 comprising means for altering the frequency of the square wave voltage and the length of the said first and second level independently of each other.

11. An electrochemical detector having an electrochemical thin-layer flow cell adapted to operate on the wall-jet principle comprising a sensor electrode, a solution inlet line terminating in a fine nozzle, the said nozzle being located normally to but displaced from a surface of the sensor electrode, at least one solution exit line, at least one other electrode and means comprising a controller unit for applying a periodically changing voltage to the sensor electrode so that one part of each cycle of the applied voltage functions as a detecting potential and another part of each cycle of the applied voltage functions as a cleaning potential.

12. An electrochemical detector as claimed in claim 11 comprising means for altering the distance between the fine nozzle and the surface of the sensor electrode.

13. An electrochemical detector as claimed in claim 11 wherein the said electrochemical cell has an effective cell volume in the range from less than 1 μ

l (10^-6 l) to 100 μ

l (10^-6 l).

14. An electrochemical detector as claimed in claim 11 wherein the sensor electrode surface is planar and the sensor electrode is disc-shaped.

15. An electrochemical detector as claimed in claim 11 wherein the sensor electrode is in ring form.

16. An electrochemical detector as claimed in claim 11 wherein the sensor electrode consists of high density vitreous carbon.

17. An electrochemical detector as claimed in claim 11 wherein the electrochemical thin-layer flow cell has one solution exit line, a reference electrode and a counter electrode.

18. An electrochemical detector as claimed in claim 11 in combination with a high performance, high pressure liquid chromatography column having duct means for an effluent from the said column to enter the solution inlet line of the said electrochemical cell.