Voltammetric apparatus and method

• US 4,083,754 A
• Filed: 04/26/1976
• Issued: 04/11/1978
• Est. Priority Date: 04/28/1975
• Status: Expired due to Term

• Current Assignee: Mitsubishi Kasei Corp. (Mitsubishi Chemical Group Corp.)
• Original Assignee: Mitsubishi Kasei Kogyo Kabushiki Kaisha
• Inventors: Tanaka, Yutaka, Outsuka, Koremitsu, Kawasaki, Kazuyoshi
• Primary Examiner(s): Tung, T.
• Application Number:
  US05/679,972
• Time in Patent Office: 715 Days
• Field of Search: 204/1 T, 204/195 R, 204/195 H
• US Class Current: 205/775
• 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 27/48 using polarography, i.e. measuring changes in current under a slowly-varying voltage

Abstract

In apparatus for use in differential pulse anodic stripping voltammetry the period of the pulse voltage is selected to be in a range of from 16.7 to 400 milliseconds for the purpose of analyzing an extremely small quantity of metal ions at high speeds and at high sensitivities.

Claims

1. A method of differential pulse anodic stripping voltammetry comprising the steps of

filling a solution containing ions of a metal to be analyzed into an electrolytic cell having a working electrode and a counter electrode,

applying a plating voltage across the counter electrode and the working electrode to plate the same with the metal,

applying across the counter electrode and the working electrode a DC stripping voltage having superimposed thereon a pulse voltage having a repetition period of 16.7 to 400 milliseconds in order to strip the metal that has been plated on the working electrode by the plating voltage,

measuring a first sampling current which flows through the working electrode during a predetermined interval in which the pulse voltage is not applied,

measuring a second sampling current which flows through the working electrode while the pulse voltage is applied, and

determining the difference between the first and second sampling currents.

2. The method according to claim 1 wherein the repetition period of the pulse voltage is 33.4 to 200 milliseconds.

3. The method according to claim 1 wherein the duration of the pulse voltage is 8.3 to 100 milliseconds.

4. The method according to claim 1 wherein the stripping voltage is swept at a speed of 10 to 90 millivolts/sec.

5. The method according to claim 4 wherein the sweeping speed ranges from 20 to 60 millivolts/sec.

6. The method according to claim 1 wherein the first sampling current is measured in an interval immediately prior to each pulse voltage.

7. The method according to claim 1 wherein the second sampling current is measured during a predetermined interval of the latter half of each pulse voltage.

8. Differential pulse anodic stripping voltametry comprising:

an electrolytic cell having a working electrode and a counter electrode;

a source of plating voltage, a source of sweeping voltage and a source of pulse voltage having a repetition period of 16.7 to 400 milliseconds for impressing plating voltage, stripping voltage and pulse voltage respectively across the working electrode and the counter electrode;

a current-voltage converter for converting the current flowing through the working electrode into voltage for producing two sample voltages;

voltage holding means for holding the two sample voltages; and

a differential amplifier for amplifying the difference between the two sample voltages held by the voltage holding means.

9. The apparatus according to claim 8 wherein the period of the pulse voltage is 33.4 to 200 milliseconds.

10. The apparatus according to claim 8 wherein the duration of the pulse voltage is 8.3 to 100 milliseconds.

11. The apparatus according to claim 8 wherein the stripping voltage has a sweeping speed of 1 to 90 millivolts/sec.

12. The apparatus according to claim 11 wherein the sweeping speed is 20 to 60 millivolts/sec.