Method for determining dimethyl disulphide

Patent metadata

Field	Value
Publication number	US-10422778-B2
Application number	US-201515537592-A
Country	US
Kind code	B2
Filing date	Dec 17, 2015
Priority date	Dec 19, 2014
Publication date	Sep 24, 2019
Grant date	Sep 24, 2019

Abstract

A method for determining dimethyl disulphide proceeds by carrying out a chromatographic separation of an analyte containing at least dimethyl disulphide and methanesulphonic acid, and determining the dimethyl disulphide by pulsed amperometric detection.

First claim

The invention claimed is:

1. A method for determining dimethyl disulphide, the method comprising:
a) carrying out a chromatographic separation of an analyte comprising at least dimethyl disulphide and methanesulphonic acid; and
b) determining the dimethyl disulphide by pulsed amperometric detection,
wherein a glassy carbon electrode is used as a working electrode in the pulsed amperometric detection.

2. The method according to claim 1 , wherein the determining of the dimethyl disulphide by the pulsed amperometric detection further comprises:
b1) measuring an electrolysis current for the dimethyl disulphide by the pulsed amperometric detection; and
b2) determining an amount of the dimethyl disulphide, a concentration of the dimethyl disulphide, or both, by comparison with a calibration function previously generated for the dimethyl disulphide.

3. The method according to claim 1 , wherein the pulsed amperometric detection is carried out in an oxidative mode.

4. The method according to claim 1 , wherein a silver-silver chloride electrode or a palladium electrode is used as a reference electrode in the pulsed amperometric detection.

5. The method according to claim 1 , wherein the pulsed amperometric detection includes at least three potential profiles.

6. The method according to claim 5 , wherein the pulsed amperometric detection comprises at least one oxidation potential, at least one cleaning potential and at least one conditioning potential.

7. The method according to claim 6 , wherein the oxidation potential has a value of approximately +0.5V to approximately +1.3V, the cleaning potential has a value of at least approximately +1.3V, and the conditioning potential has a value of approximately −0.5V to approximately +0.5V.

8. The method according to claim 6 , wherein the oxidation potential has a value of approximately +0.8V to approximately +1.2V, the cleaning potential has a value of at least approximately +1.5V, and the conditioning potential has a value of approximately 0.3V to approximately +0.3V.

9. The method according to claim 6 , wherein a duration of the oxidation potential is at least approximately 60 ms, a duration of the cleaning potential is at least approximately 10 ms, and a duration of the conditioning potential is at least approximately 40 ms.

10. The method according to claim 9 , wherein the duration of the oxidation potential is at least approximately 300 ms.

11. The method according to claim 2 , wherein a measurement duration of the pulsed amperometric detection is an integer multiple of 16.7 ms.

12. The method according to claim 1 , wherein the chromatographic separation is performed by reversed phase chromatography.

13. The method according to claim 12 , wherein the chromatographic separation is performed by ion chromatography.

14. The method according to claim 1 , wherein the analyte is provided, by dissolving a sample comprising the dimethyl disulphide and the methanesulphonic acid in a protic solvent or in a mixture of protic solvents.

Assignees

• Evonik Degussa Gmbh

Inventors

• Jakob Harald
• Fonfe Benjamin
• Fuss Sebastian
• Doerflein Andreas
• Held Markus
• Duerr Nadine

Classifications

• G01N30/88 Primary

  Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 · CPC title

• G01N2030/645

  electrical conductivity detectors · CPC title

• G01N30/64

  Electrical detectors · CPC title

• G01N27/49

  Systems involving the determination of the current at a single specific value, or small range of values, of applied voltage for producing selective measurement of one or more particular ionic species · CPC title

• G01N2030/884

  organic compounds · CPC title