IP Library Granted Patent US 10,422,778
Granted Patent B2
US 10,422,778 · App. 15/537,592 · Granted Sep 24, 2019

Method for determining dimethyl disulphide

Inventors: Harald Jakob (Hasselroth, DE); Benjamin Fonfe (Frankfurt, DE); Sebastian Fuss (Flieden, DE); Andreas Doerflein (Grosskrotzenburg, DE); Markus Held (Limeshain, DE); Nadine Duerr (Alsbach, DE)
Assignee: Evonik Degussa GmbH
G01N30/88G01N27/49G01N2030/645G01N2030/884
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Quick Facts
Patent No.
US 10,422,778
App. No.
15/537,592
Granted
Sep 24, 2019
Kind
B2
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.

Claims (19)

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.

Assignments (2)
CHANGE OF NAME Recorded Jan 31, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051765/0166 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 19, 2017
From: JAKOB, HARALD; FORTE, BENJAMIN; FUSS, SEBASTIAN; DOERFLEIN, ANDREAS; HELD, MARKUS; DUERR, NADINE
To: EVONIK DEGUSSA GMBH
Reel/Frame 042747/0425 →
Priority Claims (1)
EP 14199254 · Dec 19, 2014 · regional
Continuity (1)
Related Publication 20180267002A1 · Sep 20, 2018