Galvanic process with analysis of the electrolytic bath through solid phase extraction

• Main Authors: RUETHER, ROBERT, GAIDA, JOSEF, BARTHELMES, JUERGEN, SAINZ-VILA, MARTA, MORITZ, THOMAS, LAGORCE-BROC, FLORENCE, SPRENGER, OLEG, KURTZ, OLAF
• Format: Patent
• Language: English; French; German
• Published: 18.06.2008
• Subjects: APPARATUS THEREFOR; CHEMISTRY; ELECTROFORMING; ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; METALLURGY; PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTIONOF COATINGS

The method for the galvanic deposition of a metal coating from an electrolyte bath, in which the concentrations of two components of the electrolyte bath are monitored, comprises removing a sample from the electrolyte bath, feeding the sample to a column for solid phase extraction, subjecting the column to a washing process with a first eluent, eluting the two components from the column by a second eluent, and determining the concentrations of the components in the obtained eluate by photometry, polarography and refractometry without separating the components from each other. The method for the galvanic deposition of a metal coating from an electrolyte bath, in which the concentrations of two components of the electrolyte bath are monitored, comprises removing a sample from the electrolyte bath, feeding the sample to a column for solid phase extraction, which contains a solid sorption agent, subjecting the column to a washing process with a first eluent, where the two components remain in the column and unwanted components are eluted from the column, eluting the two components from the column by a second eluent, and determining the concentrations of the two components in the obtained eluate by photometry, polarography and refractometry without separating the components from each other. The supply of the eluents to the column takes place in the same or opposite direction for the supply of the sample. The process takes place in a sequence at a regular time intervals of 1 minute to 10 hours. The monitoring of the concentration of the two components in combination is carried out with a dosing system, which supplies an appropriate fresh quantity of the component depending upon the result of the concentration regulation. Before feeding the sample, the column is conditioned with methanol or an acid solution and then equilibrated with water. Es wird ein Verfahren zur galvanischen Abscheidung einer Metallschicht aus einem Elektrolytbad beschrieben, wobei die Konzentrationen mindestens zweier Komponenten des Elektrolytbads überwacht werden, indem folgende Schritte durchgeführt werden: (a) dem Elektrolytbad wird eine Probe entnommen; (b) die Probe wird einer Säule zur Festphasenextraktion zugeführt, die ein festes Sorbens enthält; (c) die Säule wird einem Waschvorgang mit einem ersten Eluens unterworfen, wobei die mindestens zwei Komponenten auf der Säule verbleiben und unerwünschte Komponenten von der Säule eluiert werden; (d) die mindestens zwei Komponenten werden von der Säule mittels eines zweiten Eluens eluiert; (e) die Konzentrationen der mindestens zwei Komponenten in dem in Stufe (d) erhaltenen Eluat werden bestimmt, ohne dass die Komponenten voneinander getrennt werden. Dabei ist die Verwendung von Poly(divenylbenzol-co-N-vinylpyrrolidon) zur Festphasenextraktion besonders vorteilhaft.