Abstract
The use of proton nuclear magnetic resonance (1H-NMR) for the quantitation of additives in a commercial electrolytic nickel bath (Supreme Plus Brilliant, Atotech formulation) is reported. A simple and quick method is described that needs only the separation of nickel ions by precipitation with NaOH. The four additives in the bath (A-5(2X), leveler; Supreme Plus Brightener (SPB); SA-1, leveler; NPA, wetting agent; all of them are commercial names from Atotech) can be quantified, whereas no other analytical methods have been found in the literature for SA-1 and NPA. Two calibration methods have been tried: integration of NMR signals with the use of a proper internal standard and partial least squares regression applied to the characteristic NMR peaks. The multivariate method was preferred because of accuracy and precision. Multivariate limits of detection of about 4 mL L−1 A-5(2X), 0.4 mL L−1 SPB, 0.2 mL L−1 SA-1 and 0.6 mL L−1 NPA were found. The dynamic ranges are suitable to follow the concentration of additives in the bath along electrodeposition. 1H-NMR spectra provide evidence for SPB and SA-1 consumption (A-5(2X) and NPA keep unchanged along the process) and the growth of some products from SA-1 degradation can be followed. The method can, probably, be extended to other electrolytic nickel baths.
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Acknowledgements
Financial support from MICINN (CTQ2008—06751-C02-02/BQU) and from UPV/EHU (Project GIU07/58) is here acknowledged. M. V. acknowledges financial support from GV in the form of a scholar fellowship. The authors thank Dr. José I. Miranda (Servicio de RMN, Universidad del País Vasco) for help during the NMR measurements and Francesco Savorani (Faculty of Live Sciences, University of Copenhagen) for NMR peaks alignment by icoshifth algorithm.
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Ostra, M., Ubide, C. & Vidal, M. Quantitative nuclear magnetic resonance for additives determination in an electrolytic nickel bath. Anal Bioanal Chem 399, 1907–1915 (2011). https://doi.org/10.1007/s00216-010-4573-z
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DOI: https://doi.org/10.1007/s00216-010-4573-z