Quantitative nuclear magnetic resonance for additives determination in an electrolytic nickel bath |
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Authors: | Ostra Miren Ubide Carlos Vidal Maider |
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Institution: | (1) Departamento de Qu?mica Aplicada, Facultad de Qu?mica, Universidad del Pa?s Vasco, Apdo. 1072, San Sebasti?n, 20080, Spain; |
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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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