TITLE

Determination of additives in an electrolytic zinc bath by qH-NMR spectroscopy

AUTHOR(S)
Barriola, Ainara; Miranda, José I.; Ostra, Miren; Ubide, Carlos
PUB. DATE
September 2010
SOURCE
Analytical & Bioanalytical Chemistry;Sep2010, Vol. 398 Issue 2, p1085
SOURCE TYPE
Academic Journal
DOC. TYPE
Article
ABSTRACT
The use of proton nuclear magnetic resonance (H-NMR) for the quantification of additives in an electrolytic Zn bath is reported. A simple and quick method is described that does not need any prior sample preparation. Contrary to other analytical methods, the three additives in the bath, benzylidene acetone (BDA), benzoic acid (BA) and poly(ethylene glycol) (PE400), can be quantified. Two calibration methods were tried: integration of NMR signals with the use of an internal standard and partial least squares (PLS) regression applied to the characteristic NMR peaks. Both methods are compared and the univariate method was preferred because of simplicity, accuracy and precision. The following limits of detection were found: 0.30 g L BA, 0.08 g L BDA and 0.7 g L PE400 with dynamic ranges of at least 1.0–6.0, 0.1–0.6 and 3.0–18.0 g L respectively. Those concentration ranges are suitable to follow the concentration of additives in the bath in real time. H-NMR spectra provide evidence for the BDA degradation pattern. [Figure not available: see fulltext.]
ACCESSION #
53556221

 

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