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Solid phase microextraction method for characterizing the organic fraction of an industrial brine stream

Title
Solid phase microextraction method for characterizing the organic fraction of an industrial brine stream
Type
Article in International Scientific Journal
Year
2013
Authors
João F. B. Lima
(Author)
FEUP
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Arménio G. da Costa
(Author)
Other
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Carlos M. Silva
(Author)
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Francisco A. da Silva
(Author)
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Adélio Mendes
(Author)
FEUP
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Journal
Pages: 4630-4637
ISSN: 1944-3994
Indexing
Publicação em ISI Web of Knowledge ISI Web of Knowledge - 0 Citations
Publicação em ISI Web of Science ISI Web of Science
Publicação em Scopus Scopus - 0 Citations
Scientific classification
FOS: Engineering and technology > Chemical engineering
Other information
Authenticus ID: P-006-ACH
Abstract (EN): The manufacturing process of DOW Chemical Company in Portugal produces a brine stream containing organic contaminants. For recovering the sodium chloride by-product, it is necessary to fully characterize this brine stream. With this purpose, a direct immersion-solid phase microextraction-gas chromatograph (SPME-GC) analytical method was successfully optimized and implemented, being possible to quantify accurately, with reproducibility, the organic fraction at ppb levels. The effects of salt content, extraction time, temperature, and pH were investigated, and the SPME experimental conditions optimized. For the poly(dimethylsyloxane-co-divinylbenzene) fiber utilized, the resulting parameters were: 25% (wt.) of NaCl, 30¿min, 20°C, and pH 11. The fiber desorption was performed at 250°C for 15¿min. The calibration curves of the representative organics of the brine (benzenamine, cyclohexanamine, 2-methylbenzenamine, N¿cyclohexylcyclohexanamine, cyclohexyl alcohol, nitrobenzene, cyclohexanone, and 4-phenylcyclohexylamine) presented good correlation coefficients (0.991¿¿¿R 2 ¿¿¿0.997). The detection limits of the method were determined for each species for the optimized analytical conditions; the detection limits vary from 0.21 to 3.22¿ppb, respectively for N¿cyclohexylcyclohexanamine and benzenamine, the, precision ranged from 4.4 to 8.7% RSD and the validation criteria was obeyed for all analytes. The industrial brine stream was then characterized during several days to register the concentration history of contaminants. Independently of the stream composition fluctuations, the SPME methodology developed and optimized in this work was able to assess accurately their concentrations at ppb levels.
Language: English
Type (Professor's evaluation): Scientific
Notes: Publicação abrangida pelo Journal Citation Reports 2015
No. of pages: 8
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