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

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

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 chromat...

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Bibliographic Details
Published in:Desalination and water treatment Vol. 51; no. 22-24; pp. 4630 - 4637
Main Authors: Lima, João F.B., Da Costa, Arménio G., Silva, Carlos M., Da Silva, Francisco A., Mendes, Adélio
Format: Journal Article Conference Proceeding
Language:English
Published: L'Aquila Elsevier Inc 01-06-2013
Desalination Publications
Elsevier Limited
Subjects:
Alcohols
Analysis methods
Analytical chemistry
Applied sciences
Brines
Byproducts
Characterization
Chemistry
Chromatographic methods and physical methods associated with chromatography
Coefficients
Concentration (composition)
Contaminants
Correlation coefficients
Cyclohexanone
Detection
Divinylbenzene
Exact sciences and technology
Fibers
Fraction
Gas chromatographic methods
Gas chromatography
Industrial brine
Mathematical analysis
Nitrobenzene
Organic
Organic chemistry
Organic contaminants
pH effects
Pollution
Rivers
Saline water
Salt water
Sodium
Sodium chloride
Solid phase methods
Solid phase microextraction
Solid phases
Streams
Submerging
Wastes
Portugal
Solid phase microextraction
Characterization
Industrial brine
Fraction
Organic
Trace analysis
Nitro compound
Chemical analysis
Brine
Alcohol
Aniline derivatives
Flame ionization detector
Ketone
Chemical enrichment
Gas chromatography
Industrial waste
Amine
Sample preparation
Aromatic amine
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Summary: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 ⩽ R2 ⩽ 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.
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ISSN:1944-3986
1944-3994
1944-3986
DOI:10.1080/19443994.2012.758599