0000000000277540

AUTHOR

M. Muñoz-ortuño

Rapid analysis of effluents generated by the dairy industry for fat determination by preconcentration in nylon membranes and attenuated total reflectance infrared spectroscopy measurement

Abstract This paper describes a new approach for the determination of fat in the effluents generated by the dairy industry which is based on the retention of fat in nylon membranes and measurement of the absorbances on the membrane surface by ATR-IR spectroscopy. Different options have been evaluated for retaining fat in the membranes using milk samples of different origin and fat content. Based on the results obtained, a method is proposed for the determination of fat in effluents which involves the filtration of 1 mL of the samples through 0.45 µm nylon membranes of 13 mm diameter. The fat content is then determined by measuring the absorbance of band at 1745 cm −1 . The proposed method c…

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Cotton swabs supported in-situ assay for quaternary ammonium compounds residues in effluents and surfaces

Abstract Cellulose paper and cotton swabs have been tested as sampling, reaction and measurement media for quaternary ammonium compounds (QACs) using the reagent Chromo Azurol S in the presence of aluminum cations (CAS-Al). On the basis of the results obtained a new method is proposed for the analysis of QACs in water samples which only entails the successive immersion of swabs into 1 mL of the samples, 1 mL of a solution of CAS-Al for the formation of a ternary blue complex, and 1 mL of water to remove the excess of reagent. The method can be used for the visual on site detection of QACs in effluents, as well as for their quantification within the 3.62–36.2 mg/L range through the direct me…

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A solid device based on doped hybrid composites for controlling the dosage of the biocide N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine in industrial formulations

A colorimetric composite device is proposed to determine the widely used biocide N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine (ADP).This sensing device is based on a film of 1,2-Naphthoquinone-4-sulfonate (NQS) embedded into polydimethylsiloxane-tetraethylortosilicate-SiO2 nanoparticles composite (PDMS-TEOS-SiO2NPs). Semiquantitative analysis can be performed by visual inspection. Digitalized image or diffuse reflectance (DR) measurements can be carried out for quantitative analysis. Satisfactory detection limit (0.018%, w/v) and relative standard deviations <12% were achieved. The proposed device has been applied for the determination of ADP in detergent industrial formulations with reco…

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A cost-effective method for estimating di(2-ethylhexyl)phthalate in coastal sediments.

This study describes the development of a new method for the analysis of di(2-ethylhexyl)phthalate (DEHP) using 0.1-0.3 g of sediment sample, based on matrix solid phase dispersion (MSPD) using C18 as dispersant phase (0.4 g) and acetonitrile-water as eluting solvent (3.4 mL 1:3.25, v/v). No evaporation step is required. 3 mL of extracts were processed on-line by in-tube solid phase microextraction (IT-SPME) coupled to capillary liquid chromatography (CapLC) and diode array detector (DAD). A short analytical column Zorbax SB C18 (35×0.5 mm, 5 μm) provided suitable results. FTIR-ATR was employed for characterizing sediment samples and MSPD procedure. The total analysis time was less than 20 …

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A new tool for direct non-invasive evaluation of chlorophyll a content from diffuse reflectance measurements

Abstract Chlorophyll is a key biochemical component that is responsible for photosynthesis and is an indicator of plant health. The effect of stressors can be determined by measuring the amount of chlorophyll a , which is the most abundant chlorophyll, in vegetation in general. Nowadays, invasive methods and vegetation indices are used for establishing chlorophyll amount or an approximation to this value, respectively. This paper demonstrates that H-point curve isolation method (HPCIM) is useful for isolating the signal of chlorophyll a from non-invasive diffuse reflectance measurements of leaves. Spinach plants have been chosen as an example. For applying the HPCIM only the registers of bo…

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A miniaturized method for estimating di(2-ethylhexyl) phthalate in bivalves as bioindicators.

This work has developed a miniaturized method based on matrix solid phase dispersion (MSPD), using C18 as dispersant and acetonitrile-water as eluting solvent, for the analysis of di(2-ethylhexyl) phthalate (DEHP) in biota samples by capillary liquid chromatography coupled to in-tube solid phase microextraction and diode array detection. Recovery studies showed that the combination of C18-Florisil® was optimal using low amount of samples (0.1 g) and with low volumes of acetonitrile-water (2.6 mL 1:3.25, v/v). The sample is processed in less than 30 min, no evaporation step is required. The proposed method was applied to the analysis of DEHP in mussels and of the coastal waters in which they…

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Polydimethylsiloxane composites containing 1,2-naphtoquinone 4-sulphonate as unique dispositive for estimation of casein in effluents from dairy industries.

A unique dispositive to determine casein which is the most abundant protein in dairy sewages has been proposed. In this sensing technology, the derivatization reagent 1,2-naphtoquininone 4-sulphonate (NQS) is embedded into a polydimethylsiloxane-tetraethylortosilicate-SiO2 nanoparticles composite (PDMS-TEOS-SiO2NPs). When the composite is immersed into the samples, casein is extracted from the solution and derivatized inside the PDMS matrix after 10 min at 100°C. The sensing support changes its color from yellow to orange depending on the casein concentration. Quantitative analysis can be carried out by measuring the absorbance with a reflection probe or by image-processing tool (GIMP). Thi…

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Multiresidue analysis of organic pollutants by in-tube solid phase microextraction coupled to ultra-high performance liquid chromatography-electrospray-tandem mass spectrometry.

In this work, in-tube solid phase microextraction (IT-SPME) coupling with ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) multiresidue analytical method has been proposed for the first time for on-line enrichment of 9 analytes included in Water Frame Directive 2000/60/EC (WFD). The device was equipped with a GC TRB-5 capillary column, used as pre-concentration loop, and two conventional six-port injection valves. Water sample and desorption solvent volumes were tested. The optimum conditions were 4mL of processed sample followed by elution with 40μL of methanol. The analytes were detected with a mass spectrometer after being ionized positively using an elect…

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On-line in-tube solid phase microextraction-capillary liquid chromatography method for monitoring degradation products of di-(2-ethylhexyl) phthalate in waters

Abstract The main di-(2-ethylhexyl) phthalate (DEHP) degradation products, (2-ethylhexyl) phthalate (MEHP), diethyl phthalate (DEP) and dibutyl phthalate (DBP), have been tested. The proposed cost-effective method combines on-line, in-tube solid-phase micro extraction (IT-SPME) in in-valve configuration and capillary liquid chromatography with UV diode array detection (Cap-LC-DAD). Acidification of the samples at pH 3 improved markedly the estimation of MEHP. Aliquots of 4 mL of acidified water samples were directly processed. After sample loading, the analytes were desorbed with the mobile-phase and transferred to the monolithic capillary column. Satisfactory linearity and precision, absen…

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