University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Spectrophotometry

Citations 53

"Flow Injection Fourier Transform Infrared Determination Of Caffeine In Coffee"
Vib. Spectrosc. 1999 Volume 21, Issue 1-2 Pages 143-150

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Zouhair Bouhsain, Jose M. Garrigues, Salvador Garrigues and Miguel de la Guardia

Abstract: A fully automatized procedure has been developed for the Fourier transform infrared (FT-IR) spectroscopic determination of caffeine in coffee samples. The method involves the online extraction of caffeine with CHCl3. Samples, weighed inside empty PTFE cartridges of 0.5 cm internal diameter (i.d.) and 1.5 mL volume, were humidified with four drops of 0.25 M NH3. The cartridge was installed in a flow manifold, in which samples were extracted in a closed-flow system with 1 mL CHCl3, during 6 min. Four hundred microliters of the extract were introduced in a microflow cell and absorbance measured as a function of time at 1659 cm-1, with a baseline established between 1900 and 830 cm-1, thus providing a fiagram. Peak height values of the Fl recordings, obtained for samples, were interpolated in an external calibration line established from standard solutions of caffeine in CHCl3,. The method provided a limit of detection (LOD) of 9 mg L-1 caffeine, a relative standard deviation of 0.6% for five independent measurements of a solution containing 1 mg mL-1 and a sampling frequency of the whole procedure of 6 h-1. Results obtained for market samples agree well with those found by the official chromatographic-spectrometric method, but involving a drastic reduction of solvents, from the 200 mL ether and 50 mL CHCl3, required for each sample preparation by the reference procedure to less than 30 mL CHCl3, necessaries for the whole determination of caffeine in a sample, also including standards and carrier solution.
Caffeine Coffee Interface Optimization Method comparison

"Sheath-flow Fourier Transform Infrared Spectrometry For The Simultaneous Determination Of Citric, Malic And Tartaric Acids In Soft Drinks"
Anal. Chim. Acta 2000 Volume 417, Issue 1 Pages 41-50

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María José Ayora-Cañada and Bernhard Lendl

Abstract: A new approach for the determination of organic acids in soft drinks based on pH modulation and Fourier transform infrared spectroscopic detection is presented. The analytical readout was taken from the spectral changes induced by the pH change of the sample. The pH modulation was carried out in a novel sheath-flow cell which was connected to a sequential injection analysis system. The sheath-flow cell comprised three stream lines flowing adjacent to each other in a strongly laminar fashion, The sample (pH similar to 9) was introduced in the central channel whereas reagent (hydrochloric acid) was introduced in the outer channels. As a consequence of the laminar flow profile, hardly any mixing between the stream lines was observed while maintaining the flow, hence allowing the measurement of the sample spectrum at alkaline pH (similar to 9). Upon stopping the flow, diffusion of protons from the outer stream lines into the central line occurred resulting in a complete protonation of the analyte (pH similar to 2). The spectral changes were calculated and the region between 1400 and 1180 cm-1 used to set-up a partial least squares (PLS) calibration model. For the PLS model only standards containing the analytes but no matrix molecules were used. By evaluation of the spectral changes induced by the pH modulation the PLS model could successfully be applied to test samples containing sugars as well as to natural soft drinks.
Citric acid l-Malic acid Tartaric acid Soft drink Sequential injection Sheath flow Partial least squares Stopped-flow

"Sequential Injection Fourier Transform Infrared Spectroscopy For The Simultaneous Determination Of Organic Acids And Sugars In Soft Drinks Employing Automated Solid Phase Extraction"
Anal. Chim. Acta 2000 Volume 422, Issue 1 Pages 63-69

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Hai LeThanh and Bernhard Lendl

Abstract: A fully automated method for the rapid determination of organic acids (citric-, malic- and tartaric acid) and sugars (glucose, fructose, and sucrose) in soft drinks by sequential injection Fourier transform infrared (FTIR) spectroscopy is presented. A convective interaction media (CIM) disc carrying quaternary amino moieties was added as a solid phase extraction column to the flow system. Upon injection of a sample the organic acids were completely retained on the CIM disc whereas sugars passed to the flow cell. The organic acids were subsequently eluted by injection of an alkaline (pH 8.5) 1 M sodium chloride solution and recorded in their fully deprotonated form as a second flow injection peak. In both cases, the FTIR spectra corresponding to the peak maxima were selected for data evaluation. Two partial least squares models, one for sugars and the other for organic acids, were constructed based on the analysis of standards containing all six analytes. The developed method was applied to natural samples yielding results which were in good agreement with those obtained by an external reference method (enzymatic test kits). Deviations in the results were 3.4. and 4.1% for citric and malic acid and ranged from 4.7-5.1% for the sugars. The developed method is characterized by its short analysis time, experimental simplicity and its potential applications in routine analysis and process control.
Citric acid l-Malic acid Tartaric acid Glucose Fructose Sucrose Soft drink Sequential injection Preconcentration Method comparison Solid phase extraction

"Flow Injection Fourier Transform Infrared Spectrometric Analysis"
Anal. Chim. Acta 1992 Volume 261, Issue 1-2 Pages 53-57

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M. de la Guardia*, S. Garrigues and M. Gallignani, J. L. Burguera and M. Burguera

Abstract: A µflow cell with KBr windows (Specac, Orpington, UK) and a demountable µflow-through cell (Spectra Tech, Warrington, UK) were used in a Perkin-Elmer model 1750 FTIR spectrometer with data station to detect o-xylene (as test species) injected into a stream of hexane. Programs were written to obtain and accumulate the IR spectra (820 to 670 cm-1) of the sample zone, which took only 19 s. The effects of cell thickness, injection volume and carrier flow rate on the sensitivity, limit of detection and reproducibility of measurement were assessed. A flow rate of 0.5 mL min-1 gave the best results, and a resolution of 4 cm-1 afforded good sensitivity and reproducibility. The two cells showed similar performance. A limit of detection of 0.01% (v/v) was attainable, and for 0.4% of o-xylene the coefficient of variation was ~1% (n = 5). A method has been developed for obtaining and storing the complete Fourier transform spectrum, of a sample in a flowing stream in only 19 s. A resolution of 4 cm-1 is recommended. The determination of o-xylene in xylol was employed as a test system, using hexane as a carrier and diluent in all the experiments A classical liquid flow cell and a demountable flow-through cell were compared. The best limit of detection obtained was 0.01%(v/v). The effects of flow-rate and injection volume were studied for the two cells used. The relative standard deviation (0.4% o-xylene, n = 5) was ~1%.
2-Xylene Organic compound Computer Optimization

"Exploiting Stopped-flow Injection Methods For Quantitative Chemical Assays"
Anal. Chim. Acta 1992 Volume 261, Issue 1-2 Pages 11-21

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