0000000000329008
AUTHOR
Jose M Garrigues
Fourier-transform infrared determination of nicotine in tobacco samples by transmittance measurements after leaching with CHCl3
Abstract A new procedure is proposed for the FT-IR spectrometric determination of nicotine in tobacco. The method is based on the extraction of nicotine in CHCl 3 from tobacco samples, wetted with an aqueous solution of NH 3 (0.1 M), and the measurement of absorbance in the stopped-flow mode at 1316 cm −1 , using a spectral baseline correction established from 1334 to 1300 cm −1 . The procedure developed does not requires a complex sample preparation, and provides a limit of detection of 0.045 mg ml −1 nicotine, a sampling frequency of 3.3 h −1 and a coefficient of variation of 0.3% for five independent measurements of a tobacco sample with a nicotine content of 1.5% w/w. The accuracy of th…
Flow injection Fourier transform infrared determination of nicotine in tobacco
A fully automated procedure is proposed for the Fourier transform infrared (FTIR) determination of nicotine in tobacco. The method is based on the on-line extraction of nicotine with CHCl3. Samples, weighed inside empty extraction cartridges, were humidified with NH3 and the cartridges were installed in a flow manifold in which they were extracted with 2 ml CHCl3 for 2 min, then 400 microliters of the extract were introduced into a micro-flow cell using a carrier of CHCl3 and the IR spectrum was registered continuously. The absorbance, in the wavenumber range 1334-1300 cm-1, was measured, obtaining a peak as a function of time. The area of this peak was interpolated on a calibration line es…
Selection of calibration set samples in determination of olive oil acidity by partial least squares–attenuated total reflectance–Fourier transform infrared spectroscopy
Abstract A chemometric method has been applied for the determination of the free fatty acid (FFA) concentration in commercial olive oil samples of different types an origins by using Fourier transform infrared spectroscopy (FTIR) attenuated total reflectance (ATR) measurements. Different methods for selecting the training set, including hierarchical cluster analysis, were applied and compared. The prediction capabilities of partial least squares (PLS) multivariate calibration methods, net analyte signal (NAS) preprocessing followed by PLS or classical least squares (CLS) regression method of ATR–FTIR data were evaluated. Several aspects, like spectral range to be considered, different prepr…
Flow injection Fourier transform infrared determination of caffeine in coffee
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 on-line 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, …
Direct ATR-FTIR determination of sucrose in beet root.
A simple and fast procedure has been developed for the direct determination of sucrose in beet root samples through attenuated total reflectance Fourier transform infrared absorbance measurements (ATR-FTIR) at 1056 cm(-1) with a baseline established between 1187 and 887 cm(-1). The method only requires a previous crushing or liquefaction of samples and it is free from matrix effects and from the interference of minoritary sugars and fermentation molecules. Aqueous solutions of sucrose can be used as standards and recovery values from 101 to 103% were found for spiked concentration levels from 3.5 to 10.5% (w/w). The limit of detection provided by this method corresponds to 0.15% (w/w) of su…
Direct determination of ethanol and methanol in liquid samples by means of vapor phase-Fourier transform infrared spectroscopy
Abstract A FTIR procedure is proposed for the direct determination of methanol and ethanol in liquid samples, such as alcoholic beverages and eau-de-cologne, based on vapor generation from small injected volumes of untreated samples into a heated Pyrex glass reactor in which, at a temperature of 80°C, ethanol and methanol are volatilized and introduced into a long-path IR gas cell by means of a N2 carrier flow. The IR spectra obtained present two characteristic ethanol bands (1050 and 880 cm−1) and a single characteristic methanol band (1030 cm−1). The measurement of the area of the transient recording obtained for the wavenumber range between 1025–950 and 950–820 cm−1 allows us the determi…