Refine
Document Type
Conference Type
- Konferenzartikel (1)
Has Fulltext
- no (4) (remove)
Is part of the Bibliography
- yes (4)
Keywords
- Vergleich (4) (remove)
Institute
Open Access
- Closed Access (3)
- Open Access (1)
The Raman spectra from the chemical compounds toluene and cyclohexane obtained using a Fourier Transform (FT)-Raman spectrometer prototype have been contrasted with the Raman spectra of these same materials collected with two different commercial FT-Raman devices. The FT-Raman spectrometer consist of a Michelson interferometer, a self-designed photon counter and a reference photo-detector. The evaluation methodology of the spectral information, contrary to the commercial devices that commonly use the zero-crossing method, is carried out by re-sampling the Raman scattering and by accurately extracting the optical path information of the Michelson interferometer. The FTRaman arrangement has been built using conventional parts without disregarding the spectral frequency precision that usually such a FTRaman instruments deliver. No additional complex hardware components or costly software modules have been included in this FT-Raman device. The main Raman lines from the spectra obtained with the three FT-Raman devices have been compared with the Raman lines from the standard Raman spectra of these two materials. The values obtained using the FT-Raman spectrometer prototype have shown a frequency accuracy comparable to that obtained with the commercial devices without facing the need for a large investment. Although the proposed FT-Raman prototype cannot be directly compared to the last generation of FT-Raman spectrometers from the commercial manufacturers, such a device could give an opportunity to users that require high frequency precision in their spectral analysis and are provided with rather scarce resources.
An interlaboratory comparison was carried out to evaluate the effectiveness of a method based on HPTLC in which reagent-free derivatization is followed by UV/fluorescence detection. The method was tested for the determination of sucralose (C12H19C13O8; (2R,3R,4R,5S,6R)-2-[(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan-2-yl]oxy-5-chloro-6-hydroxymethyl)oxane-3, 4-diol; CAS Registry No. 56038-13-2) in carbonated and still beverages at the proposed European regulatory limits. For still beverages, a portion of the sample was diluted with methanol-water. For carbonated beverages, a portion of the sample was degassed in an ultrasonic bath before dilution. Turbid beverages were filtered after dilution through an HPLC syringe filter. The separation of sucralose was performed by direct application on amino-bonded (NH2) silica gel HPTLC plates (no cleanup needed) with the mobile phase acetonitrile-water. Sucralose was determined after reagent-free derivatization at 190 degrees C; it was quantified by measurements of both UV absorption and fluorescence. The samples, both spiked and containing sucralose, were sent to 14 laboratories in five different countries. Test portions of a sample found to contain no sucralose were spiked at levels of 30.5, 100.7, and 299 mg/L. Recoveries ranged from 104.3 to 124.6% and averaged 112% for determination by UV detection; recoveries ranged from 98.4 to 101.3% and averaged 99.9% for determination by fluorescence detection. On the basis of the results for spiked samples (blind duplicates at three levels), as well as sucralose-containing samples (blind duplicates at three levels and one split level), the values for the RSDr ranged from 10.3 to 31.4% for determinations by UV detection and from 8.9 to 15.9% for determinations by fluorescence detection. The values for the RSDR values ranged from 13.5 to 31.4% for determinations by UV detection and from 8.9 to 20.7% for determinations by fluorescence detection.