Search results for " Time"
showing 10 items of 3005 documents
Focused microwave-assisted Soxhlet extraction: An expeditive approach for the isolation of lipids from sausage products
2003
A prototype of extractor based on the conventional Soxhlet principles but assisted in the cartridge zone by focused microwaves is proposed for accelerating the extraction of lipids from sausage products. The extraction process has been optimised using a multivariate design involving the main variables influencing the performance of the prototype (namely, irradiation power P, irradiation time T and number of cycles C). Under the optimum working conditions (P=160 W, T=10 s and C=14), the extraction of lipids from different Spanish sausage products is complete in 45 min. The extracts thus obtained have been compared with those provided by conventional Soxhlet extraction for 8 h by development …
Evaluation of extraction alternatives for Fourier transform infrared spectrometric determination of oil and greases in water
1997
Abstract Liquid-liquid extraction (LLE), solid phase extraction (SPE) and microwave-assisted extraction are evaluated for Fourier transform infrared (FTIR) spectrometric determination of oil and grease in polluted waters. A fast microwave-assisted quantitative procedure is proposed for the total extraction of oil and grease into CCl 4 from water samples, with an irradiation time of 1 min at an exit power of 520 W using closed PTFE vessels. The FTIR quantification of oil and grease is carried out by the measurement of the area under the absorbance spectra in the range between 3058 and 2780 cm −1 , with a baseline established between 3200 and 2700 cm −1 . The analytical features of the propos…
On the measurement of consistent long-term retention factor values in micellar liquid chromatography
2007
Abstract In the field of the quantitative structure–retention and retention–activity relationships (QRAR and QSRR) is crucial to obtain consistent retention factors (k). For this purpose, two unbiased approaches to estimate k are used: (i) the IUPAC approach (based on the extra-column time correction) and (ii) the ‘2-references’ approach (based on the k estimation respect to two prefixed reference k values). Three reference chemicals were selected attending to their retention time, chemical stability and non-ionic character. Consistent retention factor values for these references were estimated for C18 chromatographic columns and Brij35 solutions as mobile phases after statistical analysis.…
Emerging approaches to estimate retention factors in high performance liquid chromatography.
2004
The retention factor is one of the most universally used parameters in chromatography. The errors associated with the conventional ways to determine the retention factor of compounds in liquid chromatography are studied and compared with those corresponding to new approaches. The later avoid the use of extra-column time and hold-up time values, which have proven to be tedious and ambiguous. Simulations and real data, used to examine the accuracy of four different approaches (two classic and two new), suggest that the new approaches could be considered more satisfactory than the classic ones.
Performance of Markers and the Homologous Series Method for Dead Time Estimation in Reversed-Phase Liquid Chromatography
2009
Abstract Two methods for dead time estimation (the use of markers and the homologous series mathematical method) are revised. Out of twelve assayed common markers, only KBr, KI, tartrazine, thiourea, uracil, and urea yielded retention times independent of the mobile phase composition in the range 10–90% acetonitrile, using a Zorbax Eclipse XDB−C18 column. On the other hand, the quality of the estimations provided by the homologous series method was limited by the mathematical approach and the data quality. With this method, the estimated dead time is an extrapolated value, which is severely affected by the data of the most retained compounds that act as leverage points, biasing the result. …
A multinjection strategy for mercury speciation.
2005
Abstract A multiinjection strategy has been developed to increase the sampling throughput of the high-performance liquid chromatography determination of inorganic-mercury, methylmercury, ethylmercury and phenylmercury. The method involves the injection of samples each 3.5 min, in spite of the fact that phenylmercury retention time corresponds to 9.04 min. In the selected conditions, the sampling frequency was 11 h −1 in front of that of 6 h −1 , obtained by conventional injection of each sample after the complete elution of Hg species. Additionally, the analytical reagents consumption was reduced drastically in almost 50%. The main characteristics of the chromatographic separation were main…
Reliability of the retention factor estimations in liquid chromatography.
2004
The retention factor is one of the most universally used parameters in chromatography. However, large differences in the experimental retention factor values are observed when the same compound is injected in a given stationary/mobile phase system under intermediate precision conditions. Conventional protocols for estimating retention factors have problems that mainly arise from difficulties in the hold-up time measurements and the omission of the existence of extra-column times by practicing chromatographers. In the present paper, three different approaches for estimating retention factors are tested: (i) classical retention factor estimations based on the gross hold-up time, (ii) based on…
On the Measurement of Dead Time in Micellar Liquid Chromatography
1996
Abstract Modelling of the retention of solutes in micellar liquid chromatography allows the optimization of the resolution of a mixture of solutes and the determination of physico-chemical retention parameters. Both tasks imply the calculation of capacity factors, which are severely affected by the value of dead time. However, the determination of the dead time is not easy when a micellar mobile phase is used owing to the wide and variable perturbations that appear at the heads of the chromatograms. Four different criteria of determination of a reference time in the chromatograms are proposed and compared. The criteria are applied to mobile phases containing a varying concentration of surfa…
H-point standard additions method for resolution of overlapped chromatographic peaks with a conventional fluorescence detector. Determination of phen…
1996
The H-Point Standard Additions Method (HPSAM) is proposed in order to resolve overlapping peaks in liquid chromatography by using a conventional fluorescence detector. The method uses as analytical signals the heights or the areas obtained at two previously selected emission wavelengths, and good results are obtained for highly overlapping peaks with highly overlapping fluorescence spectra. The principal benefits of the method are the ease of finding the required wavelengths, its insensitivity to changes in the retention time of the peak from one injection to another, and the possibility of using it in highly or only partially overlapping peaks. We have applied the method to the determinati…
Global treatment of chromatographic data with MICHROM
1997
Abstract The program MICHROM for the general treatment of chromatographic data is presented. MICHROM takes part in all the stages of the analytical process. It allows determination of dead time, smoothing of chromatograms, measurement of peak parameters, fitting of skewed peaks, and deconvolution of overlapped peaks. Tools for the experimental design, optimization of the mobile phase composition to resolve a mixture of analytes, and simulation of chromatograms in several experimental conditions, are implemented. Routines for the graphical representation of chromatograms, resolution surfaces, contour maps, management of data series, optimization and regression analysis, are also included. Th…