Search results for "Gel permeation chromatography"
showing 10 items of 115 documents
1981
The dynamical region of the measured calibration curves is investigated using the results of the theory published previously. The kinetic constants of the flow-equilibrium are calculated from the measurements according to two different models for a spontaneous polymer diffusion of the transported P-mer from sol into gel of the Phase Distribution Chromatography (PDC)-column. The corresponding lateral concentration profiles in the gel are found by analytical integration of Fick's second law under the corresponding boundaries. An energetic model of this flow-equilibrium is stated, giving the activation enthalpy and -entropy of the rediffusion of the polymer from gel into sol after some retarda…
Determination of PAHs in airborne particles by accelerated solvent extraction and large-volume injection-gas chromatography-mass spectrometry.
2006
Abstract A sensitive and automated method is presented for the determination of polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter. The procedure includes extraction of PM10-bound PAHs by accelerated solvent extraction (ASE) followed by gel permeation chromatography (GPC) clean-up, and large-volume programmable temperature vaporizer (PTV–LV) injection coupled to GC–MS. The limit of detection (LOD) of the whole method, based on a signal-to-noise ratio (S/N) of 3:1, ranged from 0.26 pg m−3 to 3 pg m−3 when air volumes of 760 m3 are collected. The hexane–acetone mixture (1:1, v/v) gave the best recoveries when ASE parameters were fixed at 125 °C, 1500 psi, and a total time …
A rapid and reliable size-exclusion chromatographic method for determination of kojic dipalmitate in skin-whitening cosmetic products
2007
A size-exclusion chromatographic method has been developed to determine the relatively novel skin-whitening agent called kojic dipalmitate (KDP) in skin-whitening cosmetic products. Preliminary experiments were carried out in order to select the solvent for standard and sample solution, and also for mobile phase composition. A PLGel Mixed-D (polystyrene/divinylbenzene co-polymer) column and isocratic mobile phase of pure tetrahydrofuran (at 1.5 mL min(-1) flow rate) were used. Detection was carried out by means of an UV/vis spectrometry detector set at 248 nm. A study of interferences reveals that KDP can be determined without interferences coming from cosmetic matrices. Most other cosmetic…
Contributions to the analysis of organic xenobiotics in fish
1995
For the residue-analysis of fish samples, a method has been developed to separate the medium polar triazines and acetamides together with lipophilic xenobiotics (organochlorine pesticides, PCBs and octachlorostyrene) from fish tissue. The detection limits of the analytes are mostly within the ppt-range (ng/kg fillet) and vary between 40 and 1050 ng/kg fillet of fish. Their recoveries range from 75 to 108%, spiked at 1.5 μg/kg. The substances are extracted with a mixture of petroleum ether/ethylacetate (2:1) using a soxhlet apparatus. Subsequently, the lipids in the sample extracts are reduced to 0.4% by gel chromatography. A 5 g silica gel clean-up separates the analytes according to their …
Development of a method for the analysis of seven banned azo-dyes in chilli and hot chilli food samples by pressurised liquid extraction and liquid c…
2008
An automated, confirmatory and sensitive procedure has been developed and validated for the determination of Sudan (I-IV), Sudan Orange G, Sudan Red 7B and Para Red in hot chilli food samples. The proposed method includes pressurised liquid extraction (PLE) with acetone, gel permeation chromatography (GPC) clean-up and detection by liquid chromatography (LC) coupled to electrospray ionization in positive mode tandem mass spectrometry (ESI-MS-MS). The main parameters affecting the performance of the different ionization sources and PLE parameters were previously optimised using statistical design of experiments (DOE). The method was in-house validated on chilli powder and chilli meat. Linear…
On-line gel permeation chromatography–attenuated total reflectance–Fourier transform infrared determination of lecithin and soybean oil in dietary su…
2007
Gel permeation chromatography (GPC) with attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectrometry detection has been proposed for the simultaneous determination of lecithin and soybean oil in dietary supplements. The method involves the extraction of analytes with dichloromethane in an ultrasound water bath and the injection of 2 ml of centrifuged and filtered extracts into the system integrated by two Envirogel GPC columns (19 mm x150 mm, 19 mm x 300 mm) coupled on-line. Dichloromethane was used as mobile phase. A method has been developed to select the most appropriated wavenumber to be used for the determination of each considered compound from the calculation of a…
Polymerization of methyl methacrylate through ionizing radiation in CO2-based dense systems
2000
Herein, we report the use of ionizing radiation to induce a dispersion polymerization reaction in dense CO2. As a model system, the polymerization of methyl methacrylate in the presence of poly(dimethylsiloxane) stabilizers was investigated. It was demonstrated that the dose plays the key role in the progress of the reaction and in the morphology of the resulting polymer. Dispersion polymerization carried out in the presence of mono- and bifunctionalized surfactants gave differently structured polymers. The polymers obtained have been characterized by scanning electron microscopy, solubility tests, and gel permeation chromatography, and the molecular structure has been related to dynamic me…
1988
Synthese par alkylation reductrice de l'anthracene par des electrophiles bifonctionnels comme le dibromo-1,3 propane. Le polymere du titre est un precurseur du polymere redox polyanthrylenetrimethylene
Molekulargewichtsverteilungen bei der rein thermischen Substanzpolymerisation von Styrol
1972
An rein thermisch in Substanz polymerisiertem Styrol wurden an Testfraktionen mittels kombinierter Gelchromatographie und Viskosimetrie die Molekulargewichte bestimmt. Dabei erhalt man die absoluten Molekulargewichte unabhangig von einer in den Praparaten auftretenden Verzweigung. Die Verteilungen selbst wurden gelchromatographisch gemessen. Fur die Breite der Molekulargewichtsverteilungen ergeben sich im Mittel Mw/Mn-Werte von 2,2. Dies entspricht einer Uneinheitlichkeit U = 1,2, die also etwas groser ist, als bei einer ScHuLzverteilung mit Kopplungsgrad 1. Der hohere U-Wert last sich durch die Nichtstationaritat des realen Polymerisationsvorganges und den Verzweigungsmechanismus erklaren.…
Strukturuntersuchung von polyestern durch direkten abbau im massenspektrometer, 3. Poly-β-propiolacton, poly-β-pivalolacton und poly-δ-valerolacton
1978
Poly(oxycarbonylethylene) (poly-β-propiolactone), poly(oxycarbonyl-1,1-dimeothylethylene) (poly-β-pivalolactone), and poly(oxycarbonyltetramethylene) (poly-δ-valerolactone) were pyrolyzed directly in the ion source of a mass spectrometer and their thermal and electron impact induced degradation mechanisms are established. Poly-β-propiolactone is thermally degraded by rupture of the OCH2-bond by a cis elimination to give carboxyl and acryloyl endgroups, whereas poly-δ-valerolactone depolymerizes to δ-valerolactone. Poly-β-pivalolactone degrades thermally to cyclic oligomers of pivalolactone, which could be proved by a separated pyrolysis and IR-spectroscopy and gel chromatography.