Chemical fractionation methods

With heavy metals, the problem L an increasing one. Earlier studies [1,2 ] indicate that heavy metal accumulation in environmental sink.s, such as lake and river sediments and soil and vegetation in the Kuala Lumpur area, exceed the baseline values by several magnitudes. Further studies based on chemical fractionation methods show that the anthropogenic contributions of heavy metals, especially of Pb, Zii, anil Cd are rather substantial [3 -5 ]. 

Chemical fractionation methods used in this study were gel cFromatography, acid-base neutral solvent partitioning and chromatography on silica gel columns. Identification of compounds was done by gas chromatography/mass spectrometry (GC/MS). Proton nuclear magnetic resonance (PMR) spectroscopy was used to characterize fractions and subfractions which were not amenable to GC/MS analysis. 

In addition, there is a better understanding of chemical fractionation methods (e.g., Mester et al., 1998 Sahuquillo et al., 1999). 

The experimental studies cited below have isolated and tested the impact of caffeine, different methods of preparation, and different chemical fractions of coffee beans on serum cholesterol levels over a varied range of time periods. 

Fractionation Methods. Ultrafiltration and gel filtration are nondestructive methods which, based on limited experience, can be used for fractionation of mineral complexes from digests. In earlier studies mineral absorption on the gel material was a problem. Lonnerdal (30) introduced a method of treating dextran gels with sodium borohydride in order to eliminate the mineral-binding sites on the gel. In preliminary studies we have recovered more than 90 of Ca, Mg, Fe, Zn and P in samples applied to a borohydride-treated gel column (Sephadex G-50, Pharmacia Fine Chemicals, Piscataway, NJ). Recovery of Ca (Table IV) and Mg, Fe and Zn from ultrafiltration was also good. 

We have employed two different protocols for the chemical fractionation of GSE obtained from MegaNatural-AZ based on the amounts needed for bioactivity-based assays. Batches of GSE (50 g) were extracted in acetone/water (7 3) under N2 with mechanical agitation for 12 h. The acetone was removed on a rotary evaporator and the aqueous phase was freeze-dried to yield 48 g of tannin crude extract (TCE). TCE was further fractionated following two different methods. 

The development of a commercial mass spectrometer and its application to hydrocarbon gas analysis by the method of Washburn et al. (63) made gas analysis rapid, economical, and, what is even more important, inspired a confidence in the results of routine hydrocarbon gas analysis which was badly lacking. A complex gaseous mixture comprising the atmospheric gases, carbon monoxide, and Ci to C6 hydrocarbons required more than 20 hours of applied time by the previous methods of low temperature fractional distillation coupled with chemical absorption methods. With the mass spectrometer such an analysis is completed in 2 hours or less, about 15 minutes of which is consumed in the... 

In considering photoactivity on metal oxide and metal chalcogenide semiconductor surfaces, we must be aware that multiple sites for adsorption are accessible. On titanium dioxide, for example, there exist acidic, basic, and surface defect sites for adsorption. Adsorption isotherms will differ at each site, so that selective activation on a particular material may indeed depend on photocatalyst preparation, since this may in turn Influence the relative fraction of each type of adsorption site. The number of basic sites can be determined by titration but the total number of acidic sites is difficult to establish because of competitive water adsorption. A rough ratio of acidic to basic binding sites on several commercially available titania samples has been shown by combined surface ir and chemical titration methods to be about 2.4, with a combined acid/base site concentration of about 0.5 mmol/g . 

Chromatography is a physico-chemical process that belongs to fractionation methods in the same vein as distillation, crystallisation or fractionated extraction. It is believed that the separation method in its modern form originated at the turn of the century from the work of Tswett to whom we attribute the terms chromatography and chromatogram. 

The liquid-liquid, acid-base fractionation method was preferred over HPLC by the liquid waste panel members because it is a better validated technique for the isolation of components that are toxic or that might otherwise interfere with the assay. Also, the distribution of activity in the acid, base, and neutral fractions provides a preliminary estimate of the types of chemicals responsible for the mutagenicity. 

In the early history of gas chromatogra-phy/olfactometry (GC/O vn/tgu), the goal of GC/O analysis was to determine when an odor elutes from a GC in order to identify it. The analysis yielded a list of times and, with appropriate standards, retention indices. When combined with other chemical analysis methods, such as mass spectrometry (MS), a name for a particular odorant could be proposed. Comparing both the chemical and sensory properties of the odorant with those of authentic standards allowed researchers to identify the odorant with considerable certainty. The number of odorants that are detected, however, is determined by a number of factors, including the design of the olfactometer, the fraction of the extract injected, and, as we now suspect, the genetics of the sniffer. 

Abstract Overcoming the complexity of cheese matrix to reliably analyze cheese composition, flavor, and ripening changes has been a challenge. Several sample isolation or fractionation methods, chemical and enzymatic assays, and instrumental methods have been developed over the decades. While some of the methods are well... 

An alternative approach for screening the composition of phytoplankton exudates is to use either 14C-tracer methods combined with chemical fractionation (Hama and Handa, 1987 Siuda and Wcisko, 1990 Sundh, 1991) or colorimetric methods (Obernosterer and Herndl, 1995 Biddanda and Benner, 1997) to characterize the contribution of different classes of organic compounds (carbohydrates and amino acids in polymeric or monomeric forms) to the total pool of exudates. These studies revealed that monomeric and combined carbohydrates were the major components of exudates, typically accounting for 20-90% of the total extracellularly released DOM. 

Humic substances account for 40-70% of the DOC in rivers and 5-25% of the DOC in the ocean (Table I). It is important to note that recoveries of adsorbed humic substances from XAD resins are not quantitative, so the chemical characteristics of the recovered humic substances are not necessarily representative of all the humic substances retained by the resin. Tangential-flow ultrafiltration retains 45-80% of the DOC in rivers and 25-40% of the DOC in the surface ocean (Table I). Essentially all of the DOC retained during ultrafiltration is recovered for chemical characterization. In general, ultrafiltration recovers a larger fraction of the DOM from these systems. These methods also isolate DOM based on different mechanisms. Adsorption onto XAD resins at low pH chemically fractionates the DOM and isolates the more hydrophobic components, whereas ultrafiltration principally separates components of DOM on the basis of size and shape. 

This paper outlines the basic principles and theory of sedimentation field-flow fractionation (FFF) and shows how the method is used for various particle size measurements. For context, we compare sedimentation FFF with other fractionation methods using four criteria to judge effective particle characterization. The application of sedimentation FFF to monodisperse particle samples is then described, followed by a discussion of polydisperse populations and techniques for obtaining particle size distribution curves and particle densities. We then report on preliminary work with complex colloids which have particles of different chemical composition and density. It is shown, with the help of an example, that sedimentation FFF is sufficiently versatile to unscramble complex colloids, which should eventually provide not only particle size distributions, but simultaneous particle density distributions. 

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