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D Melucci

Publications and source records attributed to D Melucci.

3 recordsLinked to original sources

Working without accumulation membrane in flow field-flow fractionation.

Nonideal interaction of sample with the separation device is a difficulty found in chromatographic methods as well as in field-flow fractionation. However, in field-flow fractionation (FFF), greater flexibility in the choice of carrier solution composition is possible, thus reducing the need of a wide choice of surface chemistry when nonideal sample interaction is to be minimized. The use of an ultrafiltration membrane as the surface for the accumulation wall is common practice in flow field-flow fractionation. Typical membranes in use are laminates of a skin membrane onto a backing material such as woven polyester. At this point, only a limited choice of membrane chemistries is available. Many membranes have been developed for protein applications as membranes are widely used in the pharmaceutical industries. While these membranes work well for protein applications, flow field-flow fractionation is applicable to polymeric particulate as well as protein samples. Thus, sample interaction with the membrane surface is possible with nonprotein applications and these interactions can induce significant secondary effects on retention ratio and affect instrumental reliability. Also, the woven texture of membranes may detrimentally affect the FFF separation. For these reasons, the study of flow field-flow fractionation using a flat, smooth surface of controlled chemistry is of relevance. We present here the results of a new, membraneless channel that uses a bare frit as the accumulation wall and that is intended for analysis of micrometer-sized particles only. Selectivity results are comparable to those obtained with the membrane, while relative sample recovery indicates that the best quantitative performance can be obtained without the membrane. Moreover, neither sample immobilization nor losses through the frit occur when operating membraneless. On the other hand, first experimental evidence of a certain level of frit surface activity suggests that optimization of experimental conditions is required.

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Quantitative analysis in field-flow fractionation using ultraviolet-visible detectors: an experimental design for absolute measurements

In previous works, it has been shown that a standard ultraviolet-visible detection system can be used for quantitative analysis of heterogeneous systems (dispersed supermicron particles) in field-flow fractionation (FFF) by single peak area measurements. Such an analysis method was shown to require either experimental measurements (standardless analysis) or an accurate model (absolute analysis) to determine the extinction efficiency of the particulate samples. In this work, an experimental design to assess absolute analysis in FFF through prediction of particles' optical extinction is presented. Prediction derives from the semiempirical approach by van de Hulst and Walstra. Special emphasis is given to the restriction of the experimental domain of instrumental conditions within which absolute analysis is allowed. Validation by statistical analysis and a practical application to real sample recovery studies are also given.

Journal Article↗

A new fast and standardless method for direct determination of metals associated with particulate matter in air: avoiding errors in the determination of Pb in an urban environment.

We describe a new method and the relevant instrumentation necessary for its implementation in the analysis of metals associated with particulate matter in air. The procedure can be divided into two steps: in the first step the sample is accumulated in a device through electrostatic precipitation whose center is a graphite tube; in the second step the graphite tube itself is used as an atomization device for the determination of the metals present in the sample through the electrothermal atomic absorption technique. The method is simple, fast, accurate, and inexpensive. Moreover, if the experimental conditions are well chosen, there is no need for calibration, which is very convenient in the case of samples such as particulate matter in the air. The elements that can be determined with the present apparatus are Hg, Cd, Tl, Ag, Mg, and Mn. These are highly or medium volatile because the materials used cannot reach very high temperatures for long periods. The experiments are confined to air, but other gases, in which a corona discharge is possible, would give the same results. With the method proposed, it was possible to show that the official method for Pb determination in the urban environment of Bologna presents a negative systematic error of about 25%.

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