Speciation of Se,Fe and Zn in Human Milk Whey: The use of Instrumental Neutron Activation Analysis (INAA) to corroborate element profiles measured with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

In human milk trace elements normally exist in a form which can easily be absorbed by the newborn infant. For investigations of the bioavailability of trace elements it is necessary to carry out a speciation analysis of the elements of interest. An independent analytical method has been used for the quality control of the shape of the element profiles obtained from the speciation analysis of Se, Fe and Zn in individual samples of human milk whey after chromatographic separation. For the element detection in the untreated milk fractions Instrumental Neutron Activation Analysis (INAA) was chosen as the reference method. Element distribution patterns have been obtained with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) using on-line digestion of the fraction, reduction and hydride formation of Se ("T"-mode). Prior results are compared with those obtained by means of element detection in the untreated fractions ("U"-mode) with ICP-AES. The elution profiles of Se, Fe and Zn in human milk whey obtained by means of ICP-AES detection using the "T"-mode show good agreement with the distribution patterns obtained with INAA. Recoveries of 103% for Fe, 86% for Zn and 87% for Se were obtained. The element distribution patterns of Fe and Zn obtained with ICP-AES speciation using the "T"-mode also show good agreement with those obtained by means of ICP-AES using the "U"-mode.     

Electronic properties of aluminum clusters compared with the jellium model

The experimental polarizabilities, ionization potentials and electron affinities of aluminum clusters are compared with jellium predictions. It is found that the clusters have radii and work functions which are close to the jellium model predictions for clusters with more than 13 atoms. The polarizabilities of Al _n correspond with the jellium only forn>40 and the shell structure features in the ionization potentials are anomalous up to 37. We conclude that nonjellium effects are important up ton=40.     

PoraPLOT Q: A porous layer open tubular column coated with styrene-divinylbenzene copolymer

A porous polymer is deposited on the inner wall of fused silica capillary columns. The retention characteristics of this porous polymer were evaluated and found to be comparable with Porapak Q. The porous polymer has a high retention volume which enables the separation of permanent gases at ambient temperatures or higher. The hydrophobic character of the porous polymer allows the injection of water containing samples without changing retention due to adsorption of water. The inertness of the porous polymer allows the elution of a range of apolar and polar compounds. The maximum temperature of the porous polymer was estimated to be 250°C. With this new type of capillary column, high resolution separations are obtained in combination with short analysis times.     

Synthesis and characterization of MCM-48 tubular membranes

MCM-48 membranes have been prepared on alumina supports of different pore sizes. A battery of characterization techniques has been used to study the physical properties and the quality of the membranes prepared. The highest quality membranes were prepared on supports with pore size of up to 60 nm. The MCM-48 membranes were tested in the separation of gas phase mixtures and a cyclohexane/O₂ selectivity higher than 270 was obtained. The selective separation of organic compounds from inert components is a result of the cooperative effects of capillary condensation in MCM-48 pores and of the specific interactions of the permeating compounds and the membrane material.     

Racemic ofloxacin separation by supported-liquid membrane extraction with two organic phases

As the relation of chirality and activities of drugs is researched deeply, people become to re-alize the clinic importance of chirality. The different enantiomers of a drug can have vastly differ-ent pharmacological activities, pharmacokinetic processes and toxicity[1,2]. The most well-docu- mented example is that of the drug substance thalidomide. Bitter lessons and scientific research promote the interest in single-enantiomer drugs, so the potential of the chiral drug market is enormous[3]. …     

Evaluation of the efficiency of extraction of PAHs from diesel particulate matter with pressurized solvents

Pressurized Fluid Extraction (PFE) was evaluated for the extraction of polycyclic aromatic hydrocarbons (PAHs) and nitro-derivatives from diesel particulate matter. Extraction conditions were set up by performing several tests in which temperature, solvent strength, pressure, and static time were gradually increased. The results obtained on a laboratory test material made of a "lean" (low content of soluble fraction) Diesel particulate matter indicate that very severe conditions were needed in order to obtain better recoveries of the higher molecular weight molecules. Moreover, extraction efficiency seems to be influenced by the amount of soluble matter in the particulate, so that a "lean" particulate appears more difficult to extract. Recoveries of the deuterated standards of certain PAHs (i.e. indeno[1,2,3- cd]pyrene) were incomplete even with the toughest conditions tested. Experiments carried out on a certified material (SRM 1650 from NIST) also indicate that PFE can perform a better extraction of some of the PAHs than the method used for certification, but still incomplete. Comparison of results obtained on the SRM with different extraction techniques suggests that the composition of the extract varies considerably with the extraction technique and conditions. It is relevant to notice that recent Diesel engines produce leaner particulate: for future materials more drastic extraction conditions will be required.     

A Highly Sensitive and Selective Assay for Cysteine Using the Chemiluminescence Reaction of Luminol and Hydrogen Peroxide

A very simple, highly sensitive and selective chemiluminescence (CL) method was established for the determination of cysteine. This method is based on the fact that the CL reaction of luminol and hydrogen peroxide can be greatly enhanced by cysteine. The CL intensities at maximum light emission were linearly correlated with the concentration of cysteine over the range of 2.0×10^–8–6.0×10^–6molL^–1 with a detection limit of 7.5×10^–9molL^–1. The relative standard deviation was 1.7% for the determination of 1.0×10^–7molL^–1 cysteine (n=9). The feasibility of utilizing the proposed method for the determination of total concentration of cysteine in human serum was examined.     

Thermogravimetric study of some crosslinked copolymers based on poly(acrylonitrile-co-divinylbenzene)

Copolymer networks based on acrylonitrile (AN)/divinylbenzene (DVB) have been investigated by thermogravimetric analysis (TG) to evaluate their thermal stability in nitrogen atmosphere. Thermal stability was determined from TG-DTG curves to investigate the influence of AN and DVB in the synthesis of copolymers on the copolymer thermal properties. The TG and DTG curves of copolymers clearly show two thermodegradation stages. The solid residues produced after thermodegradation stages were analyzed by FTIR and elemental analysis (CHN). The decomposition temperatures were dependent on amount of AN and DVB used as the crosslinking agent. The degradation temperatures of copolymers were influenced by the diluent system during their synthesis. FTIR analyses indicate that the cyclization of the polymer proceeds before any mass loss.