Headspace SPME–GC Method for Acetone Analysis and its Biomedical Application

A new method for extraction and analysis of acetone in human urine based on headspace solid phase microextraction using a mixture of activated carbon and zeolite as sorbents in a PVC matrix coated on a silver wire and its application to the determination of ketone bodies is described. Unlike commercial fibers, which are coated on fused silica, the coating adheres strongly to the silver wire and is thermally stable up to 250 °C. After optimization of coating composition and microextraction conditions the fiber was used for the analysis of acetone in human urine.     

Joule-Thomson inversion curve prediction by using equation of state

In this paper five equations of state are tested for checking their ability to predict the Joule-Thomson inversion curve.These five equations of state are:Mohsennia-Modarres-Mansoori(MMM),Ji-Lemp(JL),modified Soave-Redlich-Kwang(SRK)equation of state by Graboski(MSRK1),modified SRK equation of state by Peneloux and Rauzy(MSRK2),and modified Peng-Robinson (PR)equation of state by Rauzy(PRmr).The investigated equations of state give good prediction of the low-temperature branch of the inversion curve,except for MMM equation of state.The high-temperature branch and the peak of the inversion curve have been observed,in general,to be sensitive to the applied equation of state.The values of the maximum inversion temperature and maximum inversion pressure are calculated for each component used in this work.     

Synthèse du mèthyl-1 diformyl-2,3 pyrrole,de la méthyl-1 pyrrolo[2,3-d] pyridazine et de la méthyl-1 oxo-6 (6h)cycloheptatrieno[b] pyrrole

This communication describes the synthesis of l-methyl-2,3-diformylpyrrole. This new compound is used to prepare a new heterocycle, l-methylcyclohepta[b]pyrrol-6-one and thus allows a new synthesis of l-methylpyrrolo[2,3-d]pyridazine.     

Semi-micro solvent extraction as a rapid and efficient preconcentration technique for the determination of n-alkanes in oil-contaiminated water and soil samples by capillary gas chromatography

Summary In this study, a rapid and efficient semi-micro extraction procedure is presented for the extraction of some higher n-alkanes from water and soil samples. In the case of water samples n-hexane was used as the organic phase in a phase volume ratio (volume of aqueous phase/volume of organic phase) higher than 285, while in the case of soil samples, extraction with n-hexane was carried out in the presence of an excess of 2 M NaCl solution. The extraction rate from soil samples is very high and is better than Soxhlet extraction, comparable with supercritical fluid extraction. High preconcentration factor in water samples allows the limits of detection to be in the ng.mL⁻¹ level with the use of gas chromatographic analysis. Flame ionization detector was used for monitoring the analytes. The obtained recoveries of all studied compounds from both water and soil samples are higher than 90%. This method was successfully used to determine some n-alkanes in municipal wastewater and contaminated soil.     

HPLC and GC Methods for Determination of Lubricants and Their Evaluation in Analysis of Real Samples of Polyethylene

High performance liquid chromatography (HPLC) and gas chromatography (GC) are introduced for analysis of polymer lubricants (stearamide, oleamide and erucamide). In the HPLC method, a reverse phase octadecylsilane (ODS) column along with acetonitrile/methanol (60:40) as a mobile phase were used. Detection of analytes was performed by a UV detector at 202 nm. The analysis time was less than 8 min. In the GC method, polar capillary column and flame ionization detector (FID) were used for separations and detection, respectively. The analysis time by GC was longer than HPLC and was about 30 min. Limits of detection, linear range and repeatability of both methods are similar, but determination of oleamide in real samples by HPLC method is difficult due to complexity of the initial part of HPLC chromatogram in polyethylene samples. That problem is not observed in the GC method. Detection limits in both methods for all analytes are lower than 0.003% which are much lower than the amount of lubricants in commercial polymers (0.05–0.2%).     

Hydration of short-chain poly(oxyethylene) in carbon tetrachloride: an infrared spectroscopic study

Hydration of short-chain poly(oxyethylene)s, CH(3)(OCH(2)CH(2))(m)OCH(3) (abbreviated as C(1)E(m)()C(1)) (m = 1-3), in carbon tetrachloride has been studied by infrared spectroscopy. The O-H stretching vibrations of water in ternary solutions with H(2)O:C(1)E(m)C(1):CCl(4) mole ratios of 0.000418:0.005:0.995 to 0.000403:0.04:0.96 were analyzed. Two types of hydrogen bonds are formed in the interaction between water and C(1)E(m)C(1) in carbon tetrachloride; one is a monodentate hydrogen bond, in which only one of the O-H bonds of a water molecule participates in hydrogen bonding, and the other is a bidentate hydrogen bond, in which both of the O-H bonds of a water molecule participate in hydrogen bonding by bridging oxygen atoms separated by two or more monomer units on the polymer chain. An important finding is that the bidentate hydrogen-bond bridge is not formed between the nearest-neighbor oxygen atoms. This experimental observation supports the results of previous molecular dynamics simulations. The shortest oligomer of poly(oxyethylene), i.e., CH(3)OCH(2)CH(2)OCH(3) (1,2-dimethoxyethane) with a single monomer unit, is suggested not to be an adequate model for this polymer with respect to hydrogen bonding to water. The hydrogen bonding in a 1:1 C(1)E(m)C(1)-water adduct in carbon tetrachloride represents primitive incipient hydration of poly(oxyethylene). The present results indicate that both monodentate and bidentate hydrogen bonds are important and the latter is destabilized more rapidly than the former with increasing temperature. This dehydration process can be a potential mechanism of the poly(oxyethylene)-water phase separation.     

Ketoconazol‐Triiodide Ion Pair Complex as a Suitable Carrier in an Iodide Selective Membrane Electrode

A novel membrane sensor for selective monitoring of iodide, consisting of a triiodide‐ketoconazole ion pair complex dispersed in a PVC matrix, plasticized with a mixture of 2‐nitrophenyl octyl ether and dioctylphtalate with unique selectivity toward iodide ions, is described. The influence of membrane composition, pH of test solution and foreign ions on the electrode performance were investigated. The optimized membrane demonstrates a near‐Nernstian response for iodide ions over a wide linear range from 1.0 × 10^?2 to 1.0 × 10^?5 M, at 25 ± 1 °C. The electrode could be used over a wide pH range 3–10 and has the advantages of high selectivity, fast response time and good lifetime (over 4 months). It was successfully used as indicator electrode in potentiometric titrations and direct potentiometric assay of iodide ions.     

Different PES nanofibrous membrane parameters effect on the efficacy of immunoassay performance

The contribution of electrospun nanofibrous membranes (e.NFMs) in the biosensing platforms opens up a new prospect for the invention of faster and more sensitive analytical devices. In this paper, we utilized e.NFM of polyethersulfone (PES) as a solid substrate for the protein immobilization through two different approaches: physical and covalent. Scanning electron microscopy (SEM) and Fourier‐transform‐infrared (FTIR) tests were performed to study the effect of plasma treatment on protein immobilization efficacy. Moreover, taking advantage of ELISA technique, the influence of different parameters, namely, nanofibers diameter, membrane thickness, plasma treatment time, an incubation time of ethyl‐3‐(3‐dimethylaminopropyl)‐carbodiimide/N‐hydroxysuccinimide (EDC/NHS), and their ratio on antibody immobilization efficacy through two mentioned approaches, was also assessed.