Effect of an admixture on the electrical and thermal properties of triglycine sulphate crystals

The influence of chloroacetic acid amide (AC) on the temperature-dependence of the electrical conductivity (), thermal expansion (_ij) and specific heat ((C _p) of triglycine sulphate crystals was studied in the phase transition range (T _c=49°). The addition of isostructural AC increased the electrical conductivity, decreased the thermal expansion and changed theC _p peak. The mechanism is discussed on a thermodynamic basis.

---

Zusammenfassung Der Einfluß der Zumischung von Chloressigsäureamid (AC) auf die Temperaturabhängigkeit der elektrischen Leitfähigkeit, der Wärmeausdehnung _ij und der spezifischen WärmeC _p von Triglycinsulfat-Kristallen wurde im Phasenübergangsgebiet (T _c=49 °C) untersucht. Die Beimischung von isostrukturellem AC erhöht die elektrische Leitfähigkeit und vermindert die Wärmeleitfähigkeit, während derC _p-Peak verändert wird. Der Mechanismus kann thermodynamisch diskutiert werden.

---

(), () _ij) () , T _c=49°. , , , , C _p. .

     

Reactivity of indolizines in organic synthesis

This review reports the reactivity of indolizines. The reactions section covers, in general, electrophilic, oxidation, reduction, addition, cycloaddition, condensation, and Mannich and multicomponent reactions. The synthesis of bis-indolizines and cyclazines are reported. The reaction mechanisms are discussed.     

A highly sensitive and specific polyclonal antibody-based enzyme immunoassay for therapeutic monitoring and pharmacokinetic studies of atorvastatin

This study describes the development and validation of a highly sensitive and specific enzyme immunoassay (EIA) for therapeutic monitoring and pharmacokinetic studies of atorvastatin (ATR). The assay employs a polyclonal antibody that recognizes ATR with high specificity and affinity, and ATR conjugated to bovine serum albumin (ATR-BSA) immobilized onto microwell plates as a solid phase. The assay involved a competitive binding reaction between ATR and the immobilized ATR-BSA for the binding sites on a limiting amount of the anti-ATR antibody. The bound anti-ATR antibody was quantified with horseradish peroxidase-labeled anti-immunoglobulin secondary antibody and 3,3′,5,5′-tetramethylbenzidine as a substrate for the peroxidase enzyme. The concentration of ATR in the sample was quantified by its ability to inhibit the binding of the anti-ATR antibody to the immobilized ATR-BSA and subsequent color development in the assay wells. The conditions for the EIA were investigated and optimized for the determination of ATR in plasma samples. The limit of detection was 0.04 ng mL^?1 and the effective working range at relative standard deviations (RSD) of ≤5% was 0.1–10 ng mL^?1. Mean analytical recovery of ATR from spiked plasma was 99.3?±?2.8%. The precision of the assay was satisfactory; RSD were 2.7–4.6 and 3.3–5.7% for intra- and inter-assay precision, respectively. The reliability of the EIA was confirmed by HPLC. The EIA is convenient, and one can analyze ～ 200 samples per working day, facilitating the processing of large-number of samples of ATR.     

Phase-selective a.c. adsorptive stripping voltammetry of lumazine on a hanging mercury drop electrode

The electrochemical behavior of lumazine (LMZ), an important antibacterial agent, has been studied at the hanging mercury drop electrode (HMDE). The nature of the process taking place at the HMDE was clarified. Its adsorption behavior at HMDE has been studied by using a.c and cyclic voltammetry (CV). Both the molecule and its reduced product appeared to be adsorbed at the surface of the electrode. Controlled adsorptive accumulation of LMZ on the HMDE provides the basis for the direct stripping measurement of that compound in the subnanomolar concentration level. Experimental and instrumental parameters for the quantitative determination were optimized. Phase-selective a.c voltammetry provided the best signal and gave a detection limit of 0.15 microg L(-1) (9.0 x 10(-10) mol/L) LMZ in aqueous solution. Molecules or ions which may interfere were studied.     

Catalytic activity of a zirconium(IV) oxide surface supported with transition metal ions

The kinetics of H₂O₂ decomposition have been investigated using ZrO₂ supported with transition metal ions including Cu^II, Ag^I, Hg^II, Co^II, Mn^II, Ni^II and Fe^III. At pH = 6.8, the reaction rate exhibits a first order dependence on the initial H₂O₂ concentration at low concentrations. The order of activity of the different catalysts is strongly dependent on the [H₂O₂]₀ used. The reaction proceed via the formation of the peroxo-intermediate which has an inhibiting effect on the reaction rate. The rate increases with increasing pH, and attains a limiting rate at higher pH's. A reaction mechanism is proposed involving liberation of HO₂ radicals from the peroxo-intermediate as the rate-determining step.     

Imide and anhydride bridged organoiron dinuclear homo and hetero dichalcogeno carboxylate complexes [CpFe(CO)2ECO(C6H4)CO]2NH and [CpFe(CO)2ECO(C6H4)CO]2O; E = S,Se

Organoiron thio- and seleno-terephthaloyl chloride complexes CpFe(CO)₂ECO(C₆H₄)COCl (E = S and Se) react with NaOH and NaNH₂ to give quantitative yields of the acid Cp(CO)₂ECO(C₆H₄)CO₂H and the amide CpFe(CO)₂ECO(C₆H₄)CONH₂ respectively. These amide and acid derivatives react with the terephthaloyl chloride complexes to give a new series of imide-bridged [CpFe(CO)₂ECO(C₆H₄)CO]₂NH and anhydride-bridged [CpFe(CO)₂ECO(C₆H₄)CO]₂O organoiron dinuclear homo and hetero dichalcogeno terephthalate complexes. The complexes were characterized by elemental analysis, i.r. and ¹H-n.m.r. spectra. This revised version was published online in June 2006 with corrections to the Cover Date.     

Fatty amides synthesized from vegetable oil as extractant of molybdenum(VI)

In this study, fatty amides (FAs) synthesized from palm olein were used to extract and separate Mo(VI) from acidic media. Effects of various parameters upon the separation of Mo(VI) from Co(II), Ni(II), Al(III) and Mn(II), including extractant concentration, metal ion concentration, contact time, diluent, and acidity, were investigated. It was found that Mo(VI) was successfully separated from the above commonly associated metal ions by stripping from the loaded organic phase. Different acidic and alkaline solutions were used. Ammonium hydroxide solution was an optimal. Extraction of Mo(VI) into the organic phase involved the formation of 1:3 complexes. This work presents the development of a low-cost and environmentally friendly extractant to recycle and recover molybdenum.     

Determination of neutron flux parameters in PUSPATI TRIGA Mark II Research Reactor, Malaysia

In standardization NAA, it is necessary to characterize the neutron spectrum parameters such as epithermal neutron flux shape factor (α), thermal to epithermal neutron flux ratio (f), thermal neutron flux (φ _th) and epithermal neutron flux (φ _epi) in the irradiation facility to determine the concentration of an element in the sample using absolute and k ₀ standardization methods. The α and f were determined using Cd-ratio multi monitor method using experimental data obtained in PUSPATI TRIGA Mark II research reactor at four irradiation positions (10, 20, 30 and 40) of the rotary rack. The calculated values of α and f ranged from 0.006 to 0.0281 and 18.56 to 19.12 respectively. The average values of φ _th and φ _epi were found as 2.33 × 10¹² and 1.23 × 10¹¹ n cm^?2 s^?1 respectively. Moreover, a comparison of the neutron flux parameters in the present study shows an acceptable level of consistency with those of previous studies.     

A simple microextraction and preconcentration approach based on a mixed matrix membrane

A simple adsorption/desorption procedure using a mixed matrix membrane (MMM) as extraction medium is demonstrated as a new miniaturized sample pretreatment and preconcentration technique. Reversed-phase particles namely polymeric bonded octadecyl (C₁₈) was incorporated through dispersion in a cellulose triacetate (CTA) polymer matrix to form a C₁₈-MMM. Non-steroidal anti-inflammatory drugs (NSAIDs) namely diclofenac, mefenamic acid and ibuprofen present in the environmental water samples were selected as targeted model analytes. The extraction setup is simple by dipping a small piece of C₁₈-MMM (7 mm × 7 mm) in a stirred 10 mL sample solution for analyte adsorption process. The entrapped analyte within the membrane was then desorbed into 100 μL of methanol by ultrasonication prior to high performance liquid chromatography (HPLC) analysis. Each membrane was discarded after single use to avoid any analyte carry-over effect. Several important parameters, such as effect of sample pH, salting-out effect, sample volume, extraction time, desorption solvent and desorption time were comprehensively optimized. The C₁₈-MMM demonstrated high affinity for NSAIDs spiked in tap and river water with relative recoveries ranging from 92 to 100% and good reproducibility with relative standard deviations between 1.1 and 5.5% (n = 9). The overall results obtained were found comparable against conventional solid phase extraction (SPE) using cartridge packed with identical C₁₈ adsorbent.     

Synthesis and spectroscopic characterization of indomethacin-Cd(II), Ce(III), and Th(IV) complexes: IR, 1H NMR,thermal, and biological studies

Solid complexes have been prepared and characterized by IR, UV-Vis, elemental analysis, and ¹H NMR. Indomethacin forms complexes with Cd(II), Ce(III), and Th(IV) ions in molar ratios (ligand: metal) (2: 1), (3: 1), and (4: 1), respectively. The IR spectra of the complexes suggest that the Indomethacin behaves as a monobasic monodentate ligand coordinated to the metal ions via the deprotonated carboxylate group. Prepared complexes exhibit higher antimicrobial activity against several microorganisms, compared to free ligand.