Structural,morphological and mechanical properties of niobium nitride thin films grown by ion and electron beams emanated from plasma

The influence of variation in plasma deposition parameters on the structural, morphological and mechanical characteristics of the niobium nitride films grown by plasma-emanated ion and electron beams are investigated. Crystallographic investigation made by X-ray diffractometer shows that the film synthesized at 10?cm axial distance with 15 plasma focus shots (PFS) exhibits better crystallinity when compared to the other deposition conditions. Morphological analysis made by scanning electron microscope reveals a definite granular pattern composed of homogeneously distributed nano-spheroids grown as clustered particles for the film synthesized at 10?cm axial distance for 15 PFS. Roughness analysis demonstrates higher rms roughness for the films synthesized at shorter axial distance and by greater number of PFS. Maximum niobium atomic percentage (35.8) and maximum average hardness (19.4?±?0.4?GPa) characterized by energy-dispersive spectroscopy and nano-hardness analyzer respectively are observed for film synthesized at 10?cm axial distance with 15 PFS.     

Synthesis of Some New Benzopyranopyrimidin-2-Thiol Derivatives

Reaction of 2-mercapto-4-hydroxy-5H-[1]-benzopyrano-[4,3- d ]-pyrimidin-5-one ( 3 ) with phenyl isothiocyanate and methyl acrylate yielded the corresponding 2-(substituted)thio-4-hydroxy-5H-[1]-benzopyrano-[4,3- d ]-pyrimidin-5-ones ( 4 , 5 ). Hydrolysis and hydrazinolysis of 5 gave acid derivative 6 , and hydrazone 7 . Treatment of hydrazone 7 with ethyl acetoacetate, diethyl malonate, and phenyl isothiocyanate yielded the corresponding 2-(substituted)thio-4-hydroxy-5H-[1]-benzopyrano- [4,3- d ]-pyrimidin-5-ones ( 8 , 9 , and 11 ). Cyclization of 11 with 2 N NaOH led to 12 .     

SYNTHESIS OF SPIRO [1,3-BENZODIOXOLE-2,4′-(3′H) QUINAZOLINES]

Abstract

In the present investigation, the authors could obtain a new series of spiranes (1) through the reaction of the high potential quinone tetrachloro-o-benzoquinone with 2-aryl-3-phenyl-3H-quinazoline-4-thiones. Thus, 2,3-diphenyl- (2a), 2-p-tolyl-3-phenyl- (2b) and 2-p-anisyl-3-phenyl- (2c)-3H-quinazoline-4-thiones react readily with tetrachloro-o-benzoquinone, in boiling toluene, to give the corresponding spiro-1,3-benzodioxole-2,4′-(3′H)-quinazolines (1a-c), respectively.     

SYNTHESIS AND BIOLOGICAL ACTIVITY OF SOME NEW 8-HYDROXYQUINOLINE SULPHONAMIDE DERIVATIVES

Abstract

Some new derivatives containing both 8-hydroxyquinoline and sulphonylamino β-lactams and thiazolidinones have been prepared. These compounds were synthesized from the corresponding 8-hydroxyquinoline sulphonylhydrazide (1) by converting it to hydrazones (2). The latter hydrazones (2) were easily transformed to β-lactams (3) and thiazolidinones (4) by cyclocondensation reaction with chloroacetyl chloride and/or mercaptoacetic acid. Some metal chelates with Fe³⁺. Co²⁺+, Ni²⁺, Cu²⁺ and Cd²⁺ have been prepared for some of the compounds and screened in vitro for their biological activity.     

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.     

Mixed-Isotope Labeling with LC-IMS-MS for Characterization of Protein–Protein Interactions by Chemical Cross-Linking

Chemical cross-linking of proteins followed by proteolysis and mass spectrometric analysis of the resulting cross-linked peptides provides powerful insight into the quaternary structure of protein complexes. Mixed-isotope cross-linking (a method for distinguishing intermolecular cross-links) was coupled with liquid chromatography, ion mobility spectrometry and mass spectrometry (LC-IMS-MS) to provide an additional separation dimension to the traditional cross-linking approach. This method produced multiplet m/z peaks that are aligned in the IMS drift time dimension and serve as signatures of intermolecular cross-linked peptides. We developed an informatics tool to use the amino acid sequence information inherent in the multiplet spacing for accurate identification of the cross-linked peptides. Because of the separation of cross-linked and non-cross-linked peptides in drift time, our LC-IMS-MS approach was able to confidently detect more intermolecular cross-linked peptides than LC-MS alone.      

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.