Photoconductivity and photoluminescence in chemically deposited films of (Cd0.95-Pb0.05)S: CdCl2,Ce

The results of photoconductivity (PC), photoluminescence (PL), optical absorption spectra, XRD and SEM studies are presented for (Cd_0.95-Pb_0.05)S: CdCl₂,Ce films prepared by chemical bath deposition technique. PC gains ∼10⁷ are found in doped films. PL emission spectrum is found in red region which is related to 5d to 4f transition in Ce. Films prepared at 60°C show better PC while those prepared at room temperature (RT) show better PL. Optical absorption studies show reduction in band gap due to addition of PbS. A peak due to Ce is also observed in absorption spectrum. XRD studies show the presence of both CdS and PbS. SEM studies show presence of microcrystals, cluster of grains along with some rod type structures.     

Analysis of multicomponent mixture and simultaneous enantioresolution of proteinogenic and non-proteinogenic amino acids by reversed-phase high-performance liquid chromatography using chiral variants of Sanger’s reagent

Four chiral derivatizing reagents (CDR 1–4), namely, FDNP-l-Ala, FDNP-l-Val, FDNP-l-Phe, and FDNP-l-Leu, were synthesized using microwave (MW) irradiation by substituting one of the fluorine atoms in difluoro dinitro benzene (DFDNB) with l-Ala, l-Val, l-Phe, and l-Leu (CDR 1–4). The other set of CDRs, namely, FDNP-l-Phe-NH₂, FDNP-l-Val-NH₂, and FDNP-l-Leu-NH₂, was also prepared. These reagents were used for synthesis of diastereomers of 18 proteinogenic and 08 non-proteinogenic amino acids, which were resolved by reversed-phase high-performance liquid chromatography using C18 column and gradient eluting mixture of aq.TFA and acetonitrile with UV detection at 340 nm. The reagents were used for resolution of a complex mixture of 18 racemic proteinogenic amino acids in a single chromatographic run of 65 min and to determine concentration of the d-amino acid in a solution of dl-amino acid. The resolution (R _S) and selectivity (α) obtained for the two sets of diastereomers were compared among themselves and among the two groups. The method was validated for accuracy, precision, limit of detection (LOD), and limit of quantification. LOD is 0.001% impurity of d-enantiomer.     

Paper electrophoretic determination of the stability constants of binary and ternary complexes of copper(II) and cobalt(II) with nitrilotriacetate and cysteine

A paper ionophoretic method is described for the study of equilibria in mixed ligand (nitrilotriacetate-cysteine) complex system in solution. The proportion of ionic species of nitrilotriacetate (NTA) and cysteine were varied by changing the pH of background electrolyte. The stability constants of Cu(II)-NTA-cysteine and Co(II)-NTA-cysteine complexes were found to be 6.35+/-0.05 and 5.45+/-0.02 (logarithm stability constant values), respectively, at ionic strength 0.1 M and a temperature of 35 degrees C.     

Tandem SN2-Michael addition to vinylogous carbonates for the stereoselective construction of 2,3,3,5-tetrasubstituted tetrahydrofurans

A stereoselective method for the synthesis of substituted tetrahydrofuran derivatives employing a tandem alkylation-Michael addition sequence to vinylogous carbonates is developed. The method could be used to synthesize THFs bearing tertiary ethers. Further, the method is extended to the synthesis of adjacent bis-THFs.     

Alkylphosphonate modified aluminum oxide surfaces

The surface properties of aluminum, such as chemical composition, roughness, friction, adhesion, and wear, can play an important role in the performance of micro-/nano-electromechanical systems, e.g., digital micromirror devices. Aluminum substrates chemically reacted with octadecylphosphonic acid (ODP/Al), decylphosphonic acid (DP/Al), and octylphosphonic acid (OP/Al) have been investigated and characterized by X-ray photoelectron spectroscopy (XPS), contact angle measurements, and atomic force microscopy (AFM). XPS analysis confirmed the presence of alkylphosphonate molecules on ODP/Al, DP/Al, and OP/Al. No phosphonates were found on bare Al as a control. The sessile drop static contact angle of pure water on ODP/Al and DP/Al was typically more than 115 degrees and on OP/Al typically less than 105 degrees indicating that all phosphonic acid reacted Al samples were highly hydrophobic. The root-mean-square surface roughness for ODP/Al, DP/Al, OP/Al, and bare Al was less than 15 nm as determined by AFM. The surface energy for ODP/Al and DP/Al was determined to be approximately 21 and 22 mJ/m2, respectively, by the Zisman plot method, compared to 25 mJ/m2 for OP/Al. ODP/Al and OP/Al were studied by friction force microscopy, a derivative of AFM, to better understand their micro-/nano-tribological properties. ODP/Al gave the lowest coefficient of friction values while bare Al gave the highest. The adhesion forces for ODP/Al and OP/Al were comparable.     

Direct TLC Resolution of (±)-Ketamine and (±)-Lisinopril by Use of (+)-Tartaric Acid or (−)-Mandelic Acid as Impregnating Reagents or Mobile Phase Additives. Isolation of the Enantiomers

Direct resolution of the enantiomers of the racemic drugs ketamine and lisinopril has been achieved by TLC. Enantiomerically pure tartaric acid and mandelic acid were used as chiral impregnating reagents and as mobile phase additives. When (−)-mandelic acid was used as chiral impregnating reagent use of ethyl acetate–methanol–water 3:1:1 (v/v) as mobile phase enabled successful resolution of the enantiomers of both compounds. For lisinopril, the mobile phase acetonitrile–methanol–water–dichloromethane 7:1:1:0.5 (v/v) was successful when (+)-tartaric acid was used as impregnating agent. When (+)-tartaric acid was used as mobile phase additive the mobile phase acetonitrile–methanol–(+)-tartaric acid (0.5% in water, pH 5)–glacial acetic acid 7:1:1.1:0.7 (v/v) enabled successful resolution of the enantiomers of lisinopril. The effects on resolution of temperature, pH, and the amount of chiral selector were also studied. The separated enantiomers were isolated and identified. Spots were detected with iodine vapour. LODs were 0.25 and 0.27 μg for each enantiomer of ketamine with (+)-tartaric acid and (−)-mandelic acid, respectively, whereas for lisinopril LODs were 0.14 and 0.16 μg for each enantiomer with (+)-tartaric acid (both conditions) and (−)-mandelic acid, respectively.

     

Triazolo[4′,3′:4,5] [1,3,4]thiadiazolo[2,3-b]quinazolin-6-one

3-Methyl-6H-[1,2,4]triazolo[4′,3′: 4,5] [1,3,4]thiadiazolo[2,3-b]quinazolin-6-one (6) has been synthesized by the condensation of isatoic anhydride (1) with 4-amino-5-mercapto-3-methyl-[1,2,4]triazole (2) and final cyclisation of the intermediate3 with POCl₃ and PCl₃. Alternatively6 could also be synthesized by the condensation of 3-amino-2-mercapto-3H-quinazolin-4-one (7) withN-carbethoxy hydrazine in presence of hydrochloric acid and final cyclisation of the intermediate8 with acetic acid. The structures have been confirmed on the basis of IR, PMR and analytical results.     

On dominant operators

This paper is devoted to the study of dominant operators with an emphasis on their spectral properties. In particular the equation (T–)f() x (T a dominant or hyponormal operator on the Hilbert space ,x andf a function from the open setU to ) is investigated in an effort to discover necessary and/or sufficient conditions for the analyticity off.Supported in part by the National Science Foundation.     

3-Methyl[1,3,4]thiadiazino[2,3-b]quinazolin-6-ones

4H,6H-[1,3,4]Thiadiazino[2,3-b]quinazolin-6-one with a methyl group in position 3 (6a) has been synthesised by the condensation of 3-amino-2-mercapto-3H-quinazolin-4-one (1) with allyl bromide (2) followed by treatment with bromine and subsequent dehydrohalogenation of the brominated product (4) with ethanolic sodium hydroxide. Its isomeric 3-methyl-2H,6H-[1,3,4]thiadiazino[2,3-b]quinazolin-6-one (6b) has also been obtained by condensation of1 and bromoacetone (7) followed by cyclisation of the intermediates (8 or9) with hydrobromic acid or with concentrated sulphuric acid. The structures have been established on the basis of IR and PMR data.

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3-Methyl[1,3,4]thiadiazino[2,3-b]chinazolin-6-one

Zusammenfassung Zur Synthese von 4H,6H-[1,3,4]thiadiazino[2,3-b]chinazolin-6-on (6a) wurde die Kondensation von 3-Amino-2-mercapto-3H-chinazolin-4-on (1) mit Allylbromid mit nachfolgender Behandlung mit Brom und Dehydrohalogenierung des bromierten Produktes4 mit ethanolischer Natronlauge herangezogen. Das zu6a isomere 2H,6H-Produkt6b wurde ebenfalls durch Kondensation von1 mit Bromaceton und nachfolgender Cyclisierung der Zwischenprodukte8 bzw.9 mit HBr oder H₂SO₄ erhalten. Die Strukturen wurden mittels IR und NMR abgesichert.