Synthesis of cross linked platinum metal containing polyyne polymers

Reaction of Pt(PⁿBu₃)₂Cl₂ (1) or Pt(AsⁿBu₃₂Cl₂ (2) with stoichiometric amounts of 1,3,5-triethynylbenzene, [1,3,5-(H? C?C? )₃C₆H₃] (3)yields monomeric, [1,3,5-Cl(PⁿBu₃)₂(Pt? C? C? )₃C₆H₃] (4), [1,3,5-(C1)(AsⁿBu₃)₂Pt? C? C? ₃C₆H₃] (5) or polymeric, {1,3,5-[(PⁿBu₃)₂Pt? C?C? ]₃C₆H₃? )ⁿ (6), {1,3,5-[(AsⁿBu₃)₂Pt? C? C? ]₃C₆H₃? }ⁿ (7) complexes. Treatment of (1) with (3) and 2,5-diethynyl-p-xylene,H? C? C? C₆H₂(CH₃)₂? C? C? H (8) in varying molar ratios yields a series of high molecular weight cross linked platinum metal containing polyyne copolymers.     

Synthesis, physico-chemical and thermal characteristics of seven and ten coordinated complexes of trivalent lanthanides derived from 4[N-(cinnamalidene)amino]antipyrine semicarbazone and diphenyl sulfoxide

In present studies a new series of twenty four complexes of seven and ten coordinated compounds derived from 4[Ncinnamalidene) amino]antipyrine semicarbazone (CAAPS) as primary ligand and diphenyl sulfoxide (DPSO) as secondary ligand has been reported. All the complexes have the general composition LnX_3.n(CAAPS).DPSO (Ln = La, Pr, Nd, Sm, Gd, Tb, Dy or Ho, X = NCS or ClO₄, n = 2, X = NO₃, n = 1). The compounds have been characterized by elemental analysis, molar conductance, magnetic susceptibility, infrared and electronic spectra. Thermal characteristics were also reported. Based on the data appropriate structures are assigned for these complexes.     

Study of the excited 0+ states through conversion electron spectroscopy of neutron rich Zr and Mo fission products

A windowless Si(Li) electron detector has been used in conjunction with the gas filled fission product separator JOSEF to study totally converted transitions in Zr and Mo isotopes. The existence of twoβ-decay modes in⁹⁶Y,⁹⁸Y and¹⁰⁰Nb is confirmed. The half-lives of theβ-decaying levels feeding O ₂ ⁺ states in⁹⁶Zr and⁹⁸Zr are 6.0 ± 0.4 sec and 0.60±0.05 sec respectively. A search for other first excited O ₂ ⁺ states shows that no such states are apparent in¹⁰⁰Zr and¹⁰⁴Mo.     

Kinetic evidence for the occurrence of kinetically detectable intermediates in the cleavage of N‐ethoxycarbonylphthalimide under N‐methylhydroxylamine buffers

The kinetics of the aqueous cleavage of N‐ethoxycarbonylphthalimide (NCPH) in CH₃NHOH buffers of different pH reveals that the cleavage follows the general irreversible consecutive reaction path NCPH ENMBC A B , where ENMBC, A , and B represent ethyl N‐[o‐(N‐methyl‐N‐hydroxycarbamoyl)benzoyl]carbamate, N‐hydroxyl group cyclized product of ENMBC, and o ‐(N‐methyl‐N‐hydroxycarbamoyl)benzoic acid, respectively. The rate constant k_{1 obs} at a constant pH, obeys the relationship k_{1 obs} = k_w + k_n^app [Am]_T + k_b[Am]_T², where [Am]_T is the total concentration of CH₃NHOH buffer and k_w is first‐order rate constant for pH‐independent hydrolysis of NCPH. Buffer‐dependent rate constant k_b shows the presence of both general base and general acid catalysis. Both the rate constants k_{2 obs} and k_{3 obs} are independent of [Am]_T (within the [Am]_T range of present study) at a constant pH and increase linearly with the increase in a_OH with definite intercepts. © 2001 John Wiley & Sons, Inc. Int J Chem Kinet 34: 95–103, 2002     

Characterization of methyl methacrylate grafting onto preirradiated biodegradable lignocellulose fiber by gamma-radiation

Gamma-radiation-induced graft copolymerization of methyl methacrylate onto natural lignocellulose (jute) fiber was carried out by the preirradiation method in an aqueous medium by using octylphenoxy-polyethoxyethanol as an emulsifier. The different factors that influenced the graft copolymer reaction process were investigated. In the case of radiation-dose-dependent grafting, samples irradiated in the presence of air produced up to 73% graft weight compared to 53% obtained in the case of irradiation in a nitrogen environment. By assuming Arrhenius reaction kinetics, the activation energy (E(a)) of the grafting reaction process was evaluated for different reaction temperatures. Moreover, the graft copolymer reaction was controlled by incorporating a homopolymer-inhibiting agent and three different chain-transfer agents in the reaction medium. The mechanical and thermal properties of jute fiber 'as received' and jute-graft-poly(methyl methacrylate) were also investigated. The results showed that the percentage of grafting with jute fiber has a significant effect on the properties. The kinetic parameters were evaluated from TGA thermograms by using Broido's method in the temperature range 240-350 degrees C. Scanning electron micrographs show that the structural changes on the surface of jute fibers were induced by graft copolymerization of methyl methacrylate monomer. Fiber-fiber surface friction was measured in terms of the average maximum load and the kinetic friction. SEM of jute-graft-poly(methyl methacrylate).     

Determination of Furosemide by Simple Diazotization Method in Pharmaceutical Preparations

A simple and rapid spectrophotometric method has been investigated for the determination of furosemide. The method is based upon simple diazotization reaction. The absorbance was measured at 480 nm. The method is optimized for acidity, amount of reagents required and heating time. The range of linearity was 0.4–10 μg mL^?1 of furosemide with molar absorptivity of 1.0 × 10⁴ l mol^?1 cm^?1. Standard deviation, coefficient of variance, limit of detection and limit of quantification were calculated using authentic standard of furosemide and were found to ± 0.0013,12.7%, 0.16 ppm and 0.52 ppm, respectively. The method was applied to various pharmaceutical preparations containing furosemide. The results of the investigated method for furosemide were compared with available official literature method. The results obtained by the proposed method agree well with the standard established method.     

Iodine binding by amylopectin and stability of the amylopectin–iodine complex

The iodine binding capacity (IBC) of amylopectin (AP, from potatoes) is determined to be around 0.38% (w/w) of the total AP in the solution. The mass of iodine bound comprises about 13.6% of the mass of AP involved with the complex, suggesting that with every four iodine atoms bound there are 23 anhydroglucose residues (AGU). Since our previous study indicates that four iodine atoms within the helix of 11 AGUs form a chromophore unit in the API complex, only 48% of the AGUs (11 out of 23) in the AP molecule are directly involved with the iodine. The heat of reaction for the API complex formation is determined to be around ?47 kJ/mol of I–I units bound and is significantly lower in magnitude than that of the amylose-iodine (AI) complex [Biopolymers, 31 , 57 (1991)]. A possible mechanism has been proposed for the formation of AI and API complexes with fixed compositions. © 1994 John Wiley & Sons, Inc.     

Synthesis of a novel, highly symmetric bis-oxa-bridged compound

A highly oxygenated, novel pentacyclic bis-oxa-bridged compound 8 was synthesized with remarkable efficiency starting from readily available tetrachloro-5,5-dimethoxyclopentadiene and 1,4-cyclohexadiene in three steps. The ruthenium-catalyzed oxidation of 2:1 bis-adduct 1 followed by a one-pot transformation of the resulting bis-alpha-diketone 3 furnished (after esterification) the title compound in an overall yield of 29.1%. The versatility of this simple method was further demonstrated with other norbornyl alpha-diketones to obtain the corresponding strained oxa-bridged derivatives.     

Anion-exchange initiation of reactions: Detection and spectrophotometric determination of aliphatic amines with 2,4-dinitrophenylhydrazine

The role of anion-exchange resin beads in the initiation of reactions of tertiary amines with 2,4-dinitrophenylhydrazine has been explored. This reagent has been used for the selective detection and determination of aliphatic amines. Radiochemical studies have been performed to show that the coloured species is adsorbed but not exchanged on ion-exchange beads. A model for the interaction is proposed.     

Rydberg states of the strontium ion

We report on the spectroscopy of highly excited strontium ions after resonant multistep laser excitation. The states observed belonged to then s (26≦n≦79),n d (25≦n≦83),n f (28≦n≦86) andn g (30≦n≦81) series of Sr⁺. A least squares fit has been applied to determine the quantum defects and their linear energy dependence in each series, together with the ionisation limit of Sr⁺. The analysis of our data lead to a revised value for this ionisation limit of 88 965.18±0.02 cm^?1, with respect to the ground state of the Sr⁺ ion. Analysis of the non core-penetratingn g states yielded experimental values for the dipole and quadrupole polarizability of Sr⁺⁺, which are in satisfactory agreement with previous calculations.