Viscometric Estimation of Unperturbed Chain Dimensions of Polymers

A new expression is proposed to determine the unperturbed dimensions of coil-like polymers viscometrically by use of the Flory and Kratky expression. The unperturbed dimensions so estimated are compared with the results obtained by using different expressions available in the literature. The results are comparable even for stiff chain polymers. The data obtained under theta conditions also fit this expression very well. The effect of molecular weight, its distribution, and that of the solvent has also been studied. It is concluded that the unperturbed dimensions are independent of molecular weight and solvent but depend on the heterogeneity of the system.     

Synthesis,characterisation and supramolecular interaction of Rh-biphenylic-imidazole-phenanthroline with antibiotics

A novel rhodium biphenylic imidazole phenanthroline metal-organic complex (BIP-MC) has been synthesised and characterised as a stable supramolecule. The structure of compound was established on the basis ESI, ¹H NMR and UV–vis spectroscopic data. The selectivity of BIP-MC as a new fluorescent chemosensor for various antibiotics has been explored. The supramolecular interaction of amoxicillin with BIP-MC enhanced the fluorescence activity of BIP-MC. A linear response of the sensor was observed in the measuring ranges of excitation 240–298 nm and emission 290–360 nm with detection limits of up to 10 μg/ml at an optimum pH 8.0. Based on the observations made here, a new quantitative method for the determination of this drug in synthetic samples without the use of separation of matrix is developed. It is also inferred that the possible fluorescence enhancement is due to the formation of exciplex between the BIP-MC and amoxicillin. These finding will thus help in pharmacokinetics studies of drugs. The sensor was used for the direct assay of amoxicillin antibiotic in commercial pharmaceutical preparations.     

Synthesis,spectroscopic and crystal structure analysis of 2-(4-fluorobenzyl)-6-(4-methoxyphenyl)imidazo[2,1-b][1,3,4]thiadiazole and its morpholinomethyl derivative

The preparation of 2-(4-fluorobenzyl)-6-(4-methoxyphenyl)-5-morpholin-1-ylmethyl imidazo[2,1-b][1,3,4]thiadiazole via the intermediate 2-(4-fluorobenzyl)-6-(4-methoxyphenyl)Imidazo[2,1-b][1,3,4] thiadiazole is described. Elemental analysis, IR spectrum, ¹H NMR and X-ray crystal structure analyses were carried out to determine the compositions and molecular structures of the two compounds. The crystal packing exhibits intermolecular C–H?O, C–H?N, C–H?F and π–π stacking interactions leading to the formation of the supramolecular network.     

On-line spectrophotometric determination of scandium after preconcentration on XAD-4 resin impregnated with nalidixic acid

An on-line scandium preconcentration and determination method was developed with spectrophotometer associated with flow injection. Scandium from aqueous sample solution of pH 4.5 was selectively retained in the minicolumn containing XAD-4 resin impregnated with nalidixic acid at a flow rate of 11.8 mL min^?1 as scandium–nalidixic acid complex. The scandium complex was desorbed from the resin by 0.1 mol L^?1 HCl at a flow rate of 3.2 mL min^?1 and mixed with arsenazo-III solution (0.05 % solution in 0.1 mol L^?1 HCl, 3.2 mL min^?1) and taken to the flow through cell of spectrophotometer where its absorbance was measured at 640 nm. The preconcentration factors obtained were 35 and 155; detection limits of 1.4 and 0.32 μg L^?1 and sample throughputs of 40 and 11 were obtained for preconcentration time of 60 and 300 s, respectively. The tolerance limits of many interfering cations like Th(IV), U (VI), rare-earths and anions like tartrate, citrate, oxalate and fluoride were improved. The method was successfully applied to the determination of scandium from mock seawater samples and good recovery was obtained. The method was also validated on certified reference material IAEA-SL-1 (lake sediment) and the result was in good agreement with the reported value.     

Regioselective Synthesis of Trichloromethyl‐Substituted Salicylates and Cyclohexenones by One‐Pot Cyclizations of 1,3‐Bis(trimethylsilyloxy)buta‐1,3‐dienes

A variety of 6‐(trichloromethyl)salicylates (=2‐hydroxy‐6‐(trichloromethyl)benzoates) were prepared by TiCl₄‐mediated cyclization of 1,3‐bis(trimethylsilyloxy)buta‐1,3‐dienes with 1,1,1‐trichloro‐4,4‐dimethoxybut‐3‐en‐2‐one. The employment of trimethylsilyl trifluoromethanesulfonate (Me₃SiOTf) as Lewis acid resulted in the formation of trichloromethyl‐substituted cyclohexenones. The cyclizations proceeded with good‐to‐very‐good regioselectivities.     

Oil Base Mud. Part I: Synthesis of Some Local Surfactants Used as Primary Emulsifiers for Oil Base Mud and Evaluation of Their Rheology Properties

Six oil soluble nonionic surfactants with different HLBs have been prepared. Their HLBs situate between 3.9 and 6.7. Transesterification was carried out for glycerol and triethanol amine with oleic acid at different moles to obtain six emusilifiers. They named glycerol momooleate (I), glycerol diooleate (II), glycerol trioleate (III), triethanol amine mono-, di- and tri-oleate (IV), (V,) and (VI). The chemical structure was confirmed using; the elemental analysis, FTIR and ¹HNMR. They were evaluated as a primary emulsifiers (PE) for thdrilling fluids (oil base mud) comparing with a currently used primary emulsifier (Fc). The water in oil base mud (w/o emulsions) was prepared. The concentration of emulsifiers and their HLB exhibited interesting rheology properties including shear-thinning behavior, yield value, viscoelastic effects, thixtropy, gel strength, and filtration loss. The rheology properties of such emulsions strongly depended on the average size distribution of the dispersed droplets that could be varied both with the bulk concentration and HLB value of the emulsifiers. The interfacial and surface properties of these emulsifiers suggest that the droplet size of the dispersed phase and bulk concentration are strongly related to the HLB value of emulsifiers. The w/o emulsion (mud formulation) stability is sensitive to the droplet size of the dispersed phase and HLB value of the used emulsifier. The results were discussed on the light the chemical structure of the primary emulsifiers and the emulsion ingredients.     

Synthesis of Some Oil Spill Dispersants Based on Sorbitol Esters and Their Capability to Disperse Crude Oil on Seawater to Alleviate Its Accumulation and Environmental Impact

In this respect mono‐, di‐, and tri‐ sorbitol oleate esters [SMO, SDO, and STO] were prepared and then ethoxylated using ethylene oxide to obtain six sorbitol esters at different ethylene oxide content (e.o=5, 12, 15, 20, 35, and 45). They were tested as oil spill dispersants individually and in blends. From the obtained data, it was found that the blends are more effective than the corresponding individual surfactants. The maximum dispersion capability for the prepared surfactants was obtained at HLB range from 9 to 11 for the both individual surfactants and blends. The increase of total carbon number in the surfactant alkyl group leads to increase dispersion capability of the dispersant. The wide range of ethylene oxide content was used, but the maximum dispersion efficiency was obtained at ethylene oxide=20 in E(20)STO. Meanwhile, the dispersion capability increases when the interfacial tension decreases.     

Micellar Enhanced Ultrafiltration of Reactive Black 5 from Aqueous Solution by Cationic Surfactants

Reactive black 5 (RB-5) dye was removed from a water stream using two cationic surfactants, cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC), via micellar enhanced ultrafiltration. Three membranes with different pore size were used for the determination of rejection coefficient and permeate flux of the solution at 1.5 bar trans-membrane pressure (TMP). The two surfactants (CPC and CTAB) played an almost negligible role in rejection efficiency with 5000 and 10,000 molecular weight cut-off membrane (MWCO), respectively. In this case, high rejection and low permeate flux was the result of a larger molecular size of RB-5 DYE being retained by comparatively smaller sized pores of membrane via ultrafiltration. However, CPC and CTAB surfactants showed 83% and 98% rejection coefficient, respectively, at a concentration greater than their CMC values against 30,000 MWCO. Permeate flux remained low and constant in presence of 5000 and 10,000 MWCO with a small variation against 30,000 MWCO for the two surfactants, thereby no appreciable effect on both surfactant concentrations on concentration polarization was estimated. Thus, RB-5 dye alone was determined to be responsible for membrane plugging or concentration polarization and ultimately for low permeate flux. The effect of trans-membrane pressure was also investigated during this study.     

The Surface and Thermodynamic Properties of Ethoxylated Sodium Monoalkyl Sulfosuccinate Surfactants

A series of ethoxylated sodium monooctyl sulfosuccinates [E(n)SMOSS] and ethoxylated sodium monolauryl sulfosuccinates [E(n)SMLSS] have different units of ethylene oxide (n = 9, 14, 23) were synthesized. The surface and thermodynamic properties of these surfactants have been compared with sodium dioctyl sulfosuccinate surfactant (SDOSS) as a commonly used surfactant. The surface tension measurements at 25, 35, 45, and 55°C were used to determine of the critical micelle concentration (CMC) and surface active properties of these surfactants. The effect of the ethylene oxide (EO) unit and the alkyl chain length on the surface properties for the prepared surfactants was studied. The results show that the ethoxylated sodium monoalkyl sulfosuccinates generally have lower values of CMC than that of sodium dioctyl sulfosuccinate. The values of surface active parameters indicate that the ethoxylated sodium monooctyl sulfosuccinates and ethoxylated sodium monolauryl sulfosuccinates surfactants have adsorption properties better than the sodium dioctyl sulfosuccinate surfactant as a resulted presence of ethylene oxide in molecules of the prepared surfactants. The thermodynamic parameters show that the (EO) unites in the chemical structure of ethoxylated sodium monoalkyl sulfosuccinate surfactants improve their micellization and adsorption properties.     

小麦秸秆发酵产生的真菌Pleurotus ostreatus IBL-02锰过氧化物酶的溶胶-凝胶固定化及其催化污水脱色(英文)

Solid state bio-processing of wheat straw was carried out through an indigenous fungal strain Pleurotus ostreatus IBL-02 under pre-optimized fermentation conditions. The maximum activity, 692±12 U/mL, of the industrially important manganese peroxidase (MnP) enzyme was recorded after five days of still culture incubation. The crude MnP was 2.1-fold purified with a specific activity of 860 U/mg after purification on a Sephadex-G-100 gel column. On native and SDS-PAGE electrophoresis gels, the purified MnP fraction was a single homogenous band of 45 kDa. An active fraction of MnP was immobilized using hydrophobic sol-gel entrapment comprising tetramethoxysilane (T) and propyltrimethoxysilane (P) at different T:P molar ratios. Characterization revealed that after 24 h incubation at varying pH and temperatures, the MnP fraction immobilized at a T:P ratio of 1:2 in the sol-gel retained 82% and 75% of its original activity at pH4 and 70 ℃, respectively. The optimally active fraction at a 1:2 T:P ratio was tested against MnSO4 as a substrate to determine the kinetic catalytic constants KM and Vmax . To explore the industrial applicability of P. ostreatus IBL-02 MnP, both the free and immobilized MnP were used for the decolorization of four different textile industrial effluents. A maximum of 100% decolorization was achieved for the different textile effluents within the shortest time period. A lower KM , higher Vmax , hyper-activation, and enhanced acidic and thermal resistance up to 70 ℃ were the novel catalytic features of the sol-gel immobilized MnP, suggesting that it may be a potential candidate for biotechnological applications particularly for textile bioremediation purposes.