ELECTRO-OPTICAL DETERMINATION OF α-FeOOH PARTICLE SIZES

Electric light scattering method is used for revealing the presence of aggregates in very diluted aqueous α-FeOOH suspensions. Three theoretical models are used for the geometrical form of aggregates. The comparison between the electro-optical results -theoretical and experimental - shows that even in the most diluted suspensions exist aggregates with irregular form. Using the comparison between electron microscopy and electro-optical results the geometric shape of the aggregates is determined.     

Effects of polymer addition on the rheology of o/w microemulsions

Microemulsions are profitably employed in the pharmaceutical field to prepare drug delivery systems release for guest drugs sparingly soluble in water. In particular, they can be used for topical and transdermal administration in place of ointments or creams, on condition that their rheological properties are properly modulated. The present work concerns the analysis of the rheological effects produced by the addition of different amounts of Carbopol 940, a polymer widely used for topical applications, to an O/W microemulsion containing a lipophilic phase (Labrafac Hydro, 21 wt%) and stabilized by the surfactant (Cremophor RH40)/co-surfactant (Transcutol) couple. The contribution of the disperse phase is evaluated by comparing the linear and nonlinear properties of the Carbopol/microemulsion system (CM) with those of the corresponding aqueous Carbopol systems with co-surfactant (CWT) and without co-surfactant (CW). Four polymer concentrations (0.25%, 0.5%, 1%, and 2%) are taken into consideration. The linear viscoelastic properties of the microemulsions essentially mirror those of the corresponding aqueous Carbopol systems when the polymer concentration is sufficiently high (1–2%). In these conditions the oil phase is reasonably hosted within the meshes of the three-dimensional polymeric gel network and gives only a slight contribution to the connectivity of the whole system. Similar considerations can be drawn from the flow behavior of the systems examined in the low shear region. Received: 6 February 2000 Accepted: 13 November 2000     

The effect of hydration on the thermal behaviour of hydrophilic non-aqueous gels stabilised by Carbopol 974P

A thermal analysis of the effect of hydration of non-aqueous polymer-stabilised gels was investigated using differential scanning calorimetry (DSC). The interaction of water with the polymer and its distribution within the gel are critical to the physicochemical behaviour of the gel, and consequently affects the utility of the gel matrix as a drug delivery vehicle. Addition of water at levels up to and including 50% (w/w) did not result in an observable freezing event in the thermogram. However, at 60 and 80% (w/w) water, phase transitions were observed, the magnitude of which were found to be independent of the annealing time within the range used. The observed melting enthalpies increased as the water concentration increased for all formulations, but were always smaller than that of pure water. There was no evidence of multiple transitions that might be attributed to different populations of water molecules. However, the results demonstrate that DSC can be employed to differentiate between freezable and non-freezable water, in these particular formulations.     

锌铋合金电极在溶胶电解液中的电化学行为

锌电极的自腐蚀速率, 持续放电下的阳极溶解速率和电极钝化的难易程度是碱性电池性能的重要电化学参数. 本文应用线性极化、恒流放电等电化学实验方法研究了电解液中添加Carbopol树脂以及电极中添加Bi对锌电极电化学行为的影响. 并应用金相显微镜和环境扫描电子显微镜(ESEM)对锌电极和锌铋合金电极浸蚀及放电后的形貌进行了表征. 结果表明: 电解液中添加适量的Carbopol树脂可明显提高电极的极化电阻, 显著降低电极的自腐蚀速率; 阳极的溶解电位出现不同程度的正移, 阳极过电位显著增大且大电流密度放电时较明显促进电极钝化. 锌电极中添加一定量的Bi对改善电极表面氧化物膜的沉积形貌和电极表面固液界面的传质条件, 减小电极的自腐蚀速率, 抑制电极自腐蚀等方面具有显著作用.     

Characterization of cyclodextrincarbopol interactions by DSC and FTIR

The interactions between Carbopol and β-cyclodextrin (BCD) or hydroxypropyl-β-cyclodextrin (HPBCD) were studied by differential scanning calorimetry (DSC) and FTIR spectroscopy. Aqueous solutions of both components were desiccated by freeze-drying or heating in an oven (films) at various temperatures. The use of different drying procedures allowed their influence on the interactions to be studied. The evolution of the Carbopol glass-transition was also evaluated by DSC using first heating runs up to different temperatures. Disappearance of the Carbopol glass-transition was observed in the freeze-dried systems prepared with either of the cyclodextrins and in the films that contained HPBCD. The changes in the FTIR band of Carbopol at 1700 cm^-1 confirmed the existence of interactions with both cyclodextrins, especially with HPBCD. This information may be useful for optimising the solubilizing capacity and controlled release performance of aqueous Carbopol-cyclodextrin systems. This revised version was published online in July 2006 with corrections to the Cover Date.     

Phase Behavior and Formulation of Palm Oil Esters o/w Nanoemulsions Stabilized by Hydrocolloid Gums for Cosmeceuticals Application

Palm oil esters (POEs) are wax esters derived from palm oil and cis-9-octadecen-1-ol. The excellent wetting behaviour of the esters without the oily feel make them have great potentials in the manufacture of cosmeceutical and pharmaceutical products. However, little is known about their phase behaviors in ternary systems. The purpose of this investigation was to construct phase diagram of the POEs and mixed surfactants and to consequently select nanoemulsions composition for further studies. The preparation and characterization of oil-in-water nanoemulsions stabilized by hydrocolloid gums were then studied. Two types of nonionic surfactants were selected, namely Tween 80 (T80) and Span 80 (S80). Ternary phase diagram of POEs:Tocotrienol/T80:S80 (80:20)/water system was constructed at 25.0 ± 0.5°C. The emulsification properties of 2 hydrocolloids gum (xanthan gum, carbopol ultrez 20 copolymer) were investigated. Gum dispersions were prepared in water (0.8%) and emulsified with 30% oil using a Polytron homogenizer. The flow curve of the emulsions always exhibited shear thinning behavior and obeys the power law viscosity. The emulsions with carbopol ultrez 20 copolymer was the most stable emulsions which composed of very small oil droplets (50% < 142.43 nm) with a narrow size distribution.     

Mucin/carbopol matrix to immobilize oxalate oxidase in a urine oxalate amperometric biosensor

An enzymatic amperometric electrode with extended analytical range and improved stability for oxalate determination has been developed. Glutarlaldehyde/mucin/carbopol matrix was used for the crosslinking of the enzyme between polymeric membranes to form a classical laminate construction (sandwich) and compared with the glutaraldehyde/mucin/enzyme and glutaraldehyde/albumin/enzyme.The use of a sulphonated membrane as internal membrane allowed rejection of the most important electrooxidable urine interferents. The recovery assays were highly satisfactory. The wide linear response in the range 2-400 μM after 1/10 urine dilution (corresponding to 20-4000 μM) made it suitable for clinical range. High correlation with the standard spectrophotometric method was obtained (r² = 0.98, y = 0.89x, n = 25).     

An investigation of squeeze flow as a viable technique for determining the yield stress

A systematic study of squeeze flow (SF) was performed on different concentrations of Carbopol with varying yield stresses. A sample of constant volume was placed between two parallel plates and a series of constant force steps applied, following the plate separation as a function of time. Precise rheological measurements of the model yield stress fluids were performed in addition to the well-controlled SF tests. These rheological measurements were used in conjunction with the SF equations to determine the time-dependent plate separation, allowing a direct comparison of theory and experiment throughout the entire test. The limiting height achieved during constant force SF reveals information about the yield stress of the fluid as predicted by the theory. It appears that by carefully controlling the experimental conditions of the squeeze test one can obtain yield stress values that agree with the rheological measurements within 10%. Additionally, the validity of the lubricational theory was tested; not only for the determination of the yield stress but throughout the flow as well.     

New measurements of the flow-curves for Carbopol dispersions without slip artefacts

The thickening properties of many commercial thickeners are difficult to measure because of wall slip artefacts. Here we report a series of experiments on a typical thickener where these artefacts have been successfully eliminated. As a result, complete, steady-state flow-curves of aqueous Carbopol 980 (the toxicologically preferred version of the older and more well-known Carbopol 940) dispersions are reported for a range of concentrations of 0.045–1.0 wt%. The vane-and-basket flow geometry was used to avoid slip problems at low shear stress, with the geometry housed in a TA AR1000-N controlled-stress rheometer, whilst a Haake RV2 viscometer with an SV2P and MV2P concentric-cylinder geometries were used at higher shear rates. The flow-curves obtained show a smooth but steep transition from a very high Newtonian viscosity at low shear stress to a much lower viscosity at high shear stress. No real yield stresses were detected, but the higher shear rate results can be fitted to the Herschel-Bulkley model, which assumes an apparent yield stress. The various model parameters are displayed as a function of Carbopol concentration. Received: 29 November 2000/Accepted: 26 February 2001     

Osmotic deswelling of microgels by linear polyelectrolytes

Polyacrylate microgels used as absorbers or viscosifiers in water are known to have these useful qualities reduced in the presence of linear poly-electrolytes. An osmotic deswelling mechanism is postulated whereby the counterions from linear chains sterically excluded from the gel act to draw solvent from the gel phase. This postulate is tested using intrinsic viscosity measurements of Carbopol microgels, made with the linear polyelectrolyte considered as parr of the solvent. The intrinsic viscosity is used to calculate the swollen-to-dry volume ratio for the microgel in the presence or absence of 0.1% linear sodium polyacrylate over a range in ionic strength. Simultaneously, a standard treatment for the free energy of a network of non-Gaussian chains containing fixed charges is modified to include the osmotic effect of the excluded counterions. In the absence of linear polymer, the theory is fit to the data, the fitting parameter being the 3100 monomer units between crosslink sites in the network. In the presence of high (350 000) molecular weight linear polymer, good agreement is found between the observed deswelling and that predicted if the linear chains are totally excluded. Lower molecular weight linear chains are found to give a reduced deswelling which is shown to be self-consistent with their partitioning into the network.Presented in part at the 64th Colloid and Surface Science Symposium, Lehigh University, June 1990