The gas barrier coating of 3-aminopropyltriethoxysilane on polypropylene film

Nonporous films were formed on polypropylene (PP) films using 3-aminopropyltriethoxysilane (APTEOS) as the only precursor. The PP film was modified by corona-plasma treatment to provide appropriate adhesion between coating layer and substrate. Gas permeation properties of coating films were evaluated, and the influences of water ratio and film storing time on the gas permeability were investigated. Structural and surface properties of coating layers were characterized by ²⁹Si-NMR, FT-IR, and contact angle analyzer. The APTEOS coating films exhibit much higher barrier properties than PP film. The permeability coefficient of APTEOS coating film with water ratio of 3 is 0.011Barrer for nitrogen, 0.044Barrer for oxygen, and 0.002Barrer for carbon dioxide, while each permeability coefficient of PP bare film is 0.233, 0.858, and 2.886Barrer, respectively. The gas permeability coefficient is increased slowly along with storage time. Although additionally formed siloxane network may lead to a higher inorganic network density, the enhancement of gas permeability during storing period is largely attributed to film-swelling effect by the water vapor from atmosphere.     

Study of corrosion protection of mild steel by eco-friendly silane sol–gel coating

The effects of dipping duration in the silane solution and the sol pH on the protective performance of an eco-friendly silane sol–gel coating consisting a mixture of tetraethoxysilane, methyltriethoxysilane and glycidyloxypropyltrimethoxysilane applied on mild steel substrate were studied in this paper using electrochemical techniques and surface analysis. In consistency with the data obtained from electrochemical impedance spectroscopy and polarization curves, electrochemical current noise fluctuation analysis, appearance of the power spectral density plots and noise resistance indicated the most efficient sol pH and immersion time in the silane solution. In this regard, field emission type scanning electron microscopy images and water contact angle values revealed impact of the sol pH on the film structure. The enhancement in protective performance of the hybrid coating resulting from optimum immersion in the silane solution with appropriate pH was connected to the film homogeneity and higher cross linking and thickness as well. Moreover, a good trend correlation was observed between the noise resistance and low-frequency impedance modulus data.     

The effect of storage on the behaviour of Eudragit NE free film

Eudragit NE 30 D aqueous dispersion is a commonly used coating material, which contains methacrylate copolymers as film-forming agent and nonoxynol 100 as an endogenous emulsifier. The dissolution of the active ingredient from Eudragit NE-coated samples during storage is known to undergo a change. The crystallization of the emulsifier agent can play an important role in this. This polymer is not soluble in the gastrointestinal tract, but is permeable. Various parameters can influence the permeability of this film, e.g. via the tensile properties of the film. Change in the film thickness can cause the stretching of the film on a solid surface. Alterations in this physical parameter of the film were measured and the effects of different storage conditions were evaluated. The free film was prepared by spraying onto teflon. The crystallization of nonoxynol was followed via the changes in the DSC curve of the free film. A relationship was found between the film thickness and the crystallization of nonoxynol. It was established that the different storage conditions influence these changes. The temperature and the air humidity are important in this phenomenon. Lengthening of the storage time increased the difference in film thickness and crystallisation of emulsifier. This revised version was published online in July 2006 with corrections to the Cover Date.     

Solvent vapor annealing of block copolymer thin films: removal of processing history

The ordering processes of PS-b-P2VP block copolymer thin films with different processing histories were studied during solvent vapor annealing by in situ grazing incidence small-angle X-ray scattering (GISAXS). We compared cylinder-forming PS-b-P2VP thin films with 34 kg/mol molecular weight that were prepared in three different ways: spin coating, spin coating and subsequent solvent vapor annealing where the solvent vapor was removed instantaneously, and spin coating and subsequent solvent vapor annealing where the solvent vapor was removed slowly. Block copolymer thin films retained the morphology resulting from the different “processing histories” at smaller swelling ratios. This processing history was erased when the samples reached a higher swelling ratio (~1.4). After the solvent was slowly removed from the swollen film, the surface morphology was characterized by ex situ AFM. All samples showed the same morphology after solvent annealing regardless of the initial morphology, indicating the morphology of solvent annealed samples is determined by the polymer concentration in the swollen film and the solvent vapor removal rate, but not the processing history.     

An electropolymerized aniline-based fiber coating for solid phase microextraction of phenols from water

An aniline-based polymer was electrochemically prepared and applied as a new fiber coating for solid phase microextraction (SPME) of some priority phenols from water samples. The polyaniline (PANI) film was directly electrodeposited on the platinum wire surface in sulfuric acid solution using cyclic voltammetry (CV) technique. The efficiency of new coating was investigated using a laboratory-made SPME device and gas chromatography with flame ionization detection for the extraction of some phenols from the headspace of aqueous samples. The scanning electron microscopy (SEM) images showed the homogeneity and the porous surface structure of the film. The results obtained proved the ability of this polymer as a suitable SPME fiber coating for trapping the selected phenols. Influential parameters affecting the extraction process were optimized and an extraction time of 50 min at 50 °C gave maximum efficiency, when the aqueous sample was saturated with NaCl and adjusted at pH 2. This new coating can be prepared easily in a reproducible manner and it is rather inexpensive and stable against most of organic solvents. The PANI thickness can be precisely controlled by the number of CV cycles. At the optimum conditions, the R.S.D. for a double distilled water spiked with phenol and chlorophenols at ppb level were 4.8-17% (n = 3) and detection limits for the studied compounds were between 0.69 and 3.7 ng ml⁻¹, except for phenol and 4-chlorophenol. The optimized method was successfully applied to some real-life water samples.     

Indirect Competitive Enzyme-Linked Immunosorbent Assay for Detection of Tylosin in Milk and Water Samples

A specific polyclonal antibody was prepared based on a new hapten with stable structure. Based on this, an indirect competitive enzyme-linked immunosorbent assay (icELISA) was established for determination of tylosin residues in food and environmental samples. The experimental conditions were optimized as follows: the coating antigen and antibody were respectively diluted by 6000 times and 2000 times, and the competitive reaction time was 40 min. Under the optimized conditions, the method showed a detection limit of 0.07 ng mL^?1, an IC₅₀ of 1.39 ng mL^?1 and a linear range of 0.17–11.0 ng mL^?1. The recoveries of spiked raw milk and water samples were ranged from 78.4% to 105.6%, with the RSDs of less than 15%. Good correlation between icELISA and HPLC method was obtained for spiked samples (R² = 0.97). This method was suitable for the determination of tylosin residues in milk and water samples.     

Surface Treatment of Dimenhydrinate Crystals

Dimenhydrinate is a heat-sensitive antihistamine with a low melting point. The heat-sensitive feature is of importance if direct compression is used. Direct measurement of the heat originating in the texture of tablets during compression is very difficult. Thermoanalytical methods were used as indirect methods to describe the changes in material properties at high temperature: differential scanning calorimetry, thermomicroscopy and thermogravimetric analysis. Film coating method is widely used in pharmaceutical technology. A fluidized bed apparatus was applied to coat the crystals. The coating film forming agent was hydroxy-propyl-methylcellulose (HPMC), which is a gastric-soluble polymer. Thermoanalytical measurements reveal that dimenhydrinate crystals are sensitive to heat. Film coating method does not alter the shape of the DSC curve of dimenhydrinate, but increases the melting point. The presence of a macromolecular film reduces the thermal conductivity, because it separates the particles. This revised version was published online in August 2006 with corrections to the Cover Date.     

Analysis of human tear fluid by Raman spectroscopy

Tear fluid is a complex aqueous solution containing proteins, metabolites, electrolytes and lipids. This study uses Raman spectroscopy to analyse the composition of human tear fluid from three healthy volunteers. Two different methods are used to obtain Raman spectra from the 3 μL tear samples: (i) solution-phase Raman spectroscopy, and (ii) drop coating deposition Raman spectroscopy (DCDRS). Tear samples were either basal fluid, or yawn reflex secreted fluid. Calibration of the solution technique with standard protein solutions (5-15 mg mL⁻¹) showed that this method could predict the protein concentration (cross-validation) with an error of less than 1 mg mL⁻¹. The Raman signals from the tear fluid were very weak but signals due to protein and urea were clearly observable in all samples. The drop coating deposition technique was shown to produce very high signal-to-noise spectra for relatively short acquisition times, and small sample volumes. Raman point mapping combined with principal components analysis showed that the protein, urea, bicarbonate and lipid could all be detected in the tear samples and that the distribution of these components was inhomogeneous. Their position within the drying pattern was shown to depend on their relative solubilities. The results of this study suggest that solution Raman measurements may be calibrated to give the total tear protein concentration and DCDRS could be used to give a fingerprint of the tear protein (and lipid) composition.     

液相沉积法制备TiO2颗粒表面包覆SiO2纳米膜

研究了用液相沉积法在TiO2颗粒表面包覆SiO2纳米膜的过程.通过透射电镜(TEM)和酸溶实验分析,证实本实验在TiO2颗粒表面包覆了一层连续、致密的SiO2纳米膜.ζ-电位分析表明,颗粒表面只需少量包覆就可以显著改变颗粒表面的电动力学行为.采用 X射线荧光光谱分析仪（XRF）测定SiO2包覆量随包覆过程的变化.通过X射线光电子能谱（XPS）分析,获得Ti 2p、Si 2p及 O 1s电子结合能及其相对强度随包覆过程的变化规律,揭示硅酸分子在TiO2颗粒表面的包覆过程.分析表明,初期形成的活性硅酸分子与TiO2颗粒表面的羟基反应形成Ti－O－Si键,后期形成的硅酸分子与已键合在表面的硅酸发生缩合反应,形成连续致密的硅膜,膜层在陈化过程中继续缓慢生长.     

Comparison of mathemical methods for the calculation of retention indices at high temperature in gas chromatography

The retention indices of three homologous series (2-alkanones, 1-alkanols, cycloalksanones) have been determined at high temperature by the application of two new adaptation methods: A multiparametric least-squares regressions iterative method based on the dertermination of the adjusted retention times and a cubic interpolation directly using the uncorrected retention times without dead time correction. The two methods were applied to two types of columns. The first group includes eight packed columns (seven OV polymethylphenylsiloxane and Apolane-87 stationary phases), while the second includes five glass capillary columns (four methyl-silicons with different film thicknesses and Apolane-87 stationary phases). The retention indices obtained with a multiparametric and a cubic interpolation methods were compared with each other and with those calculated by Grobler's, Guardino's, Kaiser's and Kovàts' methods. The influence of coating, film thickness, and temperature on them was investigated.     

Interfacially synthesized thin film composite RO membranes for seawater desalination

A composite RO membrane with high salt rejection and high flux for the desalination of seawater was prepared by treating a porous polysulfone (PS) support sequentially with a di-amine and then with a polyfunctional acid chloride, thereby forming a thin film of polyamide (PA) on the PS support. In order to establish conditions for the development of suitable thin film composite (TFC) membranes on a coating machine, various parametric studies were carried out which included varying the concentration of reactants, reaction time, curing temperature and curing time for thin film formation by the interfacial polymerization technique. By suitable combination of these factors,a desired thin film of polyamide with improved performance for seawater desalination could be obtained. Moreover, the product water fluxes were considerably enhanced by post-treatment of the TFC membrane. Continuous sheets of TFCs were developed on the mechanical coating unit and tested for RO performance in a plate-and-frame configuration with synthetic seawater. The performance of these composite membranes was also determined for the separation of organics and compared with cellulose acetate (CA) membranes.     

铝合金表面改性对有机涂层附着力的影响及腐蚀防护性能研究

利用电化学阻抗（EIS）、扫描微参比技术（SRET）、接触角、粗糙度、附着力、盐雾等测试方法,研究了铝合金阳极氧化与贻贝黏附蛋白（MAP）/CeO₂/硅烷γ-APS（MCA）表面复合修饰的腐蚀防护性能以及对改性聚氨酯涂层附着力和耐蚀性的影响。结果表明,MCA复合膜可抑制铝合金的腐蚀,并具有一定的自修复功能;阳极氧化和MCA表面复合修饰可为铝合金提供有效的早期腐蚀防护作用,且能提高铝合金表面粗糙度和润湿性,显著提升改性聚氨酯涂层在铝合金表面的附着力和耐蚀性,因而结合改性聚氨酯涂层和表面复合修饰可实现对铝合金长期有效的腐蚀防护。     

An aniline-based fiber coating for solid phase microextraction of polycyclic aromatic hydrocarbons from water followed by gas chromatography-mass spectrometry

A fiber coating from polyaniline (PANI) was electrochemically prepared and employed for solid phase microextraction (SPME) of some polycyclic aromatic hydrocarbons (PAHs) from water samples. The PANI film was directly electrodeposited on the platinum wire surface in sulfuric acid solution using cyclic voltammetry (CV) technique. The applicability of this coating was assessed employing a laboratory-made SPME device and gas chromatography with mass spectrometry (GC-MS) for the extraction of some PAHs from the headspace of aqueous samples. Application of wider potential range in CV led to a PANI with more stability against the temperature. The homogeneity and the porous surface structure of the film were examined by the scanning electron microscopy (SEM). The study revealed that this polymer is a suitable SPME fiber coating for extracting the selected PAHs. Important parameters influencing the extraction process were optimized and an extraction time of 40 min at 40 degrees C gave maximum peak area, when the aqueous sample was added with NaCl (20%, w/v). The synthesis of the PANI can be carried out conveniently and in a reproducible manner while it is rather inexpensive and stable against most of organic solvents. The film thickness of PANI can be precisely controlled by the number of CV cycles. The resulting thickness was roughly 20 microm after 20 cycles. At the optimum conditions, the relative standard deviation (RSD) for a double distilled water spiked with selected PAHs at ppb level were 8.80-16.8% (n = 3) and detection limits for the studied compounds were between 0.1-6 pg mL(-1). The performance of PANI was, also, compared with a commercial solid coated-based SPME fiber, carbowax/divinylbenzene (CW/DVB), under similar experimental conditions.     

Surface Pretreatments of AA5083 Aluminum Alloy with Enhanced Corrosion Protection for Cerium-Based Conversion Coatings Application: Combined Experimental and Computational Analysis

The effects of surface pretreatments on the cerium-based conversion coating applied on an AA5083 aluminum alloy were investigated using a combination of scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), polarization testing, and electrochemical impedance spectroscopy. Two steps of pretreatments containing acidic or alkaline solutions were applied to the surface to study the effects of surface pretreatments. Among the pretreated samples, the sample prepared by the pretreatment of the alkaline solution then acid washing presented higher corrosion protection (~3 orders of magnitude higher than the sample without pretreatment). This pretreatment provided a more active surface for the deposition of the cerium layer and provided a more suitable substrate for film formation, and made a more uniform film. The surface morphology of samples confirmed that the best surface coverage was presented by alkaline solution then acid washing pretreatment. The presence of cerium in the (EDS) analysis demonstrated that pretreatment with the alkaline solution then acid washing resulted in a higher deposition of the cerium layer on the aluminum surface. After selecting the best surface pretreatment, various deposition times of cerium baths were investigated. The best deposition time was achieved at 10 min, and after this critical time, a cracked film formed on the surface that could not be protective. The corrosion resistance of cerium-based conversion coatings obtained by electrochemical tests were used for training three computational techniques (artificial neural network (ANN), adaptive neuro-fuzzy inference system (ANFIS), and support vector machine regression (SVMR)) based on Pretreatment-1 (acidic or alkaline cleaning: pH (1)), Pretreatment-2 (acidic or alkaline cleaning: pH (2)), and deposition time in the cerium bath as an input. Various statistical criteria showed that the ANFIS model (R² = 0.99, MSE = 48.83, and MAE = 3.49) could forecast the corrosion behavior of a cerium-based conversion coating more accurately than other models. Finally, due to the robust performance of ANFIS in modeling, the effect of each parameter was studied.     

Determination of phosphate in natural waters by capillary electrophoresis Influence of solution composition on migration time and response

This paper deals with the determination of the more complex phosphate anion by capillary electrophoresis using indirect UV detection. First, the pH of the running electrolyte influences both the migration time and the response of the phosphate anion. Both effects could be explained well by taking into account phosphorus speciation in solution. In addition, the experimental method has been applied to three different sets of natural water systems; (i) groundwater, (ii) surface water and (iii) stemflow samples. The migration time behaviour of phosphate was different for the three sample sets and, hence, difficulties arise with respect to a clear and unique identification of the compound. Deviations herein could be minimized by applying a correction method for migration time drift. Concentrations of phosphate could be quantified in most samples and were confirmed by a calorimetric method. Average recoveries of additions of phosphate to groundwater, surface water and stemflow samples were 105, 83 and 103%, respectively. For one stemflow sample, quantitative recovery of phosphate was possible only by changing the pH of the running electrolyte solution. The latter observation might be very useful in setting up speciation-related measurement methods.     

The origin of the formation of cavities in galvanized coatings

The role of water‐soluble corrosion products on galvanized wires was examined. The samples used were industrial hot‐dip galvanized wires, which were exposed to the open air under all weather conditions for a relatively short time (6 and 12 months), in an urban environment close to the sea. The samples were studied by different methods, i.e. scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD) and optical microscopy (OM). Several phases were detected because of the galvanization procedure and the steel substrate. Furthermore, phases which were formed as a result of the reaction of zinc with the atmosphere were also detected. These were oxides like ZnO, carbonates like ZnCO₃ and hydrated Zn and Fe sulfates. Their presence influences the corrosion resistance of the wires, which finally, strongly depends on the solubility of the wires in water. The SO₄^2? compounds especially are very soluble and consequently are easily removed from the coating surface, leading to its degradation by the formation of cavities. In any case, their presence, even after a short period of exposure, implies that the coating is highly affected by the atmosphere of the modern city. Copyright © 2006 John Wiley & Sons, Ltd.     

Polyphosphate-doped polypyrrole coated on steel fiber for the solid-phase microextraction of organochlorine pesticides in water

A solid-phase microextraction technique using steel fiber coated with 20 μm polypyrrole (Ppy) doped with polyphosphate was developed for the GC determination of a group of organochlorine pesticides (OCPs) in water. The coating was prepared using a three-electrode electrochemical system from a 10% aqueous sodium polyphosphate solution containing 0.05 M pyrrole by applying a constant potential of 1.2 V for 30 min. In order to obtain an adherent, smooth and stable film of polypyrrole, experimental parameters related to the coating process consisting of the type of dopant or counter-ion, deposition potential, concentration of the monomer, concentration of the counter-ion, and deposition time were optimized. The effects of various parameters on the efficiency of SPME process such as extraction time, extraction temperature, ionic strength, desorption time, and desorption temperature were also studied. The coating was highly stable and extremely adherent to the surface of the steel fiber. The method was linear for at least three orders of magnitude with correlation coefficients varying from 0.9818 to 0.9977. The accuracies found through spiking blank samples showed high recoveries between 82 and 110%. Intra- and inter-day precisions of the method were determined from mixed aqueous solutions containing 1.0 ng ml⁻¹ of each OCP. The intra-day precisions varied from 4.7% for heptachlor to 11.4% for methoxychlor, while the inter-day precisions varied from 6.8% for endosulfan I to 13.0% for p,p′-DDD and o,p-DDD. Limits of detection based on S/N = 3 were in the range 0.015-0.66 pg ml⁻¹. The proposed method was applied to monitor organochlorine pesticides in some well water samples.     

The determination of copper at thin film electrodes by constant current stripping potentiometry

A comparison of the determination of copper by constant current stripping potentiometry (CCSP) at mercury and gold films has been carried out. The preferred solution conditions for the mercury film study were determined to be 0.1M ammonium acetate at pH 4.5 and 0.1M HCl for the gold film study. The influence of chloride on the stripping signal was investigated and it was found that for the mercury film conditions, well-formed stripping signals could be obtained up to a chloride concentration of 0.5 M which permitted the ready determination of copper in seawater. With the gold film, high chloride concentrations affected both the film stability and the glassy carbon surface and repeatable results were difficult to obtain. The optimized CCSP methods were applied to various aqueous samples including tap water, seawater, TCLP (acetic acid) extracts as well as TCLP extracts using groundwater and ocean water. Based on the results obtained for these various matrices, it was concluded that there are several advantages favoring the mercury film. The interference from organic components in the sample matrix on the general applicability of CCSP for the determination of copper at either a mercury or gold film is discussed.     

Evaluation of methoxy polyethylene glycol‐polylactide diblock copolymers as additive in hypromellose film coating

This paper deals with a new application of diblock methoxy polyethylene glycol‐polylactide block copolymers, a class of synthetic biomaterials largely studied in the pharmaceutical and biomedical fields owing to their favorable properties such as biocompatibility, biodegradability, low immunogenicity, and good mechanical properties. In this work, these materials were evaluated as additives for gastro‐soluble pharmaceutical coating aimed to reduce film stiffness and water permeability. Two copolymers with different polylactide chain lengths were synthesized and characterized in term of molecular weight and solid‐state properties. A series of free films with different hypromellose/copolymers ratio were prepared and characterized in terms of appearance, components miscibility, plasticity, and water vapor permeability. The obtained results demonstrate that copolymers effectively influence hypromellose film properties according to their concentration and molecular weight. Specifically, the addition of the copolymer with a molecular weight of 6.5 kDa in a ratio hypromellose:polymer 5:1, allowed to obtain films with good appearance, improved plasticization, and water permeability properties. For higher molecular weight, copolymer or different ratios was not possible to observe the improvement of all the properties at the same time. The results also make possible to define the critical features to improve in order to use block copolymers as additive in hypromellose film coating. The availability of new water‐soluble additives able to work as plasticizer and moisture sealer in polymeric films represents an important progress not only in the field of pharmaceutical coating but also in that of food coatings, as for example in the formulation of edible films. Copyright © 2013 John Wiley & Sons, Ltd.     

The effects of cotton gauze coating with microbial cellulose

Microbial cellulose is a pure form of cellulose with widespread applications. It is very applicable for medical usage specially wound dressings due to its high liquid absorbency and hygienic nature. In this study, microbial cellulose formed/coated on cotton gauze samples during its biosynthesis in a static medium (Hestrin & Scharm) for 6 days by Acetobacter Xylinium. Some essential factors of treated gauze samples, like water absorbency, drying time (water holding time), and amount of vertical wicking were determined and compared with untreated samples. Results showed that cotton gauze coating with microbial cellulose increases water absorbency and wicking ability over 30%, and reduces drying time about 33%. It can be concluded that covering of cotton gauze with microbial cellulose can promote some important characteristics of it specially for wound dressings.