Factors affecting membrane fouling reduction by surface modification and backpulsing

Several factors affecting microfiltration membrane fouling and cleaning, including backpulsing, crossflushing, backwashing, particle size, membrane surface chemistry, and ionic strength, were investigated with suspensions of latex beads. Approximately two-fold permeate volume enhancements over 1 h of filtration were obtained by using water or gas backpulsing, and 50% enhancement was obtained with crossflushing, for filtration of 1.0 μm diameter carboxylate modified latex (CML) particles using unmodified polypropylene (PP) membranes of 0.3 μm nominal pore diameter. When 0.2 μm diameter CML particles or mixtures of 1.0 and 0.2 μm CML particles were used, however, the average flux decreased 60% compared with using 1.0 μm CML particles for experiments with or without backpulsing.PP membranes were rendered hydrophilic with neutral or positively on negatively charged surfaces by grafting monomers of poly(ethylene glycol 200) monomethacrylate (PEG200MA), dimethyl aminoethyl methacrylate (DMAEMA), or acrylic acid (AA), respectively, to the base PP membranes. Filtration experiments show that fouling is not strongly dependent on membrane surface chemistry for filtration of 1.0 μm CML particles without backpulsing. With backpulsing, however, a 10% increase and a 20% decrease of permeate volumes collected in 1 h were observed when the CML particles and the membranes had like charges and opposite charges, respectively, compared to the permeate collected with the unmodified membrane. Using the PP membranes modified with AA, permeate volumes with backpulsing decreased 30 and 40% when NaCl concentrations of 0.01 and 0.1 M, respectively, were added to the feed. However, the permeate volumes did not vary significantly with changing ionic strength for filtration without backpulsing.     

Bacterial passage through microfiltration membranes in wastewater applications

Two polyvinylidenefluoride microfiltration membranes (GVHP and GVWP: Millipore, Bedford, MA) with a nominal pore size of 0.22 μm were challenged with mixed microbial cultures present in Milli-Q™ water and in secondary effluent, and with a Gram-negative model bacterium, SW8, to investigate bacterial passage. Total bacterial counts measured microscopically using the DNA fluorochrome DAPI revealed that the small bacteria in Milli-Q™ water passed MF membranes totally. The model bacterium, SW8 and bacteria from secondary effluent were mostly retained with log reduction values (LRV) of 4 and 3.5, respectively. Transmembrane pressure did not influence the levels of bacterial passage significantly. Pore size effects were investigated with track-etched membranes (Poretics™: Osmonics, Minnetonka MN) with nominal pore sizes of 0.2, 0.1 and 0.05 μm. The LRV of 0.2 μm membranes for SW8 and secondary effluent cells was 3 and 1.5, respectively (total counts). Both membranes with pore sizes smaller than 0.2 μm acted similarly, they still transmitted secondary effluent cells with LRV 2 log higher than 0.2 μm membranes, but for SW8 only 50% higher. In contrast to total count results, removal of bacteria was 100% with all membranes when assessed by cultureable counts, i.e. numbers of bacterial colonies recovered on R2A agar plates. Transmitted bacteria failed to grow on standard basal microbiology media most probably because they were injured during passage through the membranes to the extent that recovery in laboratory media did not occur. However, tests with CTC, an indicator of cell viability, indicated that approximately half of the cells of SW8 which passed the membranes had what appeared to be functional electron transfer chains in their membranes. All membranes had a pore size distribution which included pores larger than the nominal value. Field emission scanning electron microscopy (FESEM) provided evidence for entrapment of bacteria within the membrane matrix.     

Evaluation of boronate-containing polymer brushes and gels as substrates for carbohydrate-mediated adhesion and cultivation of animal cells

Boronate-containing thin polyacrylamide gels (B-Gel), polymer brushes (B-Brush) and chemisorbed organosilane layers (B-COSL) were prepared on the surface of glass slides and studied as substrates for carbohydrate-mediated cell adhesion. B-COSL- and B-Brush-modified glass samples exhibited multiple submicron structures densely and irregularly distributed on the glass surface, as found by scanning electron microscopy and atomic force microscopy. B-Gel was ca. 0.1 mm thick and contained pores with effective size of 1–2 μm in the middle and of 5–20 μm on the edges of the gel sample as found by confocal laser scanning microscopy. Evidence for the presence of phenylboronic acid in the samples was given by time-of-flight secondary ion mass-spectrometry (ToF SIMS), contact angle measurements performed in the presence of fructose, and staining with Alizarin Red S dye capable of formation specific, fluorescent complexes with boronic acids. A comparative study of adhesion and cultivation of animal cells on the above substrates was carried out using murine hybridoma M2139 cell line as a model. M2139 cells adhered to the substrates in the culture medium without glucose or sodium pyruvate at pH 8.0, and then were cultivated in the same medium at pH 7.2 for 4 days. It was found that the substrates of B-Brush type were superior both regarding cell adhesion and viability of the adhered cells, among the substrates studied. MTT assay confirmed proliferation of M2139 cells on B-Brush substrates. Some cell adhesion was also registered in the macropores of B-Gel substrate. The effects of surface microstructure of the boronate-containing polymers on cell adhesion are discussed. Transparent glass substrates grafted with boronate-containing copolymers offer good prospects for cell adhesion studies and development of cell-based assays.     

Characterization of the 3-dimensional microstructure of a graphite negative electrode from a Li-ion battery

The 3-dimensional microstructure of a porous electrode from a lithium-ion battery has been characterized for the first time. We use X-ray tomography to reconstruct a 43 × 348 × 478 μm sample volume with voxel dimensions of 480 nm, subsequent division of the reconstructed volumes into sub-volumes of different sizes allow us to determine microstructural parameters as a function of sub-division size. We show that the minimum size for a representative volume element is about 43 × 60 × 60 μm for volume-specific surface area, but as large as the full sample volume for porosity and tortuosity.     

Fabrication and supercapacitive performance of long anodic TiO2 nanotube arrays using constant current anodization

A galvanostatic anodization is used to prepare long TiO₂ nanotube arrays (TNTAs). TNTAs of over 100 μm in length, with similar nanotube size and structural regularity to the classic TNTAs made from potentiostatic mode, are achieved at 10 mA cm^− 2. After a post-anodization in a H₃PO₄-based electrolyte, the TNTAs with long nanotubes exhibit good adhesion to Ti substrate. The as-prepared long TNTAs yield a larger areal capacitance of 128.4 mF cm^− 2. Further, the long TNTAs possess a higher surface area, making them suitable as support templates for other active materials.     

Concentration and temperature dependence of surface parameters of some aqueous salt solutions

The effect of concentration and temperature on surface tension of aqueous solutions of four different salts has been studied. These include the chloride salts of lithium, sodium, potassium and ammonium. The study was conducted at five different concentrations i.e. 0.1, 0.5, 1.0, 1.5 and 2.0 M, and five different temperatures i.e. 10, 15, 20, 25 and 30 °C. By analyzing the results, the concentration and temperature dependence of surface excess concentration and thermodynamic parameters of surface formation such as enthalpy, entropy, and surface pressure have been calculated.     

Formation of porous TiOx biomaterials in H3PO4 electrolytes

In this work, formation of porous TiO_x layers and theirs corrosion behavior were studied. Application of H₃PO₄ electrolytes results in porous TiO_x formation. The process is enhanced by small amount of HF content in the electrolyte. The HF results in higher current density, enhancing dissolution. Small 0.5% HF concentration results in nanopores formation, with pore diameter of about 45 nm. Increase of HF concentration up to 10% results in pores with average diameter of about 5.2 μm. An increase of etching time results in larger pore diameter, but between large 2–5 μm diameter pores smallest ones were observed with diameter below 200 nm. In the initial etching process a remnants of the flat surface are presents with initial cracks in the surface, indicating places for growth of the pores.The TiO_x layers can be used as a biomaterial. The corrosion behavior of the layer investigated in Ringer’s solution, revealed an excellent corrosion resistance, with respect to pure Ti.     

A novel waist-regulable dumbbell-like nanosuperstructure of (3-carboxy-1-acyl-propyl)-ferrocene

Dumbbell-like nanosuperstructures of (3-carboxy-1-acyl-propyl)-ferrocene were successfully prepared by ultrasonic–pHcontrolling–reprecipitation method. The scanning electron microscope shows that as-obtained products were composed of nanorods. The length of the products is about 6–12 μm, the diameter of the two polar coronas and the middle part (waist) are respectively about 2–8 μm and 0.5–2 μm. The diameter of the nanorods that are the basic unit of the superstructures, is about 0.3 μm. X-ray diffraction analysis of the products indicated that the superstructures keep original crystal structure. The optical properties of the products were characterized by FT-IR spectrometer and UV spectrometer, and they display quantum size effect. This paper provides a novel method that has potential application in preparing other organometallic compounds superstructures, and more importantly, the as-obtained superstructures have widely applications. The possible mechanism was also proposed.     

Two-dimensional carbon cloth and three-dimensional carbon felt perform similarly to form bioanode fed with food waste

Two-dimensional carbon cloth and three-dimensional carbon felt were compared for their capacity to form bioanodes for food waste treatment. Wastewater was used as the dilution medium instead of a synthetic solution to be close to industrial conditions. In both cases, microbial cells were mainly wrapped around the fibers of the electrodes. The biofilms were around 80–120 μm thick with a 39.3% microbial volume ratio on carbon cloths. On carbon felt, the biofilms showed a lower microbial volume ratio of 16.3% on the upper layers but with a penetration depth of 200–800 μm. The biofilm patterns were different but they resulted in similar current density, around 3.5 A/m².When chemically rich media have to be implemented, 2D cloth offers a worthwhile solution that can equal 3D porous materials.     

Polysulfone — sulfonated poly(ether ether) ketone blend membranes: systematic synthesis and characterisation

The effect of sulfonated poly(ether ether ketone) (SPEEK) in membrane formation and separation properties has been investigated in polysulfone(PSU)/SPEEK/N-methyl-2-pyrrolidinone (NMP) systems. Charged ultrafiltration/nanofiltration membranes were obtained reliably in the range of 0.5–5 wt.% SPEEK in the polymer blend. All PSU/SPEEK blend membranes had substantially higher water flux, salt rejection, porosity and greatly reduced particle adhesion compared to the PSU base membrane. Further, all of these properties varied systematically with variation of SPEEK content. Reproducibility and stability of the membrane properties was excellent. Pore sizes determined from dextran retention data and AFM measurements showed reasonable agreement. Membranes with 5 wt.% SPEEK demonstrated excellent overall properties. Such membranes had very high permeability, 22.6±1.6×10⁻¹¹ m³ s⁻¹ N⁻¹, 0.999 fractional rejection of 4000 Da dextran, 0.65 rejection of 0.001 M NaCl, and only 0.75 mN m⁻¹ adhesion of a 4 μm silica particle. Such membranes are very promising for scale-up of production and testing on real process streams.     

Simultaneous determination of thirty non-steroidal anti-inflammatory drug residues in swine muscle by ultra-high-performance liquid chromatography with tandem mass spectrometry

An ultra-high-performance liquid chromatography with tandem mass spectrometric detection (UHPLC–MS/MS) method was established for the simultaneous determination of residues of thirty non-steroidal anti-inflammatory drugs (NSAIDs) in swine muscle. The samples were extracted with acetonitrile and phosphoric acid. The extracts were defatted with n-hexane, and then purified by HLB solid-phase extraction cartridge. Analysis was carried out on UHPLC–ESI-MS/MS working with multiple reaction monitoring mode with polarity switching. Limits of detection were between 0.4 μg/kg and 2.0 μg/kg, and limits of quantification were between 1.0 μg/kg and 5.0 μg/kg. The recoveries of NSAIDs were between 61.7% and 125.7% at spiked levels of 1.0–500 μg/kg. The repeatability was less than 8% and the within-laboratory reproducibility was not more than 12.3%. The method was reliable, convenient and sensitive.     

Fast formation of thick and transparent titania nanotubular films from sputtered Ti

Ti films sputtered on transparent fluorine-doped tin oxide glass substrates were anodized in fluoride-containing organic electrolyte in the presence of H₂O. In this work, anodic TiO₂ nanotubes (ATNs) as long as 9.2 ± 0.3 μm were obtained with high growth rate of 0.64 ± 0.3 μm min^?1. We demonstrated the optimum anodization conditions for ATN growth on foreign substrates, were within the range of 0.3–0.5% (wt) NH₄F, with 3–5% (vol) H₂O at 60 V. XPS and ICP-MS were utilized to elucidate the increase of thickness and volume expansion obtained from the sputtered Ti film to their ATN forms. The ATN films exhibited excellent uniformity and adhesion to the substrates.     

The process of immobilizing enzyme of glucose sensor based on diamond film

Considering the poor adhesion of electrode to substrate, diamond film as a new kind of substrate material was used to fabricate a glucose sensor. Particularly, the immobilizing enzyme was investigated in detail. SEM and XPS were chosen to identify whether organic functional groups were grafted to electrode surface or not. The response characteristics of a diamond film glucose sensor show that this glucose sensor has good properties in the linear range 0.5–11.4 mM l^-1, sensitivity 4.0 nA mM^-1 mm^-2 and peak reaction speed 2.5 μA. The glucose sensor based on diamond film was a novel microchip glucose sensor with good potential.     

Development and characterization of a titanosilicate ETS-10-coated optical fiber reactor towards the photodegradation of methylene blue

An optical fiber reactor (OFR) system containing uniformly distributed quartz fibers coated with titanosilicate ETS-10 crystals was investigated. Optimum ETS-10 film thickness (～1.5 μm) and coating length (15 cm) were determined from the light propagation analysis in a single ETS-10-coated fiber. The nearly constant value of the attenuation coefficient (α ≈ 0.10 cm^?1) for films with different thickness indicated uniform fiber surface coverage with these films. The extinction coefficient, ?, decreased from ～1.6 to ～1.0 μm^?1 with ETS-10 film thickness increasing from ～0.5 to ～1.5 μm, which suggested less contact per unit film thickness between light and ETS-10 crystals inside thicker films, likely due to their lower crystal packing density. Photodegradation of methylene blue (MB) conducted in the OFR showed higher photocatalytic activity for thicker ETS-10 films. Although higher MB photodegradation rates were obtained at higher light intensity, the apparent quantum efficiency, Φ, decreased with increasing light intensity. This is consistent with the charge separation mechanism for MB photodegradation in the UV light range investigated. All ETS-10 samples investigated showed ～4–5 times higher Φ values in the OFR than in the slurry reactor, likely due to the unique light/photocatalyst/reactant contact and high fiber packing density in the OFR.     

Bismuth nano-powder electrode for trace analysis of heavy metals using anodic stripping voltammetry

In the present work, a more sensitive and conveniently usable electrode sensor for a trace analysis of heavy metal was developed by using Bi nanopowder synthesized by levitational gas condensation (LGC) method. It was observed from the TEM image that the Bi nanopowder is spherical in shape with a size of nearly 50 nm. The XRD pattern revealed intense peaks which can be indexed as a rhombohedral structure of Bi without any other diffraction peaks corresponding to an oxide or an impurity. This indicates that the resulting nanopowder synthesized by the LGC method is a highly crystallized Bi with a high purity. The square wave anodic stripping voltammograms (SWASV), experimentally measured for the Bi nanopowder electrode, showed well-defined and highly reproducible electrochemical responses relating to the stripping of Cd and Pb. The detection limit of the electrode was estimated to be 0.15 μg/l and 0.07 μg/l for Cd and Zn, respectively, on the basis of the signal-to-noise characteristics (S/N = 3) of the response for the 1.0 μg/l solution under a 10 min accumulation.     

Surface structures and electrochemical characteristics of surface-modified carbon anodes for lithium ion battery

Petroleum coke and those heat-treated at 1860 °C, 2100 °C, 2300 °C 2600 °C and 2800 °C (abbreviated as PC, PC1860, PC2100, PC2300, PC2600 and PC2800) were fluorinated by elemental fluorine of 3 × 10⁴ Pa at 200 °C and 300 °C for 2 min. Natural graphite powder samples with average particle sizes of 5 μm, 10 μm and 15 μm (abbreviated as NG5μm, NG10μm and NG15μm) were also fluorinated by ClF₃ of 3 × 10⁴ Pa at 200 °C and 300 °C for 2 min. Transmission electron microscopic (TEM) observation revealed that closed edge of PC2800 was destroyed and opened by surface fluorination, which increased the first coulombic efficiencies of PC2300, PC2600 and PC2800 by 12.1–18.2% at 60 mA/g and by 13.3–25.8% at 150 mA/g in 1 mol/dm³ LiClO₄–ethylene carbonate (EC)/diethyl carbonate (DEC) (1:1 in volume). Light fluorination of NG10μm and NG15μm increased the first coulombic efficiencies by 22.1–28.4% at 150 mA/g in 1 mol/dm³ LiClO₄–EC/DEC/PC (PC: propylene carbonate, 1:1:1 in volume).     

Preliminary study for producing higher harmonic hard X-rays from weakly ionized nickel plasma

In the plasma flash X-ray generator, a 200 nF condenser is charged up to 50 kV by a power supply, and flash X-rays are produced by the discharging. The X-ray tube is a demountable triode with a trigger electrode, and the turbomolecular pump evacuates air from the tube with a pressure of approximately 1 mPa. Target evaporation leads to the formation of weakly ionized linear plasma, consisting of nickel ions and electrons, around the fine target, and intense Kα lines are left using a 15-μm-thick cobalt filter. At a charging voltage of 50 kV, the maximum tube voltage was almost equal to the charging voltage of the main condenser, and the peak current was about 18 kA. The K-series characteristic X-rays were clean and intense, and higher harmonic X-rays were observed. The X-ray pulse widths were approximately 300 ns, and the time-integrated X-ray intensity had a value of approximately 1.0 mGy at 1.0 m from the X-ray source with a charging voltage of 50 kV.     

Removal of suspended clay from water using transmembrane pressure pulsed microfiltration

Transmembrane pressure pulsing (TPP) uses the frequent and periodic reversal of the transmembrane pressure to reduce flux resistances due to membrane fouling. This study examined the effect of TPP on the microfiltration of simulated drinking water (hydrated aluminum silicate solution). Solutions of kaolin clay (0.1–4.0 μm particles, at an approximate concentration of 500 mg l⁻¹ and a turbidity of 402±17 NTU, 0.5 mM CaCl, 2.0 mM NaHCO₃, pH 7.5–7.8) were microfiltered with polyethersulfone (PES) 0.16 μm microfiltration membranes at an operating pressure of 30 kPa. Crossflow shear rates were varied between 165 and 1490 s⁻¹. Pulse frequency was varied between 0.3×10⁻² and 2 Hz, and pulse amplitude was varied between −3 and −16.5 kPa. It was found that the crossflow shear rates did not significantly effect the non-pulsed permeate flux. An optimum pulse amplitude of about 10 kPa was necessary to maximize the permeate flux for pulse frequencies between 0.3×10⁻² and 2.0 Hz. To insure a reduced solute flux, pulse frequencies less than 0.1 Hz were required. These results indicate that TPP can significantly reduce membrane fouling by inorganic particulate materials that are potentially important constituents of natural waters without negatively impacting the rejection of sub-micron particles due to interactions with material accumulated on the membrane.     

Lithium antimonite: A new class of anode material for lithium-ion battery

LiSbO₃ has been synthesized by chemical mixing followed by thermal treatment at 800 °C. Field emission scanning electron microscopy revealed bar shaped multifaceted grains, 0.5–4 μm long and 0.5–1 μm wide, that cluster together as soft agglomeration. 2032 type coin cell vs Li/Li⁺ shows a flat charge–discharge plateau together with low Li intercalation/de-intercalation potential (0.2/0.5 V). A high discharge capacity of 580 mA h g^?1 has been obtained in the 1st cycle with 100% Coulombic efficiency. About 96% of the Coulombic efficiency is retained up to the 12th cycle, but at the 15th cycle, the Coulombic efficiency drops down to 88%. AC impedance spectroscopy shows an increase in electrolyte resistance (R_s) from 4.43 Ohm after the initial cycle to 12.4 Ohm after the 15th cycle indicating a probable dissolution of Sb into the electrolyte causing the capacity fading observed.     

High performance cholesterol sensor based on ZnO nanotubes grown on Si/Ag electrodes

Zinc oxide nanotube (ZNT) arrays were grown on Si/Ag substrate by one-step chemical process in an aqueous solution and further used as a working electrode to fabricate an enzyme-based cholesterol biosensor through immobilization of cholesterol oxidase (ChOx). The fabricated biosensors exhibit high and reproducible sensitivity of 79.40 μA/mM/cm², wide linear range from 1.0 μM to 13.0 mM, fast response time of ~ 2 s and ultra-low detection limit of 0.5 nM (S/N = 3) for cholesterol sensing. The anti-interference ability and long-term stability of the biosensor were also assessed. Finally, the biosensor was applied to analyze cholesterol concentration in human serum samples.