Although ultrafiltration (UF) membranes are applicable in wastewater and water treatment, most UF membranes are hydrophobic and susceptible to severe fouling by natural organic matter. In this work, polysulfone (PSf) membrane was blended with silicaluminophosphate (SAPO) nanoparticles, SAPO-34, to study the effect of SAPO-34 incorporation in humic acid (HA) fouling mitigation. The casting solution was prepared by blending 5-20 wt% of SAPO-34 nanoparticles into the mixture of PSf, 1-methyl-2-pyrrolidinone and polyvinyl alcohol at 75 °C. All membrane samples were then prepared using the phase inversion method. Blending SAPO-34 zeolite into PSf membranes caused augmentation in surface hydrophilicity and pore size, leading to higher water permeation. In the HA filtration test, mixed matrix membranes (MMMs) with SAPO-34 zeolite showed reduced HA fouling initiated from pore blocking. The MMM with 20 wt% SAPO-34 loading exhibited the highest increment of water permeation (83%) and maintained about 75% of permeate flux after 2.5 h. However, the SAPO-34 fillers agglomerated in the PSf matrix and induced macrovoid formation on the membrane surface when excessive zeolite was added.
Non-covalent electrostatic interaction between amide nitrogen and carbonyl carbon of shorter chain length of polyvinylpyrrolidone (PVP-k25) was developed with in-house carboxylic oxidized multiwall carbon nanotubes (O-MWCNT) and then blended with Polyethersulfone (PES) polymer. FTIR analysis was utilized to confirm bonding nature of nano-composites (NCs) of O-MWCNT/PVP-k25 and casting membranes. Non-solvent induces phase separation process developed regular finger-like channels in composite membranes whereas pristine PES exhibited spongy entities as studied by cross sectional analysis report of FESEM. Further, FESEM instrument was also utilized to observe the dispersion of O-MWCNT/PVP based nanocomposite (NCs) with PES and membranes leaching phenomena analysis. Contact angle experiments described 24% improvement of hydrophilic behaviour, leaching ratio of additives was reduced to 1.89%, whereas water flux enhanced up to 6 times. Bovine serum albumin (BSA) and lysozyme based antifouling analysis shown up to 25% improvement, whereas 84% of water flux was regained after protein fouling than pristine PES. Anticoagulant activity was reported by estimating prothrombin, thrombin, plasma re-calcification times and production of fibrinogen cluster with platelets-adhesions photographs and hemolysis experiments. Composite membranes exhibited 3.4 and 3 times better dialysis clearance ratios of urea and creatinine solutes as compared to the raw PES membrane.
The development of wearable artificial kidney demands an efficient dialysate recovery, which relies upon the adsorption process. This study proposes a solution to solve the problem of competitive adsorption between the uremic toxins by employing two adsorptive components in a membrane separation process. Dual-layer hollow fiber (DLHF) membranes, which are composed of a polysulfone (PSf)/activated carbon (AC) inner layer and a PSf/poly(methyl methacrylate) (PMMA) outer layer, were prepared for co-adsorptive removal of creatinine and urea from aqueous solution. The DLHF membranes were characterized in terms of morphological, physicochemical, water transport, and creatinine adsorption properties. The membrane was then subjected to an ultrafiltration adsorption study for performance evaluation. The incorporation of AC in membrane, as confirmed by microscopic and surface analyses, has improved the pure water flux up to 25.2 L/(m2 h). A membrane with optimum AC loading (9 wt %) demonstrated the highest maximum creatinine adsorption capacity (86.2 mg/g) based on the Langmuir adsorption isotherm model. In the ultrafiltration adsorption experiment, the membrane removed creatinine and urea with a combined average percent removal of 29.3%. Moreover, the membrane exhibited creatinine and urea uptake recoveries of 98.8 and 81.2%, respectively. The combined action of PMMA and AC in the PSf DLHF membrane has made the adsorption of multiple uremic toxins possible during dialysate recovery.
Poly (citric acid)-grafted-MWCNT (PCA-g-MWCNT) was incorporated as nanofiller in polyethersulfone (PES) to produce hemodialysis mixed matrix membrane (MMM). Citric acid monohydrate was polymerized onto the surface of MWCNTs by polycondensation. Neat PES membrane and PES/MWCNTs MMMs were fabricated by dry-wet spinning technique. The membranes were characterized in terms of morphology, pure water flux (PWF) and bovine serum albumin (BSA) protein rejection. The grafting yield of PCA onto MWCNTs was calculated as 149.2%. The decrease of contact angle from 77.56° to 56.06° for PES/PCA-g-MWCNTs membrane indicated the increase in surface hydrophilicity, which rendered positive impacts on the PWF and BSA rejection of the membrane. The PWF increased from 15.8Lm(-2)h(-1) to 95.36Lm(-2)h(-1) upon the incorporation of PCA-g-MWCNTs due to the attachment of abundant hydrophilic groups that present on the MWCNTs, which have improved the affinity of membrane towards the water molecules. For protein rejection, the PES/PCA-g-MWCNTs MMM rejected 95.2% of BSA whereas neat PES membrane demonstrated protein rejection of 90.2%. Compared to commercial PES hemodialysis membrane, the PES/PCA-g-MWCNTs MMMs showed less flux decline behavior and better PWF recovery ratio, suggesting that the membrane antifouling performance was improved. The incorporation of PCA-g-MWCNTs enhanced the separation features and antifouling capabilities of the PES membrane for hemodialysis application.
The focus of this research is to study the potential of nanofiltration membrane technology in removing ammonia-nitrogen from the aquaculture system. One of the major fabrication parameters that directly affect the separation performance is shear rate or casting rate during membrane fabrication. In this study, asymmetric polyethersulfone (PES) nanofiltration membranes were prepared at five different shear rates within the range of 67-400 s(-1). Membrane productivity and separation performance were assessed via pure water, salt and ammonia-nitrogen permeation experiments, and their structural properties were determined by employing the combination of the irreversible thermodynamic (IT) model, solution diffusion model, steric hindrance pore (SHP) model and Teorell-Meyers (TMS) model. The study reveals that the alteration of shear rate enormously affects the membrane morphology and structural parameters, hence subsequently significantly influencing the membrane performance. It was found that, membrane produced at the shear rate 200 s(-1) or equivalent to 10s of casting speed during membrane fabrications managed to remove about 68% of ammonia-nitrogen, in which its separation performance is the most favourable by means of highest flux and rejection ability towards unwanted solutes. Besides, from the research findings, nano-membrane technology is a potential candidate for the treatment of aquaculture wastewater.
The cost of chemicals prohibits many technically feasible enhanced oil recovery methods to be applied in oil fields. It is shown that by-products from oil palm processing can be a source of valuable chemicals. Analysis of the pyrolysis oil from oil palm shells, a by-product of the palm oil industry, reveals a complex mixture of mainly phenolic compounds, carboxylic acids, and aldehydes. The phenolic compounds were extracted from the pyrolysis oil by liquid-liquid extraction using alkali and an organic solvent and analyzed, indicating the presence of over 93% phenols and phenolic compounds. Simultaneous sulfonation and alkylation of the pyrolysis oil was carried out to produce surfactants for application in oil fields. The lowest measured surface tension and critical micelle concentration was 30.2 mNm(-1) and 0.22 wt%, respectively. Displacement tests showed that 7-14% of the original oil in place was recovered by using a combination of surfactants and xanthan (polymer) as additives.
The objective of this research is to investigate the performance of blend cellulose acetate (CA)-polyethersulphone (PES) membranes prepared using microwave heating (MWH) techniques and then compare it with blend CA-PES membranes prepared using conventional heating (CH) methods using bovine serum albumin solution. The superior membranes were then used in the treatment of palm oil mill effluent (POME). Various blends of CA-PES have been blended with PES in the range of 1-5 wt%. This distinctive series of dope formulations of blend CA/PES and pure CA was prepared using N, N-dimethylformamide (DMF) as solvent. The dope solution was prepared by MW heating for 5 min at a high pulse and the membranes were prepared by phase inversion method. The performances of these membranes were evaluated in terms of pure water and permeate flux, percentage removal of total suspended solids (TSS), chemical oxygen demand (COD) and biochemical oxygen demand (BOD). The results indicate that blend membranes prepared using the microwave technique is far more superior compared to that prepared using CH. Blend membranes with 19% CA, 1-3% PES and 80% of DMF solvent were found to be the best membrane formulation.
Application of gas chromatography-triple quadrupole mass spectrometry for identification, confirmation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil, homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplements was investigated. The MS was operated in multiple reaction monitoring mode, for better sensitivity and selectivity. In this manner, the method is adequate to reduce background noise with less interference from co-eluting compounds in the samples. Two different ionisation techniques, electron ionisation (EI) and chemical ionisation (CI), were studied and compared. The chromatographic separation was performed on a short 10 m non-polar capillary column without any derivatisation step. This permitted fast analysis for all analogues with retention time less than 11 min, for both techniques. Use of backflushing can aid method retention time reduction and improves column maintenance. Evaluation of method validation included limit of detection (LOD), lower limit of quantitation (LLOQ), linearity, precision and recovery were performed for both EI and CI techniques. The LOD obtained varied from 0.03 to 1.50 μg/g and the LLOQ ranged from 0.10 to 5.00 μg/g. Good calibration linearity was obtained for all analogues for both techniques, with correlation coefficients (r(2)) higher than 0.99. Mean recoveries of all analogues using CI show higher values (83.4-108.8%) than that of EI (61.9-91.1%). The intra- and inter-assay precisions were evaluated for all analogues at spiked concentration of 10 μg/g and the relative standard deviation was less than 15% for both methods. These methods were then successfully applied to dietary supplement samples without prior derivatisation, confirming that the samples were adulterated with sildenafil and/or its analogues.
Polyethersulfone (PES) based membranes are used for dialysis, but exposure to blood can result in numerous interactions between the blood elements and the membrane. Adsorption and transformation of plasma proteins, activation of blood cells, adherence of platelets and thrombosis reactions against PES membrane can invoke severe blood reactions causing the increase rate of mortality and morbidity of hemodialysis (HD) patients. In order to minimize blood immune response, different biomimetic, zwitterionic, non-ionic, anticoagulant molecules and hydrophilic brushes were immobilized or blended with PES polymers. These additives modified the nature of the membrane, enhanced their biocompatibility and also increased the uremic waste dialysis properties. In this review, current perspectives of the different additives which are used with PES are highlighted in relation with PES membrane-associated blood reactions. The additive's purpose, compatibility, preparation techniques, methods of addition to polymer and influence on the chemistry and performance of hemodialysis membranes are described.
In this study, laundry wastewater filtration was studied using hydrophilic polyvinylpyrollidone (PVP) modified polyethersulfone (PES) ultrafiltration membranes. The performances of PES/PVP membranes were assessed using commercial PES membrane with 10kDa in ultrafiltration. Operating parameters The influence of transmembrane pressure (TMP) and stirring speed on laundry wastewater flux was investigated. A higher permeate flux of 55.2L/m(2)h was obtained for modified PES membrane with high concentration of PVP at TMP of 500kPa and 750rpm of stirring speed. The separation efficiencies of membranes were also studied with respect to chemical oxygen demand (COD), total dissolved solids (TDS), turbidity and conductivity. Results showed that PES membrane with 10% of PVP had higher permeate flux, flux recovery and less fouling when compared with other membranes. Higher COD and TDS rejection of 88% and 82% were also observed for modified membranes due to the improved surface property of membranes. This indicated that modified PES membranes are suitable for the treatment of surfactant, detergent and oil from laundry wastewater.
In this study, improvement of urea and creatinine permeability of polyethersulfone (PES) membrane by coating with synthesized tripolyphosphate-crosslinked chitosan (TPP-CS) has been conducted. Original and modified membranes, e.g. pristine PES, polyethersulfone-polyethylene glycol (PES-PEG) and PES-PEG/TPP-CS membranes were characterized using FTIR, DTG, SEM, AFM, water uptake, contact angles, porosity measurement, tensile strength test and permeation tests against urea and creatinine. The results show that the PES modification by TPP-CS coating has been successfully carried out. The water uptake ability, hydrophilicity and porosity of the modified membranes increase significantly to a greater degree. All modified membranes have good thermal stability and tensile strength and their permeation ability towards urea and creatinine increase with the increasing concentration of TPP-CS. PES membrane has urea clearance ability of 7.36 mg/dL and creatinine of 0.014 mg/dL; membrane PES-PEG shows urea clearance of 11.87 mg/dL and creatinine of 0.32 mg/dL; while PES-PEG/TPP-CS membrane gives urea clearance of 20.87-36.40 mg/dL and creatinine in the range of 0.52-0.78 mg/dL. These results suggest that the PES-PEG membrane coated with TPP-CS is superior and can be used as potential material for hemodialysis membrane.
Novel series of disulfide and sulfone hybrid analogs (1-20) were synthesized and characterized through EI-MS and (1)H NMR and evaluated for β-glucuronidase inhibitory potential. All synthesized analogs except 13 and 15 showed excellent β-glucuronidase inhibitory potential with IC50 value ranging in between 2.20-88.16μM as compared to standard d-saccharic acid 1,4 lactone (48.4±1.25μM). Analogs 19, 16, 4, 1, 17, 6, 10, 3, 18, 2, 11, 14 and 5 showed many fold potent activity against β-glucuronidase inhibitor. Structure activity relationship showed that substitution of electron withdrawing groups at ortho as well as para position on phenyl ring increase potency. Electron withdrawing groups at meta position on phenyl ring showed slightly low potency as compared to ortho and para position. The binding interactions were confirmed through molecular docking studies.
In the current study, a phase inversion scheme was employed to fabricate hydroxyapatite (HA)/polysulfone (PSF)-based asymmetric membranes using a film applicator with water as a solvent and nonsolvent exchanging medium. Fourier Transform Infrared (FTIR) and X-ray diffraction (XRD) spectroscopic studies were conducted to confirm the bonding chemistry and purity of filler. The inherent thick nature of PSF generated sponge-like shape while the instantaneous demixing process produced finger-like pore networks in HA/PSF-based asymmetric membranes as exhibited by scanning electron microscope (SEM) micrographs. The FTIR spectra confirmed noncovalent weak attractions toward the polymer surface. The leaching ratio was evaluated to observe the dispersion behavior of HA filler in membrane composition. Hydrophilicity, pore profile, pure water permeation (PWP) flux, and molecular weight cutoff (MWCO) values of all formulated membranes were also calculated. Antifouling results revealed that HA modified PSF membranes exhibited 43% less adhesion of bovine serum albumin (BSA) together with >86% recovery of flux. Membrane composition showed 74% total resistance, out of which 60% was reversible resistance. Biocompatibility evaluation revealed that the modified membranes exhibited prothrombin time (PT), and thrombin time (TT) comparable with typical blood plasma, whereas proliferation of living cells over membrane surface proved its nontoxic behavior toward biomedical application. The urea and creatinine showed effective adsorption aptitude toward HA loaded PSF membranes.
Removal of low-concentration ammonia (1-10 ppm) from aquaculture wastewater was investigated via polysulfone (PSf)/zeolite mixed matrix membrane. PSf/zeolite mixed matrix membranes with different weight ratios (90/10, 80/20, 70/30 and 60/40 wt.%) were prepared and characterized. Results indicate that PSf/zeolite (80/20) was the most efficient membrane for removal of low-concentration ammonia. The ammonia elimination by PSf/zeolite (80/20) from aqueous solution for 10, 7, 5, 3 and 1 ppm of ammonia was 100%, 99%, 98.8%, 96% and 95% respectively. The recorded results revealed that pure water flux declined in higher loading of zeolite in the membrane matrix due to surface pore blockage caused by zeolite particles. On the other hand, ammonia elimination from water was decreased in higher contents of zeolite because of formation of cavities and macrovoids in the membrane substructure.
To develop a novel granular adsorbent to remove arsenic and antimony from water, calcined Mg/Al-layered double-hydroxide (CLDH)-incorporated polyethersulfone (PES) granular adsorbents (PES-LDH) were prepared using a core-shell method having 25% PES in an N,N-dimethylformamide solution. The PES-LDH displayed a spherical hollow shape having a rough surface and the average particle size of 1-2 mm. On the PES-LDH surface, nanosized CLDH (100-150 nm) was successfully immobilized by consolidation between PES and CLDH. The adsorption of Sb(V) by PES-LDH was found to be more favorable than for As(V), with the maximum adsorption capacity of As(V) and Sb(V) being 7.44 and 22.8 mg/g, respectively. The regeneration results indicated that a 0.5 M NaOH and 5 M NaCl mixed solution achieved an 80% regeneration efficiency in As(V) adsorption and desorption. However, the regeneration efficiency of Sb(V) gradually decreased due to its strong binding affinity, even though the PES-LDH showed much higher Sb(V) adsorption efficiency than As(V). This study suggested that PES-LDH could be a promising granular adsorbent for the remediation of As(V) and Sb(V) contained in wastewater.
Polyethersulphone (PES) membranes blended with silicon dioxide (SiO2) nanoparticles were prepared via a dry-jet wet spinning technique for the removal of bisphenol A (BPA) by adsorption mechanism. The morphology of SiO2 nanoparticles was analysed using a transmission electron microscopy and particle size distribution was also analysed. The prepared membranes were characterized by several techniques including field emission scanning electron microscopy, Fourier transform infrared spectroscopy and water contact angle. The adsorption mechanism of membrane towards BPA was evaluated by batch experiments and kinetic model. The influence of natural organic matter (NOM) in feed water on membrane BPA removal was also studied by filtration experiments. Results showed that BPA adsorption capacity as high as 53 µg/g could be achieved by the PES membrane incorporated with 2 wt% SiO2 in which the adsorption mechanism was in accordance with the pseudo-second-order kinetic model. The intraparticles diffusion model suggested that the rate limiting factor of membrane adsorption mechanism is governed by the diffusion of BPA into the membrane pores. The presence of 10 ppm NOM has reported to negatively reduce BPA removal by 24%, as it tended to compete with BPA for membrane adsorption. This work has demonstrated that PES-SiO2 membrane has the potential to eliminate trace amount of BPA from water source containing NOM.
Sildenafil analogues have been found adulterated in herbal preparations and food products that claim to have natural aphrodisiacs. In this study, a gas chromatography-mass spectrometry (GC-MS) assay was developed for the screening and identification of thioketone analogues of sildenafil. Thiopyrazolopyrimidine, a precursor or a cleavage product of thioketone analogue, exhibited characteristic fragment ions of m/z 328 and m/z 299 was found to be the best marker to screen the presence of general thioketone analogues. Identification by GC-MS assay was rapid and specific as all the studied thioketones showed characteristic mass fragmentations including their intact molecular ions. The developed GC-MS assay had successfully identified thiosildenafil, thiohomosildenafil and thiodimethylsildenafil in herbal preparation and food products.
Sildenafil and its analogues (tadalafil and vardenafil) are phosphodiesterase type 5 inhibitors used in the treatment of male erectile dysfunction. Some dietary supplements, herbal preparations and food products which claim to enhance male sexual function have been found to be adulterated with these drugs. In this study, a gas chromatograph-mass spectrometer (GC-MS) assay was developed for identification of the drugs. In addition to good and short chromatographic separation that can be achieved within 6 min by using a short 10 m capillary column, no prior sample clean-up before GC-MS analysis was required, thus making this assay a cost saving and rapid method. Furthermore, the assay is specific as the identification of sildenafil, tadalafil and vardenafil were done by detection of molecular ions; m/z 474, 389 and 488, [corrected] respectively, and several other characteristic ions resulted from the mass fragmentation of individual molecules. Using our currently developed assay, sildenafil and its analogues were successfully identified in food and herbal matrices.
In this study, modified polyethersulfone (PES) and cellulose acetate (CA) membranes were used in the treatment of car wash effluent using ultrafiltration. Hydrophilic sulfonated poly ether ether ketone (SPEEK) and bentonite as nanoclay were used as additives for the PES and CA membrane modification. Performances of modified membranes were compared with commercial PES membrane with 10kDa molecular weight cut off (MWCO). The influencing parameters like stirrer speed (250-750rpm) and transmembrane pressure (100-600kPa) (TMP) were varied and their effects were studied as a function of flux. In the treatment of car wash effluent, a higher permeate flux of 52.3L/m(2)h was obtained for modified CA membrane at TMP of 400kPa and stirrer speed of 750rpm. In comparison with modified PES membrane and commercial PES membrane, modified CA membranes showed better performance in terms of flux and flux recovery ratio. The highest COD removal (60%) was obtained for modified CA membrane and a lowest COD removal (47%) was observed for commercial PES membrane. The modified membranes were better at removing COD, turbidity and maintained more stable flux than commercial PES membrane, suggesting they will provide better economic performance in car wash effluent reclamation.
Surfactants are multifunctional molecules widely used in personal care and healthcare formulations to cleanse, help disperse active ingredients (e.g., forming emulsions) and stabilise products. With increasing demands on improving biosafety, there is now mounting pressure to understand how different surfactants elicit toxicities at molecular and cellular levels. This work reports the membrane-lytic behaviour of a group of sulphonated methyl ester (SME) surfactants together with representative conventional surfactants. All surfactants displayed the clear rise of lysis of the model lipid bilayer membranes around their CMCs, but the two ionic surfactants SDS and C12TAB even caused measurable lysis below their CMCs, with membrane-lytic actions increasing with monomer concentration. Furthermore, whilst ionic and nonionic surfactants could achieve full membrane lysis once above their CMCs, this ability was weak from the SME surfactants and decreased with increasing the acyl chain length. In contrast to the conventional anionic surfactants such as SDS and SLES, the protein solubilizing capability of the SME surfactants was also low. On the other hand, MTT assays against 3T3 fibroblast cells and human chondrocyte cells revealed high toxicity from SDS and C12TAB against the other surfactants studied, but the difference between SME and the rest of conventional surfactants was small. Similar behaviour was also observed in their bactericidal effect against E. coli and S. aureus. The trend is broadly consistent with their membrane-lytic behaviour, indicating little selectivity in their cytotoxicity and bactericidal action. These results thus reveal different toxicities implicated from different surfactant head groups. Increase in acyl chain length as observed from SME surfactants could help improve surfactant biocompatibility.