Synthesis of NaA zeolite membranes from clear solution

NaA zeolite membranes were successfully synthesized on a porous alpha -Al2O3 support from clear solution. The synthesis parameters, such as surface seeding, synthesis time, synthesis stages, etc. were investigated. Surface seeding can not only accelerate the formation of NaA zeolite on the support surface, but can also inhibit the transformation of NaA zeolite into other types of zeolites. A continuous NaA zeolite membrane formed on the seeded support after 2 h of synthesis. Gas permeation results showed that a synthesis time of 3 h produced the best NaA zeolite membrane. When the synthesis time was longer than 4 h, the NaA zeolite on the support surface began to transform into other types of zeolites, and the quality of the NaA zeolite membrane decreased. The quality of the NaA zeolite membrane can be improved by employing the multi-stage synthesis method. The NaA zeolite membrane with a synthesis time of 2 h after a two-stage synthesis showed the best gas permeation performance. The permeances of H-2, O-2, N-2, and n-C4H10 decreased as the molecular kinetic diameter of the gases increased. which showed the molecular sieving effect of the NaA zeolite membrane. The permselectivities of H-2/n-C4H10 and O-2/N-2 were 19.1 and 1.8, respectively. These values are higher than the Knudsen diffusion ratios of 5.39 and 0.94. However, the permeation of n-C4H10 also indicated that the NaA zeolite membrane had certain defects with diameters larger than the pore size of NaA zeolite. A synthesis model was proposed to clarify the effect of surface seeding. (C) 2001 Elsevier Science B.V. All rights reserved.

Desenvolupament de mètodes de preconcentració emprant membranes líquides suportades i extracció en fase sòlida per a la determinació de l'herbicida glifosat i el seu metabòlit AMPA en aigües naturals

El glifosat, N-(fosfonometil) glicina, és un dels herbicides més utilitzats arreu del món a causa de la seva baixa toxicitat i al seu ampli espectre d'aplicació. A conseqüència del gran ús que se'n fa, és necessari monitoritzar aquest compost i el seu principal metabòlit, l'àcid aminometilfosfònic (AMPA), en el medi ambient. S'han descrit diversos mètodes instrumentals basats en cromatografia de gasos (GC) i de líquids (HPLC), sent aquesta darrera l'opció més favorable a causa del caràcter polar dels anàlits. Per assolir nivells de concentració baixos cal, però, la preconcentració dels anàlits. En aquest treball s'estudien diferents alternatives amb aquest objectiu. S'ha avaluat la tècnica de membrana líquida suportada (SLM) on la membrana consisteix en una dissolució orgànica, que conté un transportador (en el nostre cas, un bescanviador d'anions comercial, Aliquat 336), que impregna un suport polimèric microporós que se situa entre dues solucions aquoses: la de càrrega, que conté els anàlits inicialment, i la receptora, on es retenen els anàlits després del seu transport a través de la membrana. Les condicions d'extracció més adequades s'obtenen treballant en medi bàsic amb NaOH on els anàlits estan en forma aniònica i les majors recuperacions s'obtenen amb HCl 0,1 M o NaCl 0,5 M, la qual cosa indica que l'ió clorur és la força impulsora del transport. Un cop dissenyat el sistema, es duen a terme experiments de preconcentració amb dues geometries diferents: un sistema de membrana laminar (LSLM) on recircula la fase receptora i un sistema de fibra buida (HFSLM). Els millors resultats s'obtenen amb el mòdul de fibra buida, amb factors de concentració de 25 i 3 per a glifosat i AMPA, respectivament, fent recircular durant 24 hores 100 ml de solució de càrrega i 4 ml de solució receptora. També s'aplica una tècnica més selectiva, la cromatografia d'afinitat amb ió metàl·lic immobilitzat (IMAC), basada en la interacció entre els anàlits i un metall immobilitzat en una resina a través d'un grup funcional d'aquesta. En aquest estudi s'immobilitza pal·ladi al grup funcional 8-hidroxiquinoleïna de la resina amb matriu acrílica Spheron Oxine 1000 i s'avalua per a l'extracció i preconcentració de glifosat i AMPA. Per a ambdós anàlits l'adsorció és del 100 % i les recuperacions són superiors al 80 % i al 60 % per a glifosat i AMPA, respectivament, utilitzant HCl 0,1 M + NaCl 1 M com a eluent. Aquests resultats es comparen amb els obtinguts amb dues resines més, també carregades amb pal·ladi: Iontosorb Oxin 100, que té el mateix grup funcional però matriu de cel·lulosa, i Spheron Thiol 1000, on el grup funcional és un tiol i la matriu també és acrílica. Per al glifosat els resultats són similars amb totes les resines, però per a l'AMPA la resina Spheron Thiol és la única que proporciona recuperacions superiors al 93 %. Finalment, una altra opció estudiada és l'acoblament de dues columnes de cromatografia líquida (LC-LC). En l'estudi l'objectiu és millorar el mètode existent per a glifosat i AMPA en aigües naturals on el LOD era de 0,25 ug/l. El mètode consisteix en la derivatització precolumna amb el reactiu fluorescent FMOC i l'anàlisi amb l'acoblament LC-LC-fluorescència. Variant lleugerament les condicions de derivatització s'aconsegueix quantificar 0,1 ug/l de glifosat i AMPA. Es fortifiquen aigües naturals amb 0,1, 1 i 10 ug/l dels anàlits per validar el mètode. S'obtenen recuperacions d'entre el 85 % i el 100 %, amb desviacions estàndard relatives inferiors al 8 %. Aplicant una tècnica de preconcentració prèvia a la derivatització i anàlisi utilitzant una resina de bescanvi aniònic, Amberlite IRA-900, es millora la sensibilitat del mètode i s'assoleix un LOD per al glifosat de 0,02 ug/l.

Preparation of SnO2 supported membranes with ultrafine pores

The colloidal route of the sol-gel process was used to prepare supported SnO2 membranes. The influence of the sol and monoelectrolyte concentrations on the formation of the gel layer by sol-casting on the top of macroporous alpha-Al2O3 support was described. The stability of the colloidal suspension as a function of the concentrations was analyzed from creep-recovery measurements. The calcined supported membranes were characterized by nitrogen adsorption-desorption isotherms and scanning electron microscopy. The set of results show that homogeneous membrane layers containing the smallest quantity of cracks are formed in a critical interval of sol (1.01 less than or equal to[SnO2]less than or equal to 1.4 M) and electrolyte (2.O less than or equal to[Cl-]less than or equal to 4.0 mM) concentrations. The samples prepared from concentrated suspensions present a lot of interconnected cracks which favors the peeling of the coated layer. The membranes have pores of average diameter of about 1 nm.

Reconstruction of Mandibular Segmental Defects Using the Guided-Bone Regeneration Technique With Polylactide Membranes and/or Autogenous Bone Graft: A Preliminary Study on the Influence of Membrane Permeability

Purpose: Bone maintenance after mandibular reconstruction with autogenous iliac crest may be disappointing due to extensive resorption in the long term. The potential of the guided-bone regeneration (GBR) technique to enhance the healing process in segmental defects lacks comprehensive scientific documentation. This study aimed to investigate the influence of polylactide membrane permeability on the fate of iliac bone graft (BG) used to treat mandibular segmental defects. Materials and Methods: Unilateral 10-mm-wide segmental defects were created through the mandibles of 34 mongrel dogs. All defects were mechanically stabilized, and the animals were divided into 6 treatment groups: control, BG alone, microporous membrane (poly L/DL-lactide 80/20%) (Mi); Mi plus BG; microporous laser-perforated (15 cm2 ratio) membrane (Mip), and Mip plus BG. Calcein fluorochrome was injected intravenously at 3 months, and animal euthanasia was carried out at 6 months postoperatively. Results: Histomorphometry showed that BG protected by Mip was consistently related to larger amounts of bone compared with other groups (P ≤ .0001). No difference was found between defects treated with Mip alone and BG alone. Mi alone rendered the least bone area and reduced the amount of grafted bone to control levels. Data from bone labeling indicated that the bone formation process was incipient in the BG group at 3 months postoperatively regardless of whether or not it was covered by membrane. In contrast, GBR with Mip tended to enhance bone formation activity at 3 months. Conclusions: The use of Mip alone could be a useful alternative to BG. The combination of Mip membrane and BG efficiently delivered increased bone amounts in segmental defects compared with other treatment modalities. © 2008 American Association of Oral and Maxillofacial Surgeons.

Permeation of binary gas mixtures in ultramicroporous membranes

High-quality nanometer thick ultramicroporous membranes were prepared from silica sol-gel processes and tested for the permeation of binary gas mixtures of He, H-2, CO2, and CH4 across different temperature and partial pressure regimens. Pore size distribution by molecular probing showed that the majority of pore sizes had dimensions below 2.9 Angstrom. In 50:50 binary mixtures, the fluxes of gases increased as a function of temperature, indicating an activated transport mechanism. The ultramicroporous membranes showed high selectivities at 150 degreesC for He/CO2 (30), He/CH4 (93), H-2/CO2 (10), and H-2/CH4 (9) with lower selectivities for CO2/CH4 (5). High activation energies (E-a) were observed for the permeance of 50:50 binary mixtures containing He and H-2 of 22.1-27.5 and 17.6-23.1 kJ.mol(-1), respectively. The E-a for the permeance of the total mixture approached the E-a for the permeance of the molecule with the smaller kinetic diameter (He or H-2).

High-performance ceramic membranes with a separation layer of metal oxide nanofibers

In conventional fabrication of ceramic separation membranes, the particulate sols are applied onto porous supports. Major structural deficiencies under this approach are pin-holes and cracks, and the dramatic losses of flux when pore sizes are reduced to enhance selectivity. We have overcome these structural deficiencies by constructing hierarchically structured separation layer on a porous substrate using lager titanate nanofibers and smaller boehmite nanofibers. This yields a radical change in membrane texture. The resulting membranes effectively filter out species larger than 60 nm at flow rates orders of magnitude greater than conventional membranes. This reveals a new direction in membrane fabrication.

Ceramic membranes for separation of proteins and DNA by in situ growth of alumina nanofibres with a nanomesh of metal oxide nanofibres

Ceramic membranes were fabricated by in situ synthesis of alumina nanofibres in the pores of an alumina support as a separation layer, and exhibited a high permeation selectivity for bovine serum albumin relative to bovine hemoglobin (over 60 times) and can effectively retain DNA molecules at high fluxes.

High-flux ceramic membranes with a nanomesh of metal oxide nanofibers

Traditional ceramic separation membranes, which are fabricated by applying colloidal suspensions of metal hydroxides to porous supports, tend to suffer from pinholes and cracks that seriously affect their quality. Other intrinsic problems for these membranes include dramatic losses of flux when the pore sizes are reduced to enhance selectivity and dead-end pores that make no contribution to filtration. In this work, we propose a new strategy for addressing these problems by constructing a hierarchically structured separation layer on a porous substrate using large titanate nanofibers and smaller boehmite nanofibers. The nanofibers are able to divide large voids into smaller ones without forming dead-end pores and with the minimum reduction of the total void volume. The separation layer of nanofibers has a porosity of over 70% of its volume, whereas the separation layer in conventional ceramic membranes has a porosity below 36% and inevitably includes dead-end pores that make no contribution to the flux. This radical change in membrane texture greatly enhances membrane performance. The resulting membranes were able to filter out 95.3% of 60-nm particles from a 0.01 wt % latex while maintaining a relatively high flux of between 800 and 1000 L/m2·h, under a low driving pressure (20 kPa). Such flow rates are orders of magnitude greater than those of conventional membranes with equal selectivity. Moreover, the flux was stable at approximately 800 L/m2·h with a selectivity of more than 95%, even after six repeated runs of filtration and calcination. Use of different supports, either porous glass or porous alumina, had no substantial effect on the performance of the membranes; thus, it is possible to construct the membranes from a variety of supports without compromising functionality. The Darcy equation satisfactorily describes the correlation between the filtration flux and the structural parameters of the new membranes. The assembly of nanofiber meshes to combine high flux with excellent selectivity is an exciting new direction in membrane fabrication.

Metal oxide nanofibres membranes assembled by spin-coating method

Ceramic membranes are of particular interest in many industrial processes due to their ability to function under extreme conditions while maintaining their chemical and thermal stability. Major structural deficiencies under conventional fabrication approach are pin-holes and cracks, and the dramatic losses of flux when pore sizes are reduced to enhance selectivity. We overcome these structural deficiencies by constructing hierarchically structured separation layer on a porous substrate using larger titanate nanofibres and smaller boehmite nanofibres. This yields a radical change in membrane texture. The differences in the porous supports have no substantial influences on the texture of resulting membranes. The membranes with top layer of nanofibres coated on different porous supports by spin-coating method have similar size of the filtration pores, which is in a range of 10–100 nm. These membranes are able to effectively filter out species larger than 60 nm at flow rates orders of magnitude greater than conventional membranes. The retention can attain more than 95%, while maintaining a high flux rate about 900 L m-2 h. The calcination after spin-coating creates solid linkages between the fibres and between fibres and substrate, in addition to convert boehmite into -alumina nanofibres. This reveals a new direction in membrane fabrication.

Fouling of tubular ceramic membranes during processing of cane sugar juice

This paper examines the fouling characteristics of four tubular ceramic membranes with pore sizes 300 kDa, 0.1 μm and 0.45 μm installed in a pilot plant at a sugar factory for processing clarified cane sugar juices. All the membranes, except the one with a pore size of 0.45 μm, generally gave reproducible results through the trials, were easy to clean and could handle operation at high volumetric concentration factors. Analysis of fouled and cleaned ceramic membranes revealed that polysaccharides, lipids and to a lesser extent, polyphenols, as well as other colloidal particles cause fouling of the membranes. Electrostatic and hydrophobic forces cause strong aggregation of the polymeric components with one another and with colloidal particles. To combat irreversible fouling of the membranes, treatment options that result in the removal of particles having a size range of 0.2–0.5 μm and in addition remove polymeric impurities, need to be identified. Chemical and microscopic evaluations of the juices and the structural characterisation of individual particles and aggregates identified options to mitigate the fouling of membranes. These include conditioning the feed prior to membrane filtration to break up the network structure formed between the polymers and particles in the feed and the use of surfactants to prevent the aggregation of polymers and particles.

Sensitivity of Dot-ELISA on Nitrocellulose Membranes in Comparison with ELISA on Polystyrene Plates for the Detection of Four Plant Viruses

ABSTR.4CT Senitivity of dot-immunobindinding ELf SA on nitrocellulose membrane (DotELISA)was compared with double-antibody sandwich ELISA (DAS-ELlSA) on polystyrene plates for the detection of bean yellow mosaic virus (BYMV), broad bean stain virus (WMV-2). Dot-ELISA was 2 and 1O times more sensitive than DAS-ELISA for the detection of BBSV and WMV-2, respectively, whereas DAS-ELISA was more sensitive than Dot-ELiSA for {he detection of BYMV. Both techniques were equally sensitive for the detection of BYDV. Using one day instead uf the two-day procedure, the four viruses were still detectable and the ralative sensitivity of both techniques remained the same.