Multiple Ion Exchange Column Tests for Cesium (CS+) Removal from Hanford Site Tank 241‐AW‐101 with SuperLig® 644 Resin

Abstract

Six cycles of loading, elution, and regeneration were performed to remove cesium (Cs⁺) from a Hanford Site tank waste sample using SuperLig^® 644 resin. The sample, which was retrieved from Tank 241‐AW‐101, was diluted to 5.09 M Na⁺ and processed through dual ion exchange columns to remove ¹³⁷Cs. Each column had an inside diameter of 1.45 cm and a height of 30 cm; and contained 15 mL of wet resin in the sodium form. The columns, designated as primary (lead) and polishing (lag), were connected in series during loading, but they were separated during elution and regeneration. The cesium loading on the primary column during the six cycles ranged from 160 to 225 bed volumes (BV) at <50% breakthrough. A gradual decline of the resin loading performances was observed as a function of number of loading cycles. For all cycles, the percent removal of cesium (¹³⁷Cs) was greater than 99.99% and the decontamination factors (DFs) achieved were higher than 1.0 × 10⁴. Elution of the resin with 0.5 M nitric acid at 25 ± 2°C was effective. Approximately 99% of the ¹³⁷Cs bound on the resin was eluted with less than 15 BV of the eluent (0.5 M nitric acid). The cumulative dose absorbed by the resin in the primary column was 1.99 × 10⁷ rad with a 20% loss of ion exchange capacity was at 50% breakthrough after completing six loading cycles.     

Preparation and Characterization of Theophylline‐Imprinted Monolithic Column

Abstract

Monolithic molecularly imprinted column was prepared by an in‐situ therm‐initiated copolymerization and the effects of essential preparation conditions such as polymerization mixture composition and polymerization condition was investigated. The results showed that the selection of correct porogenic solvents and appropriate polymerization conditions are crucial for the preparation of the monolithic stationary phases. The separation efficiency was only extremely weakly dependent on flow rate and hydrogen‐bonding interaction played an important role in the retention and separation. Compared with conventional particle columns and bulk molecular imprinted polymer column, the monolithic column exhibited good stability, ease of regeneration, high separation efficiency, and fast analysis.     

Synthesis and Characterization of Dicyclopentadiene – cresol Epoxy Resin

Summary Starting from cresol, the synthesis of dicyclopentadiene (DCPD) – cresol epoxy resin was conducted. DCPD-containing phenol resin (DPR) was prepared via Friedel–Crafts alkylation, whereas DCPD-containing epoxy resin (DER) was prepared via epoxidation of DPR with epichlorohydrin. The chemical structure was characterized with FTIR and ¹HNMR. Cure behaviors and glass transition temperature (T_g) of the resulting polymers were studied by differential scanning calorimeter (DSC). The results clearly indicated that cured polymer with a mixture of DCPD-cresol epoxy resin and diglycidyl ether of bisphenol A (E51) had higher T_g comparing with E51.     

Diphonix® Resin: A Review of Its Properties and Applications

Abstract

The recently developed Diphonix® resin is a new multifunctional chelating ion exchange resin containing geminally substituted diphosphonic acid ligands chemically bonded to a styrene-based polymeric matrix. Diphonix can be regarded as a dual mechanism polymer, with a sulfonic acid cation exchange group allowing for rapid access, mostly non-specific, of ions into the polymeric network, and the diphosphonic acid group responsible for specificity (recognition) for a number of metal cations. The Diphonix resin exhibits an extraordinarily strong affinity for actinides, especially in the tetra- and hexavalent oxidation states. Therefore the resin has potential for applications in TRU and mixed waste treatment and characterization, and in the development of new procedures for rapid actinide preconcentration and separation from environmental samples. Metal uptake studies have been extended to alkaline earth cations, to transition and post-transition metal species, and to metal sorption from neutral or near neutral solutions. Also the kinetic behavior of the resin has been investigated in detail. In view of the above applications the influence of the most commonly occurring matrix constituents (Na, Ca, Al, Fe, hydrofluoric, sulfuric, oxalic and phosphoric acids) on the uptake of actinide ions has been measured. This review paper summarizes the most important results obtained in the studies on the properties of the Diphonix resin and gives an overview of the applications already in existence or under development in the fields of mixed waste treatment, actinide separation procedures, treatment of radwaste from nuclear power and fuel processing plants, and removal of iron from copper electrowinning solutions.

     

Preparation and Characterization of Two-component Waterborne Poly-urethane Comprised of Water-soluble Acrylic Resin and HDI Biuret

A two-component waterborne polyurethane （2K-WPU） was prepared by mixing water-soluble acrylic resin and hexamethylene diisocyanate biuret, and then diluted for phase inversion with water. Compared with water-soluble acrylic resin, the phase inversion of 2K-WPU occurs at lower water content. It is indicated by TEM that 2K-WPU particles show a core-shell structure, in which HDI biuret is encapsulated by hydrophilic acrylic resin. 2K-WPU emulsion with HDI biuret has larger particle size and narrower distribution index, while for 2K-WPU emulsion with HDI isocyanurate, the latex not only has large particle size, but also has two-peak distribution. FTIR shows that the reaction between HDI biuret and acrylic resin can complete in 12h. In addition, studies on effect of composition of acrylic resin on performance of 2K-WPU show that narrowing the polar difference between water-soluble acrylic resin and HDI biuret and improving the miscibility of two components are the key to prepare the transparent and high gloss films with high crosslinking density.     

Preconcentration and Determination of Copper in Aqueous Solution with Epoxy Resin‐based Monolithic Column Containing Large Interconnected Pores

Abstract

A novel monolithic column containing large interconnected pores was simply prepared from epoxy resin and triethylenetetramine (TETA) and pore‐forming reagent (polyethylene glycol, PEG‐1000) by in‐situ polymerization. PEG‐1000 was both solvent at the initial stage and phase‐separation reagent at the later stage of polymerization reaction. Its structure was characterized by Fourier transform‐infrared spectra (FTIR) and scanning electron microscopy (SEM), respectively. The results showed that the pore characteristics of monoliths depended strongly on the amount of PEG‐1000. A column method has been established for the preconcentration and determination of copper(II) combined with inductively coupled plasma atomic emission spectroscopy (ICP‐AES), using a simple glass‐tipped tube. The adsorption‐desorption characteristics of the monoliths for Cu(II) in aqueous solution were investigated in detail. The ion concentrations in batch adsorption experiments were determined by ICP‐AES. Copper ions could form complexes with the amino groups of the monoliths, and be quantitatively retained in the pH ranges of 5.0–9.0. The uploaded column was eluted by 1.0 mol L^?1 HNO₃ and recovery of Cu(II) was more than 97%.     

Batch Comparisons of Sr and Ba Retention and Capacities on AnaLig® Sr-01 and Eichrom Sr Resins

The isolation of strontium from aqueous media may be required for environmental monitoring or nuclear forensics sample analyses.^[1–4] The prevalent method is to use a strontium selective extraction chromatographic resin. Two such products are Eichrom Technologies Sr resin and IBC Advanced Technologies AnaLig® Sr-01 resin. Eichrom Technologies Sr resin utilizes a crown ether (4,4′(5′)-di-t-butylcyclohexano-18-crown-6) diluted in 1-octanol and coated onto Amberchrom^TM CG71 resin, and IBC Advanced Technologies AnaLig® Sr-01 resin features a proprietary extractant covalently tethered to a silica support. The use of each resin is reported in the literature; Eichrom Sr Resin specifications, including the resin’s weight distribution ratio and capacity factor for analytes, have been reported but no such data have been published for IBC Analig® Sr-01 resin. In this work, batch studies were completed to determine the capacity and weight distribution ratio of both AnaLig® Sr-01 and Eichrom Sr resins for strontium and barium. This work shows that both resins retained Sr from aqueous samples, but Eichrom Sr resin provided superior Sr/Ba separation compared with Analig® Sr-01 resin.     

Synthesis,Characterization and Ion–Exchanging Properties of Novel Ion-Exchange Resin,Part 1

A polyamine (PA) was prepared by condensation of 1,4-bischloromethyl benzene and 1,2-ehanedeamine. The PA was then treated with cyanuric chloride at 0°C followed by reaction with sulfanilic acid in THF in concentration. NaOH (PH 9–10) at room temperature for 8 h. The resultant polymer, designated as polyamine-s-triazine-sulfanilic acid (PATS), was characterized by elemental analysis, IR spectral studies, and thermogravimetry. The PATS sample was monitored for its ion-exchanging properties by batch equilibrium method.     

Antimicrobial Polychelates: Synthesis and Characterization of Transition Metal Chelated Barbituric Acid–Formaldehyde Resin

A monomeric Schiff base was prepared by the condensation reaction of salicylaldehyde and semicarbazide, which further react with formaldehyde and barbituric acid-formed polymeric Schiff base. Its metal polychelates were then formed with Mn(II), Co(II), Ni(II), Cu(II), and Zn(II). All the synthesized compounds were characterized by elemental analysis, magnetic moment, FTIR, ¹HNMR, and electronic spectroscopies. The elemental analysis data show the formation of 1:1 [M: L] metal polychelates. Thermogravimetric analysis was carried out to find the thermal behavior of all the synthesized polymeric compounds and thermal data revealed that all the metal polychelates are more thermally stable than their parent polymeric Schiff base. All the synthesized polymeric compounds were screened for antimicrobial activity against some clinically important microorganisms, such as Escherichia coli, Pseudomonas aeruginosa, Bacillus subtilis, Staphylococcus aureus, Staphylococcus typhi, Candida albicans, Microsporum canis, and Aspergillus niger. In vitro antimicrobial activity was determined by the Agar Well Diffusion method and the result shows that all the metal polychelates exhibited better antimicrobial activity than their parent polymeric Schiff base.     

A Vycor® Membrane with Reduced Size Surface Pores I. Preparation and Characterization

Vycor® membranes are surface-modified by a crosslinked commercial silicone which is subsequently subjected to oxygen plasma and converted to silica dioxide. Samples are examined by integral gas permeability of helium, nitrogen, methane and carbon dioxide, differential permeability of carbon dioxide and relative permeability of helium gas vs. water vapor. The modified surface is found to contain large micropores as well as a population of small nanopores. The new membrane may be appropriate for applications such as gas/vapor separations, reverse osmosis and the low molecular weight end of nanofiltration.     

Synthesis and Characterization of Mesostructured Silica Doped with Acyl‐Hydroxy‐Pyrazole Derivatives. Sorption Tests of Cu(II) and Eu(III)

Abstract

The synthesis and the characterization of mesostructured silica doped with acidic acyl‐hydroxy‐pyrazoles like extractants are described. The extractants have either a single chelating site, 1‐phenyl‐3‐methyl‐4‐stearoyl‐5‐hydroxy‐pyrazole (HPMSP), or two chelating sites, 1,12‐bis(1′‐phenyl‐3′‐methyl‐5′‐hydroxy‐4′‐pyrazolyl)‐dodecane‐1,12‐dione (HL‐10‐LH). The so‐called doped silicas were synthesized in basic medium according to a sol‐gel process beginning with the solubilization of the extractant in a micellar phase followed by the precipitation of silica around micelles. The chemical composition of the synthesized materials, especially the ligand content, was determined. High quantities of ligand loadings (up to 0.69 mol/kg) are reached. The materials obtained were characterized by X‐ray diffraction, laser granulometry, transmission and scanning electron microscopy and, after calcination, by nitrogen physisorption. Un‐doped silica is mesostructured, lamellar, and has high pore diameter as well as high specific surfaces. Doping induces the disorganization of the lamellar structure, the increase of the pore diameter, and a slight decrease of the specific surface. The capacities of extraction of Cu(II) and Eu(III) by the doped materials and the corresponding extraction rate were measured: high values are reached.     

Investigation of Structure and Oxidation Behavior of Pitch and Resin Resultant Carbon

The structure and oxidation behaviors of pitch carbon,resin carbon and their mixture re-sultant carbon have been investigated.The results indicate that the pitch carbon has relative higher true specific gravity,well developed crystalline and better oxidation resistance than resin carbon,With 20%-35% resin added to pitch,the structure of the resultant carbon can be modified and oxidation resistance will be improved significantly.     

Effects of Silanes Alone and Their Blends with HEMA on Resin–Titanium Bonding

Abstract

Two organofunctional silane coupling agents alone and two silane blend systems with HEMA were evaluated in vitro as adhesion promoters for bonding bis-GMA resin to a silica-coated titanium surface. The silanes were applied onto tribochemically silica-coated titanium surfaces. Experimental bis-GMA resin stubs were applied and photo-polymerized onto titanium. The specimens were subjected to three different conditions: (1) dry storage for 24 h, (2) storage in de-ionized water at 37°C for six months and (3) alternating storage in de-ionized water at 37°C and thermocycling (6000 cycles, 5–55°C) for 6 months. Shear bond strengths of the resin to titanium were measured using a universal testing machine. Surface examination was made with a scanning electron microscope (SEM) after the bond strength test. Highest shear bond strength was obtained with 3-acryloxypropyltrimethoxysilane stored in dry condition (20.2 ± 3.2MPa), and the lowest value was obtained with 3-methacryloxypropyltrimethoxysilane (ESPE Sil) in alternating water storage and thermocycling condition (1.4 ± 0.6 MPa). The type of storage condition affected significantly the shear bond strength (p < 0.05). The shear bond strength obtained from dry storage was the highest, while the shear bond strength obtained from alternating water storage and thermocycling condition was the lowest. Interfacial failure was the main failure mode (87.2%) followed by mixed failure (9.4%) and cohesive failure (3.4%). The addition of 0.5 vol%. HEMA into silane primers did not improve the shear bond strength between the experimental resin and silica-coated titanium.     

The Effect of Foreign Ions on Separation of Hafnium from Zirconium on Diphonix® Resin

The weight distribution coefficients (λ_M) of the most often occurring in zirconium salts ions (M(II), M(III) and M(IV)) have been determined in established earlier optimal conditions for separation of zirconium from hafnium by means of Diphonix® resin. Their values range from 21 (λ_Zn(II)) to 1830 (λ_Ti(IV)) and depend on the charge of M ion as well as on its radius. For ions of the highest λ_M (Ti(IV) and Fe(III)) their influence on hafnium – zirconium separation has been studied. Ti(IV) ions at concentration of 1% (in relation to Zr) has been found to noticeably affect separation of hafnium from zirconium by means of Diphonix® resin.     

Characterization of DSA®-type oxygen evolving electrodes: Choice of a coating

In the search for a DSA^®-type electrode for oxygen evolution in acidic solutions, nine binary coatings with IrO₂, RuO₂, Pt as conducting component, and TiO₂, ZrO₂, Ta₂O₅ as inert oxides, have been deposited on titanium, examined for their microstructural properties and tested for their electrocatalytic activity and anodic stability. Electrochemical true surfaces of the coatings were found to be dependent on structure and morphology: the mixtures that form a solid solution (RuO₂–TiO₂), or allow limited miscibility (IrO₂–TiO₂), show the lowest dispersion of active material. Differences in service lives, were attributed to differences in wear mechanism of the electrodes. It was found that Ti/IrO₂ (70 mol%)-Ta₂O₅ (30 mol%) is by far the best electrode.     

The Separation of Beryllium from Selected Elements Using the Dipex® Extraction Chromatographic Resin

Abstract

An extraction chromatographic resin containing the acidic chelating organophosphorus extractant, Dipex^®, sorbed onto an inert polymeric substrate has been evaluated for the separation of beryllium from a wide range of elements. The elements selected comprise those which can interfere with the determination of beryllium by inductively coupled plasma‐atomic emission spectroscopy (ICP‐AES) and matrix elements which commonly occur in environmental and industrial samples. Based on batch uptake measurements, a method that separates beryllium from all potential ICP‐AES spectral interfering elements using a single extraction chromatographic column is outlined. The chromatographic parameters of the separation method have been optimized using simulated samples generated using the digestion process employed in beryllium analyses by the Y‐12 National Security Complex and simulated ground water samples.     

Synthesis,Curing Behavior and Characterization of Epoxyacrylate and Triethylamine Cured Epoxy Resin of 1,1′-Bis(3-methyl-4-hydroxy phenyl) cyclohexane

Epoxy resin of 1,1′-bis(3-methyl-4-hydroxy phenyl) cyclohexane (EMC) and its acrylate (EMCA) have been synthesized and characterized. EMC has been cured by 5–25% triethyl amine at 100°C. The cured samples are characterized by solubility, IR, DSC and TGA at 10°C/min heating rate in nitrogen atmosphere. The associated kinetic parameters for EMCA, EMCT-5 and EMCT-20 have been determined according to Freeman-Anderson method and discussed. It is observed that EMCA and EMCT-20 have almost same thermal stability (300–308°C) but for EMCT-5 it is slightly lower (285°C). Cured samples followed fractional order degradation (0.63–1.44). In case of EMCT-5, all determined kinetic parameters are marginally lower than those of EMCA and EMCT-20.     

Synthesis and Characterization of Polyindole–NiO-Based Composite Polymer Electrolyte with LiClO4

There has been an increasing interest in synthesizing the novel composite polymer electrolyte (CPE) for use in lithium batteries in recent years. This paper describes the preparation and characterization of CPE containing lithium perchlorate based on polyindole–NiO nanocomposite. NiO nanoparticles were added to the monomer solution before the polymer formation in the presence of a surfactant to get the PInNiO nanocomposite. The thermal properties, surface morphology, and structural studies of the electrolyte were investigated by TGA, SEM, TEM, and XRD. An enhanced conductivity of 2.62 × 10^?4 S cm^?1 at 45°C for the composite polymer electrolyte was determined from impedance studies.     

Synthesis and Characterization of Nanoscale Mullite Powder

Nanoscale mullite powder were synthesized via solgel-SCFD and middle temperature treatment by using AIP (aluminum-isopropoxde)and TEOS(tetraethyl orthosilicate) as starting materials.Both of the binary aerogel of alumina-silica and calcined nanoscale materials were investigated by using TG-DSC(thermogravimetry-differential scanning calorimeter),TEM(transmission electron microscope),XRD(X-Ray diffractometer)and specific surface area and porosimetry.TG-DSC indicated the removal of most of the volatiles,i.e.15.98% up to about 700℃,and in the DSC curve,existence of two exothermic peak at about 445℃ and 1015℃ may be due to the crystallization of Si-O-Al-O in diphasic gels and mullitization and a small endothermic peak at about 805℃ indicated the decomposition of structural water molecules.On the colligation of the results of TG-DSC,XRD and TEM,the beginning temperature of mullitization in Al2O3-SiO2 aerogel system can be confirmed at about 1015℃.XRD results also showed the formation of mullite at the range 1100-1200℃.TEM and surface area and porosimetry results showed that the nanosized mullite were calcinated at 1100 and 1200℃ exhibited size 30nm and 50nm,specific surface area 138.91m^2/g and 95.81m^2/g.