The absorption of iodine-131 on a ceramic matrix

The retention of ¹³¹I on ceramic rod coated with silver nitrate followed by coating with a polyurethane membrane to be applied in brachytherapy was studied. The concentration of silver nitrate (20 g/l), the volume of ¹³¹I as a sodium iodide solution (100 µl), the pH of the reaction mixture (pH 9) etc., were optimized to get a maximum uptake on the ceramic rod. The concentration of coating solution (5%, polyurethane in tetrahydrofuran) was also optimized to obtain a minimum leaching of ¹³¹I activity in normal saline solution. After coating with a polyurethane membrane, the ¹³¹I absorbed on the ceramic rod exhibited low leachability (0.03%). This method can be applied for the preparation of ¹²⁵I interstitial sources to be used in eye and prostate cancer therapy.     

Formation of uniform silver particles from bis (1,2-ethanediamine)silver(I) complex

Uniform spherical silver particles were produced by decomposing the bis(1,2-ethanediamine)silver(I) complex, by aging a solution of 1.0×10^–3 mole dm^–3 in silver (I) nitrate, 1.0 mole dm^–3 in 1,2-ethanediamine, and 2.5×10^–1 mole dm^–3 in nitric acid (basic solution) at 100°C for 42 min. The average modal diameter was estimated to be 0.52 m with a relative standard deviation of 0.10. A moderately oxygenrich layer, 40 Å thick, on the surface of the particles was detected by means of photoelectron surface microanalysis (XPS). The silver particles grew through a polynuclear-layer mechanism, as judged from the concentration change in soluble silver(I) species in the supernatant solution. The particles' point of zero charge (PZC) was estimated at pH 6.5 by potentiometric titration.     

Argentimetric assay of captopril in bulk drug and in tablets

Three simple, selective and cost-effective procedures for the determination of captopril in bulk drug and in tablets are described. All the procedures make use of silver nitrate as a reagent and involve titrimetry and spectrophotometry as measurement techniques. In titrimetry (Method A), the aqueous solution of the drug is titrated directly with the standard silver nitrate solution to a potassium chromate end-point. In one spectrophotometric method (Method B), the sample solution is treated with excess of silver nitrate and a known amount of methyl orange and the increase in absorbance at 520 nm, caused by a decrease in pH due to release of nitric acid, is measured and related to drug concentration. The other spectrophotometric method (Method C) involves the addition of a measured excess of silver nitrate to the sample solution followed by the determination of residual silver ion by an ion-associate complex formation reaction involving eosin and 1,10-phenanthroline. The decrease in absorbance at 550 nm, which corresponds to Ag⁺ reacted with the drug, is measured and is found to be linearly related to drug concentration. All experimental variables involved in the methods were investigated and optimized. Stoichiometry of the reaction that forms the basis for titrimetry is found. Method A is applicable in the range of 1.0–20.0 mg of drug while methods B and C can be conveniently used in the concentration ranges of 2.5–50.0 and 0.25–4.0 μg ml^?1, respectively. Several optical characteristics such as molar absorptivity, Sandell sensitivity, limits of detection and quantification, and correlation coefficient were calculated. The methods were applied to the analysis of tablets containing captopril. Statistical treatment of the results indicates that the procedures are precise and accurate. The excipients used as additives in tablets did not interfere in the proposed procedures as revealed by the recovery studies.     

Indirect Determination of Sulfadiazine by Cloud Point Extraction/Flow Injection‐Flame Atomic Absorption (CPE/FI‐FAAS) Spectrometry

An indirect simple and rapid cloud point extraction is proposed for separation and preconcentration of sulfadiazine and its determination by flow injection‐flame atomic absorption spectroscopy (FI‐FAAS). The sulfadiazine from 35 mL of solution was readily converted to silver sulfadiazine upon addition of silver nitrate (9.7 × 10^‐5 mol/L). Then, Triton X‐114 a non ionic surfactant was added and the solution was heated to 60 °C. At this stage, two separate phases was formed and silver sulfadiazine enters the surfactant rich phase of non‐ionic micelles of Triton X‐114. The surfactant‐rich phase (～50 μL) was then separated and diluted to 300 μL with acidic methanol. The concentration of silver in the surfactant‐rich phase which is proportional to the concentration of sulfadiazine in sample solution was determined by FI‐FAAS. The parameters affecting extraction and separation were optimized. Under the optimum conditions (i.e. pH 2‐10, silver concentration (9.7 × 10 ^‐5 mol/L), Triton X‐114 (0.075% v/v) and temperature 60 °C) a preconcentration factor of 117 and a relative standard deviation of 4.9% at 37 μg L^‐1 of sulfadiazine was obtained. The method was successfully applied to analysis of milk, urine and tablet samples and accuracy was determined by recovery experiments.     

Potentiometric studies on organic compounds containing sulphur with a sulphide ion-selective membrane electrode

Phenylthiourea and N,N-diphenylthiourea can be determined in the concentration range 10¹–10^?3M by potentiometric titration with silver nitrate solution with a sulphide ion-selective membrane electrode. The influence of the alkali and acid concentration on the course of the reactions with the silver nitrate titrant was studied. When phenylthiourea is titrated in the presence of 0.1 M sodium hydroxide, silver sulphide is precipitated, and the phenylcyanamide formed simultaneously reacts further with silver nitrate to form a silver phenylcyanamide precipitate. When N,N-diphenylthiourea is titrated under similar conditions, silver sulphide is again formed, but no cyanamide-type compound can be formed owing to the presence of the second phenyl group. In 1 M sodium hydroxide both compounds studied react with two equivalents of silver to give silver sulphide and phenylurea or diphenylurea, respectively. In the presence of nitric acid both compounds react similarly with silver nitrate. Two molecules of the compounds react with one molecule of silver nitrate to give a white precipitate.     

N,N-bis-(2-benzimidazolylmethyl)L-methionine: An efficient Ag(I) extractant

A new ligand N,N-bis-(2-benzimidazolylmethyl)L-methionine has been synthesized and well characterized by different analytical techniques. The ligand has a very strong affinity for silver(I) and is used for the selective extraction of silver ions from aqueous solution into 1-butanol. The effect of concentration of Ag(I), pH, diverse ions, and temperature on the extraction is reported. The developed method has success-fully been applied to the determination of silver in different samples. Radiotracer technique, using ^110mAg(I) as a tracer, has been used for monitoring the concentration of silver ion.     

Coupled transport of Ag(I) ions through triethanolamine–cyclohexanone-based supported liquid membranes

Facilitated transport of silver(I) ions in acidic medium, across a supported liquid membrane (SLM) by using triethanolamine (TEA) as carrier, dissolved in cyclohexanone, has been investigated. The parameters studied are HNO₃ concentration variation in the feed, pH of the feed solution, carrier concentration in the membrane phase, silver(I) ions concentration in the feed phase and KCN concentration in the stripping phase. Increase in H⁺ concentration by increasing HNO₃ concentration from 0.5 to 1 M results into an increase in silver ions flux but a decrease in flux has been found beyond 1 M HNO₃ concentration in the feed, providing a maximum flux of 3.21 × 10⁻⁷ mol/m² s at 1 M HNO₃. Increase in TEA concentration inside the membrane enhances flux with its maximum value at 2.25 M TEA. Further increase in the concentration of TEA leads to a decreased rate of transport due to the increase in viscosity of membrane liquid. The optimum conditions for Ag(I) ions transport are 1 M HNO₃ (feed), 2.25 M TEA (membrane) and 1.5 M KCN in the stripping phase. It has been observed that Ag(I) flux across the membrane tends to increase with increase in Ag(I) ions concentration in the feed phase. Applying the studied conditions to silver plating waste solutions, Ag ions have been removed up to 99% in a time interval of 5 h.     

5,10,15-Tris(pentafluorophenyl)corrole as highly selective neutral carrier for a silver ion-sensitive electrode

A new highly selective silver(I) electrode was prepared with a PVC membrane using 5,10,15-tris(pentafluorophenyl)corrole as an electroactive material, 2-nitrophenyl octyl ether (o-NPOE) as a plasticizer and sodium tetraphenylborate (NaTPB) as an additive in the percentage ratio of 3:3:62:32 (corrole:NaTPB:o-NPOE:PVC, w:w). The electrode exhibited linear response with a near Nernstian slope of 54.8 mV/decade within the concentration range of 5.1 × 10⁻⁶ to 1.0 × 10⁻¹ M silver ions, with a working pH range from 4.0 to 8.0, and a fast response time of <30 s. Selectivity coefficients for Ag(I) relative to a number of interfering ions were investigated. The electrode is highly selective for Ag(I) ions over a large number of mono-, bi-, and tri-valent cations. Common interferents like Hg²⁺ and Cd²⁺ show very low interfering effect on the silver assay, which is valuable property of the proposed electrode. Several electroactive materials and solvent mediators have been compared and the experimental conditions were optimized. The sensor was applied to the determination of silver in real ore samples with satisfied results.     

Modification of catheter materials by coating with polymer layers containing silver

The surface of polyurethane based catheter material or of silicon wafers as model surfaces were modified by spin coating of solutions of poly(ethylene oxide) or poly(vinyl alcohol) in water. For the incorporation of silver ions, silver nitrate was added to some of the solutions or the as-cast surfaces were dipped into AgNO₃ solution. Furthermore, samples coated with a thin layer of metallic silver were prepared by deposition of silver vapor in vacuum. The as-prepared surfaces were studied by atomic force microscopy and X-ray photoelectron spectroscopy. During the spin coating of the solutions containing AgNO₃, clusters of the silver component were formed. They were well dispersed in a poly(vinyl alcohol) matrix but act as nucleation agents in poly(ethylene oxide) where then large spherulites are formed. The surface compositions of coated samples and the depth profiling were carried out by angle dependent X-ray photoelectron spectroscopy.     

Characterization of a Silver Modified PVCAc Electrode and Its Application as a Ag(I)‐Selective Potentiometric Sensor

An all solid‐state Ag(I) ion‐selective electrode has been prepared by simply immersing a glassy carbon rod coated with PVCAc, which contained plasticizer and additive but no ionophore, into the AgNO₃ solution. The response of the electrode was linear with a Nernstian slope of 60.25 mV/decade within the concentration range from 1×10^?1 to 1×10^?5 M and with a detection limit of 4.25×10^?6 M. The stability as an effect of various cations was defined. The electrode is suitable for use in high acidic solutions (pH<1 to 7) and has successfully been applied for the determination of silver(I) concentrations in different samples.     

Separation of iodine produced from fission with a porous metal silver column in99Mo production

In Argentina, at the Ezeiza Atomic Center,¹³¹I is produced by wet distillation of natural tellurium dioxide irradiated with thermal neutrons in a pool-type reactor. In order to recover the¹³¹I present in the production process of fission⁹⁹Mo obtained by irradiation of UAL_x/Al targets (with 90% enriched uranium) a separation method was developed. Iodine isotopes can be separated from a sodium hydroxide solution containing fission products using a column filled with alternate beds of glass microspheres and porous metal silver. Tests with tracers were performed in radiochemical laboratory. Following this results, a series of tests with higher activities (3 TBq of⁹⁹Mo and 0.7 TBq of¹³¹I) were carried out in hot cells. Molybdenum passes through the silver column, while¹³¹I retention was 92–97% in tracer test and 90% in optimised hot cell tests. This result depends on several facts that are discussed. An initial separation of iodine isotopes diminishes radiation damage on ion-exchange resin used in the subsequent molybdenum purification, improving its retention and elution yield.     

Crafting La0.2Sr0.8MnO3-δ membrane with dense surface from porous YSZ tube

This work reports a new design of asymmetric tubular oxygen-permeable ceramic membrane (OPCM) consisting of a porous Y₂O₃ stabilized ZrO₂ (YSZ) tube (with ∼1 μm of pore diameters and 31% porosity) as the support and a gas-tight mixed conductive membrane. The membrane has an interlocking structure composed of a host matrix, Ag(Pd) alloy (9:1 by wt) doped perovskite-type (LSM80, 90wt%), and the embedded constituent, pristine LSM80. The Ag(Pd) alloy component promotes not only electronic conductivity and mechanical strength but also reduction of both porosity and pore sizes in the layer (∼10-μm-thick) where it dopes. The porous structure in this layer could then be closed through a solution coating procedure by which ingress of an aqueous solution containing stoichiometric nitrate salts of La³⁺, Mn³⁺, and Sr²⁺ to the pore channels takes place first and the mixture of nitrate salts left after drying is subjected to pyrolysis to generate tri-metal oxides in situ. This is followed by calcinations at l,300 °C to consolidate the embedded trioxide and to cohere them with the Ag(Pd)-LSM80 host matrix. The structure formed is dubbed LSM80(S)-Ag(Pd)-LSM80, which was confirmed gas-tight by electron micrograph and N₂ permeation test. Finally, we assess the chemical compatibility between LSM80 and YSZ at the sintering temperature by X-ray diffraction and electrochemical impedance analysis. The oxygen permeation of the fabricated LSM80(S)-Ag(Pd)-LSM80-YSZ membrane is within the temperature range of 600 to 900 °C. The tests reveal good compatibility between the LSM80 and YSZ and a reasonably high oxygen permeation flux in association with this OPCM assembly.     

Radiometric analysis of silver in galena

A radiometric procedure for quantitative analysis of traces of silver in galena has been demonstrated. The mineral sample was dissolved in HNO₃ (31) and silver present in the solution was precipitated as insoluble AgI by adding an excess amount of¹³¹I-labeled KI solution and was coprecipitated with zirconium hydrogen phosphate, Zr(HPO₄)₂, in 0.5N H₂SO₄ medium. The method of radiometric analysis of silver which was estimated from the knowledge of the loss of¹³¹I activity in solution, was found to be effective in determination of the element even below ppb level. Applicability of the radiometric procedure in routine analysis or preconcentration of traces of silver in galena has been stressed.     

Newly-designed proteinic membrane for low ultrafiltration

This article deals with a new proteinic formed-in place membrane built on top of an α-alumina macroporous ceramic support (0.2 μm SCT membrane). The initial proteinic deposit is obtained through tangential filtration of gelatin solutions. Then subsequent chemical and/or physical treatments are applied. In a first part of the study it is shown that by tanning (with formaldehyde) plus thermal drying of the gelatin layer low ultrafiltration performance may be reached. In the second part, the effect on membrane performance of the protein deposition conditions (concentration and pH of protein solution, velocity, pressure) is analyzed. From experimental results, it appears clearly that the best membrane so obtained has a cut-off point around 2 kDa and a flux as high as 101 h⁻¹ m⁻² under 200 kPa.     

Separation of silver from waste waters by ion-exchange resins and concentration by microbial cells

Summary Waste waters of film processing plants are rich with silver. Part of the silver is regenerated electrochemically, but the rest (0.5 g) remains in waste waters and is sent to sewers. This is a bad politic from both the environmental (toxic waste waters) and the economical point of view (a waste of silver). In this work, the silver was isolated by ion-exchange resins and then concentrated by microorganisms. For exchange of silver, Ionenaustauscher I, II and IV were used. The batch method was used to obtain a static equilibrium. Silver elution from exchangers is based on silver transformation to a stable cation or anion complex. By varying the ligands, pH and eluent concentrations, optimum elution is found at 1 mol/l Na₂S₂O₃, 1 mol/l NH₃, 2 mol/l HNO₃ and 1 mol/l (NH₂)₂CO. The concentration of silver in the eluent is about 50 mg/l. The silver ion uptake from solutions after ion exchange by mixed bacterial culture isolated from photographic waste water drain and pure bacterial cultures Escherichia coli 3009 and Bacillus subtilis 3053. was studied. Experiments were carried out in submerse culture at pH 7 with different Ag⁺ concentrations (4, 8 and 40 mg/l) on a rotary shaker (100 rpm) at 37°C. At the lower Ag⁺ concentrations a good growth and simultaneous removal of Ag⁺ from the solutions was achieved. At Ag⁺ concentration of 40 mg/l growth and removal of Ag⁺ by mixed and pure culture differed significantly. Thus mixed bacterial culture grew well and at the same time removed efficiently Ag⁺ (approximately 90%) from medium. Pure bacterial cultures on the contrary were unable to grow at 40 mg/l Ag⁺, though their biomass showed to be an effective biosorbent for Ag⁺ (approximately 80% of Ag⁺ removal).     

阴离子表面活性剂作为添加剂种子生长法制备尺寸可调的单分散金纳米棒

以不同阴离子表面活性剂作为添加剂种子生长法制备金纳米棒, 并考察阴离子表面活性剂种类对金纳米棒形貌及光学性质的影响。在十二烷基苯基磺酸钠(SDBS)存在下, 金纳米棒的产率明显高于使用十二烷基磺酸钠的反应体系。对添加SDBS的种子生长法制备金纳米棒的反应条件进行优化, 得到十六烷基三甲基溴化铵、SDBS、抗坏血酸和硝酸银的最佳浓度分别为0.04 mol·L^-1、2.4 mmol·L^-1、1.2 mmol·L^-1和0.08 mmol·L^-1。在此条件下, 金纳米棒的生长在30 min内完成, 所制备的金纳米棒表面等离子共振吸收峰位于823 nm, 其横纵比为(5±0.03)。当改变生长液中硝酸银浓度时, 金纳米棒的尺寸也随之发生改变。此外, 我们还探讨了SDBS的作用机理。相对于经典种子生长法, 新方法制备纳米金棒在尺寸可调性、单分散性和生物毒性方面明显改善, 可广泛应用于各种光学及生物分析。     

Highly-sensitive ion selective electrode based on molecularly imprinted polymer particles for determination of tetracycline in aqueous samples

In this work, a highly-sensitive polymeric membrane ion selective electrode for determination of tetracycline was constructed by using molecularly imprinted polymer (MIP) particles as quasi-ionophore. The water-compatible MIP particles targeting tetracycline were synthesized with tetracycline as a template molecule, methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, 2,2′-azobisisobutyronitrile as an initiator and lanthanum ion as a mediator. Benefited from the distinctive performance of the quasi-ionophore and the optimized composition of the membrane and the inner filling solution, the lower detection limit of the electrode was decreased to about 1 × 10⁻⁸ mol/l. It exhibited a good electrode slope 59.8 mV/decade near the theoretical Nernstian one, with a wide linear working range from 2.0 × 10⁻⁸ to 1.0 × 10⁻³ mol/l. Due to the specific recognition of tetracycline by the MIP particles, the selectivity coefficients for routine interferences were less than 10⁻⁴. The fabricated electrode should be used in pH 2–4, response time of which was less than 200 s when the concentration of tetracycline was higher than 1.0 × 10⁻⁶ mol/l and no more than 30 min at the concentration of 1.0 × 10⁻⁸ mol/l. Finally, the proposed highly-sensitive ion selective electrode has been successfully applied to the determination of tetracycline in aqueous samples.     

Development of a nitrate ion-selective electrode based on an Urushi matrix membrane and its application to the direct measurement of nitrate-nitrogen in upland soils

A solid-state nitrate ion-selective electrode based on an Urushi matrix membrane was developed. Urushi, a natural oriental lacquer, has excellent mechanical strength and binding affinity for metal electrodes. Using the same technique for a dip-coating ion-selective electrode, an electrode was prepared by coating and hardening a sensing membrane on the metal base. The effects of the metal electrode on the electrode potential stability, the liquid-membrane components and the oven temperature for hardening of membrane were studied. The sensing membrane, consisting of 27.5 wt.% of o-nitrophenyl octyl ether. 27.5 wt.% of tri-n-octylmethylammonium nitrate and 45 wt.% of raw Urushi latex, was coated with a thickness of 0.5 mm on a silver disc which was plated with Ag/AgCl, then plated with copper and hardened in the oven at 80 degrees C for 50 h. A semi-logarithmic calibration curve of potential versus nitrate ion concentration was obtained over the range 6-60 000 mg l(-1) NO(3)(poststaggered-). The slope of the linear part of the curve was -56 mV per decade change in NO(3)(poststaggered-) concentration. Compared with a PVC matrix nitrate ion-selective electrode, the Urushi matrix nitrate ion-selective electrode was superior in terms of hardness and mechanical strength of the membrane, short response time and long life. The combination of an Urushi matrix nitrate ion-selective electrode with a porous PTFE junction reference electrode, air-tight structured KCl solution chamber and a temperature sensor was applied to field measurements of nitrate-nitrogen concentrations in upland soils. The values obtained for upland soils containing 30-50% of water were good agreement with those for soil solution.     

Anodic stripping voltammetry of silver(I) using a carbon paste electrode modified with multi-walled carbon nanotubes

We describe a silver(I)-selective carbon paste electrode modified with multi-walled carbon nanotubes and a silver-chelating Schiff base, and its electrochemical response to Ag(I). Effects of reduction potential and time, accumulation time, pH of the solution and the stripping medium were studied by differential pulse anodic stripping voltammetry and optimized. The findings resulted in a method for the determination of silver over a linear response range (from 0.5 to 235 ng?mL^?1) and with a detection limit as low as 0.08 ng?mL^?1. The sensor displays good repeatability (with the RSD of ±?2.75 % for 7 replicates) and was applied to the determination of Ag(I) in water samples and X-ray photographic films.

Preparation of a carbon ceramic electrode modified by 4-(2-pyridylazo)-resorcinol for determination of trace amounts of silver

A 4-(2-pyridylazo)-resorcinol (PAR)-modified carbon ceramic electrode (CCE) prepared by the sol-gel technique has been reported for the first time in this paper. By immersing the CCE in aqueous solution of PAR (0.001 mol L⁻¹), after a short period of time, a thin film of PAR was rapidly formed on the surface of the electrode due to its strong adsorption properties. A differential pulse anodic stripping voltammetric (DPASV) method was developed for determination of Ag(I) at the modified carbon ceramic electrode. The analysis procedure consisted of an open circuit accumulation step in a sample solution which was continuously stirred for 12 min. This was followed by replacing the medium with a clean solution where the accumulated Ag(I) was reduced for 15 s in −0.6 V. Then, the potential was scanned from −0.2 to +0.2 V to obtain the voltammetric peak. The detection limit of silver(I) was 0.123 μg L⁻¹, and for seven successive determinations of 10, 100 and 200 μg L⁻¹ Ag(I), the relative standard deviations were 2.1, 1.4 and 1.03%, respectively. The calibration curve was linear for 0.5-300 μg L⁻¹ silver(I). The procedure was applied to determine silver(I) in X-ray photographic films and super-alloy samples.