Investigation of the silver iodide—p-ethoxychrysoidine adsorbate by infrared spectroscopy

Infrared measurements for p-ethoxychrysoidine and the silver iodide—p-ethoxychrysoidine adsorbate indicate that the dye is bound to silver iodide through amino groups. The interaction is discussed on the basis of surface imperfections of silver iodide and the polar nature of p-ethoxychrysoidine. Of the two possible crystal structures of silver iodide, only the γ-modification is present in the adsorbate.     

Highly sensitive determination of iodide by ion chromatography with amperometric detection at a silver-based carbon paste electrode

A silver-based solid carbon paste electrode was developed for use as a detector in ion chromatography (IC) for the sensitive determination of iodide in real samples. Micro- and nano-particles of silver were investigated for the fabrication of different electrodes. The iodide assay was based on IC with amperometric detection (IC-AD) at a silver composite electrode polarized at +0.080 V versus Ag/AgCl. Free iodide and organoiodide compounds were studied. The detection process was characterized by studying the redox behavior of iodide ions at both silver and silver composite electrodes by cyclic voltammetry (CV). The presence of iodide ions in solution was found to considerably facilitate metallic silver oxidation, with response currents directly related to iodide concentration. The calibration curve at the selected silver carbon paste electrode was linear in the concentration range comprised between 0.635 microg/L and 63.5 microg/L iodide. The relative standard deviation (R.S.D.) for successive injections was below 3% for all iodide standard solutions investigated. The limit of detection (LOD) was 0.47 microg/L (3.7 nmol/L) for an injection volume of 20 microL, i.e. 74 fmol injected. The IC-AD method was successfully applied to the determination of iodide in complex real samples such as table salts, sea products and iodide bound drug compounds. The analytical accuracy was verified by the assay of iodide in milk powder from an iodide certified reference material (CRM) Community Bureau of Reference (BCR) 150.     

Determination of silver in rocks by a stoichiometric radioreagent radioisotope dilution technique

A rapid procedure for the routine determination of nanogram amounts of silver in rocks is described. After dissolution of the sample with a hydrofluoric-nitric-perchloric acid mixture in the presence of ¹¹⁰Ag tracer, the silver is separated by extraction as the dithizonate into xylene and back-extracted into dilute hydrochloric acid. After evaporation and removal of the hydrochloric acid, the silver is taken up in an acetic acid-sodium tartrate buffer solution and reacted with a constant amount of radioactively labelled iodide. The silver iodide formed is isolated by extraction into amyl alcohol and silver is determined by the ratio of the counting rate of the iodide to that of the silver in the silver iodide complex. Results of the analyses of several U.S. Geological Survey standard rocks are given.     

Surface studies on precipitate-based cyanide electrodes

Silver iodide-based electrodes allow indirect measurements of cyanide. Potentiometric investigations and theoretical studies have suggested that a corrosion process is responsible for this cyanide response. Surface analytical methods of providing information at different depths are used to investigate mixed membranes of silver iodide/silver sulphide and pure silver iodide membranes. The results prove that in the surface corrosion process the iodide content of the mixed membrane surface decreases. Further, the membrane loses silver sulphide particles from its surface. Finally, a layer enriched with readsorbed iodide is formed on the outermost surface of the membrane. The composition of the surface layer depends on pH and buffer capacity because of the different fluxes of ions observed in the surface layer.     

Determination of nanogram amounts of sulphide by release of radioactive iodide

Two variants of a technique for determination of ng-amounts of sulphide ions in liquid samples are presented. They are based on the replacement of radioactively labelled iodide from silver iodide by sulphide. In the first variant, suitable for small sample volumes, the labelled silver iodide is fixed on a filter paper disc which is then shaken with the solution to be analysed until equilibrium is attained. In the second variant, suitable for sample volumes up to 300 ml, the sample solution is passed through a filter paper disc carrying labelled silver iodide or through a labelled silver iodide precipitate. The amount of sulphide is determined from the activity of the released radioiodide by comparison with standards which have been processed in the same way. The method is applicable to sulphide amounts greater than 5 ng and concentrations greater than 0.2 ppM. The interference by many common accompanying anions and cations has been investigated.     

Luminescence of ordered silver iodide nanoclusters inside zeolite host

Ordered silver iodide nanoclusters inside zeolite Y host were prepared by using a thermal diffusion method. The Y-AgI samples were characterized with powder X-ray diffraction, differential thermal analysis, X-ray photoelectron spectroscopy, adsorption technique and chemical analysis. The results show that silver iodide nanoclusters were situated in the ordered cages of the zeolite Y host. The results on the luminescence of the nanocomposites Y-AgI suggest that when the sizes of silver iodide nanoclusters are were very small, non-radiation surface recombination exceeds radiation process and the luminescence efficiency increases as the size of the silver iodide nanoclusters increaseds As the sizes of AgI nanoclusters increased, non-radiative surface recombination effect become equal to the radiation effect of the excitons. As the size of the nanoclusters of AgI in zeolite host further increases, the surface recombination of the nanoclusters becomes a major process.     

The coulometric production of iodide ion for titrations of mercury(I.II)

The dynamic behaviour of the silver/silver iodide electrode was studied. Iodide ions can be produced by cathodic polarization of the silver/silver iodide electrode in acidic and neutral media. This technique can be used for coulometric titrations of mercury(I) or mercury(II) both alone and in mixture. At the microequivalent level of mercury the error is less than 2%.     

Letter: Silver mediated ester bond formation in the gas phase: substrate structure is important

The silver acetate cation CH(3)CO(2)Ag(2)(+) reacted with allyl iodide via C-O bond coupling to produce Ag(2)I(+) and allyl acetate, but only underwent adduct formation with methyl iodide, highlighting the importance of substrate on reactivity. DFT calculations predicted the reaction with allyl iodide to be exothermic by 0.48 eV, and suggested that intermediates in the reaction benefit from multiple interactions between the allyl and iodide moieties of allyl iodide and the two silver atoms in CH(3)CO(2)Ag(2)(+).     

Comparative study of different cyanide-selective air-gap electrodes

The characteristics of four solid-state cyanide-selective air-gap electrodes are described. When a minute volume of dicyanoargentate(I) solution was used as electrolyte, the double-Nernstian response to cyanide concentration was obtained only with the sensors based on silver or silver sulphide. Sensors based on silver iodide or a silver sulphide/iodide mixture displayed the normal Nernstian character shown by cyanide-selective electrodes dipped in solution. A theoretical explanation of the results involves the relevant equilibrium equations and the mass balance.     

片状卤化银晶体的制备、结构与性能的研究——Ⅱ.pAg对片状颗粒的尺寸、纵横比、碘离子分布及离子电导率的影响

本文研究了双注法制备片状卤化银微晶时,pAg值对所形成的卤化银片状颗粒的尺寸、纵横此、碘离子分布以及离子电导率的影响。随着pAg值的升高,片状颗粒的尺寸和纵横比都相应地增大和升高,且越来越多的碘离子从颗粒中心向外层迁移,直至到达表层,这说明存在晶体的重结晶过程。表面层的溴碘原子比是用X射线光电子能谱仪(XPS)测定的,并测量了不同pAg值下制备的不同尺寸的片状卤化银乳剂的介电损耗频谱。其结果表明,片状颗粒的尺寸影响其离子电导率,表层碘含量的影响不明显。     

Silver/silver iodide electrodes of the second kind as sensors for cyanide

Silver/silver iodide electrodes of the second kind prepared by electrolytic coating of silver electrodes are advantageous as sensors for cyanide. They are inexpensive and exhibit characteristics similar to those of commercially available ion-selective electrodes. They can be regenerated easily when necessary; this eliminates the lifetime problems generally inherent in iodide electrodes used as cyanide sensors. The preparation, properties and selectivity characteristics of the second-kind iodide electrode are described.     

影响一步摄影正象色调与银颗粒大小的几个因素

用透射电子显微镜观察一步摄影正片(明胶介质)的银颗粒,对影响银颗粒大小的因素进行了研究。卤化银负片乳剂中的碘含量,明显地影响卤化银颗粒大小和转印后银颗粒的大小,随着卤化银乳剂中的碘含量减少,卤化银颗粒和银质点簇(即银颗粒)变大,组成银质点簇的银质点数目增多,正象色调由棕向黑转移。不同物理显影核亦显著影响正片银颗粒大小与其色调。     

A colorimetric method for highly sensitive and accurate detection of iodide by finding the critical color in a color change process using silver triangular nanoplates

In this contribution, we demonstrated a novel colorimetric method for highly sensitive and accurate detection of iodide using citrate-stabilized silver triangular nanoplates (silver TNPs). Very lower concentration of iodide can induce an appreciable color change of silver TNPs solution from blue to yellow by fusing of silver TNPs to nanoparticles, as confirmed by UV–vis absorption spectroscopy and transmission electron microscopy (TEM). The principle of this colorimetric assay is not an ordinary colorimetry, but a new colorimetric strategy by finding the critical color in a color change process. With this strategy, 0.1 μM of iodide can be recognized within 30 min by naked-eyes observation, and lower concentration of iodide down to 8.8 nM can be detected using a spectrophotometer. Furthermore, this high sensitive colorimetric assay has good accuracy, stability and reproducibility comparing with other ordinary colorimetry. We believe this new colorimetric method will open up a fresh insight of simple, rapid and reliable detection of iodide and can find its future application in the biochemical analysis or clinical diagnosis.     

片状卤化银晶体的制备、结构与性能的研究——碘离子在不同结构的片状卤化银晶体中的分布及其离子电导行为

本文制备了三种结构不同的片状卤化银晶体。用电子显微镜和X射线能谱仪相结合的方法,对单个晶体进行了微区微观结构分析,测定了碘离子在三种不同结构的片状颗粒中的分布,并测量了不同结构片状颗粒的和同一结构不同碘含量的片状颗粒的介电损耗。     

Variability of selectivity coefficients of solid-state ion-selective electrodes

The generalized model for the selectivity mechanism of solid-state ion-selective electrodes has been experimentally verified. The experimental parameters investigated were the concentration of interfering ion, temperature and stirring. Among the systems studied were electrodes sensitive to chloride (bromide, iodide), bromide (chloride, iodide), iodide (chloride, bromide), silver (copper, lead), copper (silver, lead) and lead (silver, copper), the species given in brackets being considered as the interferents. The model has been confirmed except for cases where the concentration of ions formed at the electrode surface by metathesis is too small to be the factor that dictates the electrode potential.     

Iodide adsorption on the surface of chemically pretreated clinoptilolite

The possibility to use the monoionic Ag⁺-form (eventually Hg⁺- and Hg²⁺- forms) of clinoptilolite of domestic origin for radioactive iodide elimination from waters has been studied. The capacity of the monoforms of clinoptilolite towards iodide exceeds many times that of the capacity of clinoptilolite in natural form. Due to the low solubility product of AgI, Hg₂I₂ and HgI₂ iodides generate precipitates on the zeolite surface. Rtg analyses of the silver form of clinoptilolite after sorption of iodide demonstrate the formation of new crystals on the zeolite surface. The influence of interfering anions on the adsorption capacity of silver clinoptilolite towards iodide was investigated, too. Kinetic curves of iodide desorption from the surface of silver and mercury clinoptilolite were compared. Simultaneously, adsorption isotherms for the systems aqueous iodide solution/Ag^–, Hg-clinoptilolite were determined.     

感光颗粒内碘离子的分布与乳化方法的关系

本文利用X射线光电子能谱法和X射线衍射分析,研究了双注法高感乳剂乳化过程中,碘离子的引入时刻对于乳剂颗粒内碘离子分布情况的影响.结果表明,一般说来,碘离子引入得愈早,则其出现在颗粒表面的可能性愈小;引入得愈晚,其位置愈靠近颗粒的表面.但是,早期引入碘离子同时,还有另一种效应,即倾向于使碘离子在体系中均匀分布,从而使其出现在颗粒表面的概率增大.有若干事实说明,这种“均化”效果可能是早期形成的碘化银或碘溴化银晶体在乳化过程中进行重结晶而引起的.在所有情况下,颗粒表面上均发现一层极薄的富碘层,其原因之一可能是碘离子在颗粒表面的富集可减少碘溴化银晶格的畸变.     

Measurement of hypoiodous acid concentration by a novel type iodide selective electrode and a new method to prepare HOI. Monitoring HOI levels in the Briggs-Rauscher oscillatory reaction

A new type of iodide selective electrode prepared by dipping a silver wire into molten silver iodide is reported. The electrode was calibrated for silver and iodide ions and the measured electromotive force for various Ag(+) and I(-) concentrations was close to the theoretical within a few millivolts. Besides Ag(+) and I(-) ions, however, the electrode also responds to hypoiodous acid. Thus, the electrode was calibrated for HOI as well, and for that purpose a new method of hypoiodous acid preparation was developed. To explain the close to Nernstian electrode response for HOI and also the effect of hydrogen ion and iodine concentration on that response, the corrosion potential theory suggested earlier by Noszticzius et al. was modified and developed further. Following oscillations in the Briggs-Rauscher reaction with the new electrode the potential crosses the "solubility limit potential" (SLP) of silver iodide. Potentials below SLP are controlled by the concentration of I(-), but potentials above SLP are corrosion potentials determined by the concentration of HOI. Finally, the measured HOI oscillations are compared with calculated ones simulated by a model by Furrow et al.     

用俄歇能谱和X射线能谱研究板状碘溴化银微晶中的碘离子的空间分布

本文制备了一系列不同碘含量的板状碘溴化银微晶(微晶大小约为3微米)。运用扫描透射电镜和X射线能谱仪(EDS)对单个微晶进行了分析和研究,半定量地测定了碘离子在板状微晶中的面分布;运用扫描俄歇微区棵针(SAM)和二次电子像、离子溅射剥层技术对微晶进行了表面及其纵深的碘离子的点分析,根据EDS和SAM的结果,可以得到板状碘溴化银微晶中的碘离子的空间分布。实验结果表明在板状缺溴化银微晶中,在其中心部位的碘含量最高;越靠近横向边缘的位置,碘含量越低。且在制备碘溴化银微晶时,如果pAg值较高,将会使在制备早期加入的碘离子通过不断的重结晶向微晶表面扩散,得到的微晶不是夹心结构的碘溴化银微晶。     

Polyethylenimine complexes with silver ions in aqueous solutions as precursors for synthesis of monodisperse silver iodide particles

The conditions of formation and composition of polyethylenimine complexes with silver ions in aqueous solutions are found. The complex is formed according to the model of a uniform distribution of ions throughout the macromolecule, and the composition of the complex may vary depending on pH of the medium. The size parameters are determined and the volume fractions of polyethylenimine macromolecular coils in solution are calculated. The synthesis of silver iodide particles is carried out under conditions where the silver ions are bound in the complex with polyethylenimine macromolecules and are distributed homogeneously over the volume of solution. The use of the polyethyleneimine complex with silver ions as a precursor of silver iodide allows the preparation of particles 1.2 nm in diameter with a narrow size distribution.