Ammonium dithionate- a new material for highly sensitive EPR dosimetry

Polycrystalline ammonium dithionate has been examined for its radiation response in the low dose range (<5Gy) using EPR technique. The SO(3)(-) radical ion was detected as a single EPR line with a peak-to-peak derivative width of ca. 0.44mT in irradiated samples and its intensity was found to vary linearly with dose. At equal and moderate settings of microwave power and modulation amplitude ammonium dithionate was at least seven times more sensitive than l-alanine which is the most common EPR dosimeter standard. Pulse experiments were performed on the powder samples to obtain the longitudinal relaxation time. These and microwave saturation experiments served to indicate the optimal microwave power to be applied during measurements as an EPR dosimeter for best sensitivity of this material. It is thus claimed that ammonium dithionate has excellent potential to become an EPR dosimeter with a low limit of the measurable dose for cases where tissue equivalence is not required or can be corrected for.     

Transport of sulfate anions through inorganic membranes modified by ion-exchange material

Resistance properties of systems consisting of H₂SO₄ solutions and composite ceramic membranes modified by amphoteric ion-exchange material—hydrated zirconium dioxide (HZD)—are investigated by impedance spectroscopy. Transport numbers of sulfate ions through these membranes are calculated, and their values reach 0.86–0.92 as a function of the amount of HZD inserted into the membrane. Values of the transport numbers, estimated from impedance measurements, are found to be in good agreement with data obtained in investigations of sulfate transport at constant current under conditions in which the membrane charge is determined only by anions.     

Silver nanoplates and nanowires by a simple chemical reduction method

The critical micelle concentration (cmc) of an amphiphilic drug amitriptyline hydrochloride (AMT) was determined in the presence of varying amounts of inorganic salts (NaF, NaCl, NaBr, LiCl, KCl), urea and thiourea over the temperature range 293–308 K by conductometric and dye solubilization (ambient) techniques. The cmc values showed an inverted U-shaped behavior with temperature. In the presence of salts the cmc decreased which is explained on the basis of the nature and ion size. Urea and thiourea, at low concentrations (0.2 mM urea and 0.1 mM thiourea), decreased the cmc, whereas, at high concentrations, increase was observed with both the additives. Relevant thermodynamic parameters were also evaluated and discussed.     

Separation of inorganic anions using a series of sulfobetaine exchangers

A set of five new sulfobetaine exchangers with inner quaternary amines and outer sulfonic acids have been prepared. A series of zwitterionic precursors was attached to highly porous divinylbenzene polymer using a grafting reaction, which allows a flexible adjustment of the degree of functionalisation. The resulting materials have identical spacers to the polymeric backbone and differ only in chain length between the charged functional groups. Capacities of the stationary phases were analysed by two different methods based on elemental analysis and the results obtained were found to correlate. The application of combustion elemental analysis proved an identical molar content of sulfur and nitrogen. The distance between the charged functional groups is varied from one to five methylene groups for a better understanding of the retention behaviour of inorganic anions on zwitterionic stationary phases. Inorganic anions were separated using sodium acetate eluents with varying ionic strength and pH and the behaviour of all columns has been compared to each other and to ZIC-HILIC and ZIC-pHILIC columns from Merck SeQuant. The exchangers with two and five methylene groups between the charges showed the highest retention factors. Polarity and accessibility of the anion exchange sites are dependent on the distance between the charged groups and the flexibility of the chains. These properties have a strong influence on anion separations. The exchanger with two methylene groups between the charged functional groups showed the biggest difference as compared to the commercially available ZIC-HILIC and ZIC-pHILIC exchangers.     

Electrophoretically deposited L-cysteine functionalized MoS2@MWCNT nanocomposite platform: a smart approach toward highly sensitive and label-free detection of gentamicin

The exploitation of antibiotics has caused many side effects on the agriculture, environment, and human health. The existing methods have numerous shortcomings in determining gentamicin (GEN), a broad-spectrum antibiotic that causes nephrotoxicity and ototoxicity when found in excess. Here, an immunosensing platform to detect GEN using multiwalled carbon nanotubes (MWCNTs) and molybdenum disulfide (MoS₂) nanocomposite, deposited electrophoretically on indium tin oxide (ITO) glass has been developed. A novel 2-D graphene analog MoS₂@ MWCNTs nanocomposite was made via a facile and low-cost hydrothermal technique using l-cysteine to achieve remarkable electrochemical properties. Subsequently, a highly sensitive electrochemical immunosensor was fabricated by assembling monoclonal antibodies against gentamicin (anti-GEN) on a MoS₂@MWCNTs modified ITO electrode. The hetero-nanostructure formed on the immunosensor surface appeared relatively good conductor for accelerating the electron transfer. GEN was determined on anti-GEN modified electrodes by utilizing the differential pulse voltammetry technique by measuring the difference in current owing to the transfer of electrons directly between the redox species and immunoelectrodes. Under optimal experimental conditions, the fabricated immunosensor had a wide linear detection range of 1 × 10^?6–40 μg/mL, a high sensitivity of 13.55 μA (log μg/mL)^?1 and a low limit of detection and limit of quantification of 0.039 μg/mL and 0.130 μg/mL, respectively. The developed immunosensor also exhibits high reproducibility, repeatability, and good selectivity against various interferences. This electrochemical immunosensor having MoS₂ modified MWCNTs displays the excellent potential for the point-of-care device for GEN testing.     

Subphthalocyanines as fluoro-chromogenic probes for anions and their application to the highly selective and sensitive cyanide detection

The use of a subphthalocyanine derivative as a selective chromo-fluorogenic reporter for the anion cyanide in mixed aqueous solutions is reported.     

Determination of inorganic anions in environmental waters with a hydroxide-selective column

US Environmental Protection Agency Method 300.0 specifies the use of an IonPac AS4A anion-exchange column with a carbonate-hydrogencarbonate eluent and suppressed conductivity detection for the determination of inorganic anions in environmental waters by ion chromatography. Hydroxide eluents have not typically been used for the routine analysis of common inorganic anions due to the lack of an appropriate hydroxide selective column and the difficulty in preparing contaminant free hydroxide eluents. The use of ion chromatography with a hydroxide-selective IonPac AS17 column, automated eluent generation and potassium hydroxide gradient represents a new approach to the routine determination of inorganic anions in environmental waters. This new approach, which is a modification of Method 300.0, allows equivalent method performance with improved linearity, precision, and method detection limits. The AS17 column provides superior retention of fluoride from the column void volume and improved resolution from small organic acids, such as formate and acetate, compared to the AS4A column. Quantitative recoveries were obtained for all the common inorganic anions spiked into typical environmental waters using this new approach, and the Performance Based Measurement System Tier 1 method validation quality control acceptance criteria are well within the acceptable ranges defined by Method 300.0. In addition, the EG40 eluent generator eliminates the need to manually prepare eluents, increasing the level of automation and ease-of-use of the ion chromatography system.     

HPLC-HG-ICP-MS: a sensitive and selective method for inorganic arsenic in seafood

The addition of an online post-column hydride generation (HG) step to the commonly used high-performance liquid chromatography inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) setup for arsenic speciation proved to significantly improve the detection limits for the determination of inorganic arsenic (iAs) as arsenate in seafood samples, where the limit of detection and limit of quantification were found to be 0.0004 and 0.0014?mg?kg(-1), respectively with HG. HG as an additional step further added to the selectivity of the determination of the iAs species and increased the detection and quantification of low levels of iAs (<0.002?mg?kg(-1)) in samples with complicated matrices.     

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.     

A sensitive fluorescent chemosensor for anions based on a styryl-boradiazaindacene framework

Long wavelength emitting, extended conjugation boradiazaindacenes are novel dyes with considerable ICT character. By appending a dipicolylaminylethylamine group, the parent compound was transformed into a fluorescent dye with a strong chelating ability for Zn(II) ions. The zinc complex which has bright orange fluorescence, reversibly signals anions with very large changes in both the absorption and the emission spectra. The remarkable change in the emission intensity is explained in relation to the electron donating capacity of the substituent on the styryl functionality.     

基于电催化还原化学发光法检测异烟肼的高灵敏方法

实验发现,异烟肼在汞膜修饰石墨电极表面被还原后即被溶液中的溶解氧所氧化,重新回到初始状态;而溶解氧被还原生成活性氧自由基,其与鲁米诺之间的弱化学发光信号强烈地受异烟肼的增敏,由此建立了一种新的高灵敏的测定异烟肼的电化学发光分析新方法.结果表明,在最佳的实验条件下,相对电化学发光强度与异烟肼的浓度在 2.0×10-9～2.0×10-6 g/mL范围内呈线性关系,检出限为 6.7×10-10 g/mL,相关系数为 0.9996.此方法已成功用于片剂异烟肼的测定.     

Synthesis of highly crystalline rhombohedral BN triangular nanoplates via a convenient solid state reaction

Highly crystalline rhombohedral boron nitride (r-BN) with regular triangular shapes were synthesized on a large scale in a stainless steel autoclave using B₂O₃ and NaNH₂ as reactants at 600 °C for 6 h. The as-prepared BN triangular nanoplates have an average edge length of 400 nm and the thickness of about 60 nm. The photoluminescence measurements reveal that the r-BN products show strong yellow-green emission. The as-prepared r-BN has potential optical and optoelectronic applications in high temperature devices due to its excellent thermal stability and anti-oxidation properties.     

Separation of inorganic anions on a triazole-functionalized ion exchanger in ion chromatography

The retention behavior of inorganic anions on a triazole-based stationary phase was first examined in ion chromatography. It was initially designed for hydrophilic interaction liquid chromatography and was simply prepared by introducing the triazole groups onto the surface of silica gel via click chemistry. Effective separation of common inorganic anions, including iodate, chloride, bromide, nitrate and iodide, was achieved with Na(2)SO(4) eluent. The logarithm of the retention factor of analytes was observed to be linear with the logarithm of the eluent concentration, and the slopes of the plots were almost the same as those of the ideal theoretical value. The eluent pH value in the range of 3.4-7.0 had little effect on the separation. The utility of the column was demonstrated for the determination of UV-absorbing anions in saliva and tap water.     

Silver CD-R based substrate as a SERS active material

A silver Compact Disc Recortable (CD-R) based substrate has been proposed as an alternative to silver colloids as active material successfully used in surface-enhanced Raman spectroscopy (SERS). Scanning Electron Microscope (SEM) and Energy-Dispersive X-ray Spectroscopy (EDXS) measurements revealed that silver nanoparticles are present over the entire surface of the uncovered reflective layer of commonly used CD-R. The process of preparation of the CD-R based surface is simple, fast and repeatable. Recorded Raman spectra of 10 µM Rhodamine 6G applied to the substrate corroborate strong enhancement of Raman signal. The maximum value of EF was calculated to be about 5.76 × 10⁶. Raman maps are consistent with SEM micrographs and confirmed the presence of a numerous SERS hot spots occurring on the trucks of CD-R based substrate.     

Development of a heterobimetallic Ru(II)-Cu(II) complex for highly selective and sensitive luminescence sensing of sulfide anions

A heterobimetallic ruthenium(II)-copper(II) complex-based luminescent chemosensor, [Ru(bpy)(2)(bpy-DPA)Cu](4+) (bpy: 2,2'-bipyridine; bpy-DAP: 4-methyl-4'-[N,N-bis(2-picolyl)amino-methylene]-2,2'-bipydine), has been designed and synthesized for the highly selective and sensitive recognition and detection of sulfide anions in 100% aqueous solutions. Owing to the high affinity of sulfide to Cu(II), the non-luminescent chemosensor can specifically and rapidly react with sulfide to yield the corresponding ruthenium(II) complex, [Ru(bpy)(2)(bpy-DPA)](2+), accompanied by the remarkable luminescence enhancement. The dose-dependent luminescence enhancement of the sensor shows a good linearity with a detection limit of 20.7 nM for sulfide anions. The novel luminescence sensor has a widely available pH range from 4.5 to 10 and an excellent response selectivity to sulfide only even in the presence of various other anions. Based on this chemosensor, a rapid, selective and sensitive luminescence method for the detection of sulfide anions in wastewater samples was established. The coefficient variations (CVs) of the method are less than 3.1%, and the recoveries are in the range of 90.9-108.5%.     

Applications of thin-layer chromatography and thin-layer electrophoresis in the analysis of inorganic anions: a review

JPC – Journal of Planar Chromatography – Modern TLC - This review is intended to highlight various applications of thin-layer chromatography (TLC) and thin-layer electrophoresis (TLE)...     

A hemicyanine-conjugated copolymer as a highly sensitive fluorescent thermometer

A simple-structured copolymer, poly(NIPAM-co-HC), consisting of N-isopropylacrylamide (NIPAM) and 4-(4-dimethylaminostyryl)pyridine (hemicyanine, HC) units as thermoresponsive and fluorescent signaling parts, respectively, has been synthesized. This copolymer dissolved in water shows very weak fluorescence at <25 degrees C, while showing fluorescence enhancement at >25 degrees C. The fluorescence intensity increases with a rise in temperature and saturates at >40 degrees C, enabling temperature detection at 25-40 degrees C. The fluorescence enhancement is driven by a heat-induced phase transition of the polymer from coil to globule state. The HC units within the coil state polymer exist as the nonfluorescent benzenoid form; however, the less polar domain formed inside the globule state polymer leads to transformation of the HC unit to the fluorescent quinoid form, resulting in heat-induced fluorescence enhancement. The fluorescence intensity measured at 40 degrees C is >20-fold higher than the intensity at <25 degrees C, which is the highest enhancement value among the fluorescent thermometers proposed so far. The polymer shows reversible fluorescence enhancement/quenching, regardless of the heating/cooling process. In addition, the polymer shows high reusability with a simple recovery process.     

Solid-solutioned homojunction nanoplates with disordered lattice: a promising approach toward "phonon glass electron crystal" thermoelectric materials

The concept of "phonon glass electron crystal" (PGEC) was proposed in the mid-1990s to maximize the ZT value for thermoelectric materials, based on its combined advantages of low thermal conductivity as in a glass but high electricity as in a well-ordered crystal. Although a great amount of research in complex materials systems for achieving this concept has been done, a perfect "PGEC" material has not been acquired yet. Herein, we first put forward a solid-solutioned homojunction in high temperature phase with disordered lattice, which possesses both high electrical conductivity and low thermal conductivity, as an effective way to optimize the low/mid-temperature thermoelectric property. As an example, nonambient cubic phase AgBiSe(2) was successfully stabilized to room temperature through the formation of a solid solution by Sb incorporation for the first time, and furthermore, in situ formed homojunctions on the surface of solid-solutioned nanoplates were also first achieved through a simple colloidal method. A significant enhancement of thermoelectric performance at low/mid-temperature was realized through synergistical regulation on electronic and thermal transport. As a result, compared to that of original AgBiSe(2) (ZT = 0.03 at 550 K), the ZT value of AgBi(0.5)Sb(0.5)Se(2) was increased to 0.51 at 550 K by the formation of a solid solution, and then further increased to 1.07 at 550 K by the formation of solid-solutioned homojunction.     

Development of a highly sensitive galvanic cell oxygen sensor

A highly sensitive galvanic cell oxygen sensor was successfully developed for determining parts per billion of oxygen in high purity gases such as nitrogen, argon, etc. The response of this improved sensor was proportional in the range of oxygen concentrations from 10.0 ppm to the detection limit. The response speed in this study was improved to within 90 sec for a 90% response. The detection limit was tentatively found to be less than 0.4 ppb corresponding to S N = 2 .