Determination of Uranium in Natural Waters by Solid Phase Spectrometry

Abstract

A microdetermination method (at the μg1^?1 level) for uranium has been developed, based on Solid-Phase Spectrophotometry (SPS). The uranium reacts with pyridylazo-resorcinol in the presence of fluoride to form a 1:1:1 red ternary complex, which is fixed on an anion-exchange resin. The resin absorbance is measured directly, and allows the determination of uranium in the range of 1–10μg1^?1, with an RSD of 4%. The method has been applied to the determination of U(VI) in natural waters from wells located near the deposits of industrial wastes from a uranium mineral plant in Andujar (Spain).     

False Detection of Cyanide Ion in Photographic Processing Waste Solutions Using Standardized Reference Methods

Abstract

Although cyanide compounds are not incorporated in photographic processing solutions, false detection of cyanide ion is often encountered during the determination of total cyanide by various standardized methods such as ISO, ANSI and JIS. Various organic compounds and nitrogen compounds in the processing solutions were examined because of this false detection. The results suggest that hydrogen cyanide is formed by a reaction between these compounds during the distillation process for the separation of total cyanide, even though ISO, ANSI and JIS were used. The results support the following three mechanisms of cyanide formation involved in the process: (1) Hydroxylammonium salts reacts with another ingredient, formaldehyde, to form formaldoxime, which then decomposes to HCN. (2) Hydroxylammonium is oxidized by air to form nitrite ion, which subsequently reacts with organic compounds such as aminocarboxylic acids and aromatic amines (the colour-developing agent) to form HCN. (3) Potassium permanganate oxidizes aromatic amines to form HCN.     

Chemists around the World,Take Your Part in the Circular Economy!

Based on recent examples and initiatives reported in the literature, this concept article discusses how chemistry can contribute to the circular economy approach in order to improve our current and future economical, societal, and environmental system. Through five proposed levels of contribution, chemists can take a significant part in this global approach via the consideration of green chemistry principles, the simplification of syntheses, the limitation of complex products preparation, the efficient utilization of resources but also the novel ways of waste valorization. A more systematic and generalized environmental and economic assessment from the lab-scale is also recommended. At last, chemists have to work even more collaboratively and in a multidisciplinary way, within chemistry and beyond.     

Application of acoustic methods for a non-destructive evaluation of the elastic properties of several typologies of materials

In solid phase materials, differently from what happens in the fluid phase, elastic waves propagate both through longitudinal and transverse waves. From the speed of propagation of longitudinal and transverse waves, it is possible to evaluate important elastic properties of the solids under study, namely the Young’s modulus, the Poisson’s coefficient, the bulk modulus and the shear modulus. This work suggests an accurate method for measuring wave propagation speeds in homogeneous and non-homogeneous materials with the purpose to evaluate their mechanical properties and the associated uncertainty.First of all, to assess the performance of the proposed methodology, based on the “pulse-echo” technique, in terms of accuracy and precision, measurements of wave propagation speeds have been carried out, in atmospheric conditions, in well-known homogeneous and isotropic materials, such as copper, aluminum, stainless steel and also polymethyl methacrylate (Plexiglas®), Teflon® and optical glass BK7. These results were compared with the values reported in literature (if present), showing how published speed of sound data are very disperse and not so reliable owing to the lack of a precise uncertainty evaluation and of the temperature value associated to the measurement. Then, the same experimental apparatus was used for measuring speed of sound as a function of temperature (from 274.15 to 313.15 K) for 304 stainless steel and oxygen free copper, showing a good accuracy of the results also for temperature conditions far from ambient. Finally, the same procedure was applied to a non-homogeneous solid, obtaining some very preliminary results in typical mediterranean building material, as Carrara marble.     

Thermo and mechanoluminescence studies of BZT phosphor

Mechanoluminescence (ML) and thermoluminescence (TL) in barium zirconium titanate (BZT) is reported for the first time. The BZT powder sample, belonging to perovskite category is synthesized using solid state reaction technique. The sample is prepared at a temperature of 1200 °C. The obtained specimen is thoroughly characterized paying particular attention to their structure, composition, morphology and optical properties. The surface morphology and structural properties are analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD patterns confirm the formation of crystalline perovskite type cubic structure. Also, highly agglomerated, porous and regular shaped particles are seen by SEM. The optical properties of as prepared sample is presented and discussed in terms of ML and TL. The ML intensity is found to be maximum for the sample irradiated for 10 min. More than one maxima in TL glow curve reveals that the traps are distributed in separate groups at different depths and corresponding values are calculated using initial rise method.     

Automated capillary electrophoresis with on-line preconcentration by solid phase extraction using a sequential injection manifold and contactless conductivity detection

An extension of a capillary electrophoresis instrument coupled to a sequential injection analysis manifold was developed for automated measurements with on-line solid-phase extraction preconcentration. An in-house built capacitively coupled contactless conductivity detector was employed for sensitive detection with narrow capillaries of 25 μm internal diameter. The system was assembled into standardized 19 in. frames and racks for easy transport and mobile deployment. The system can be left running unattendedly without manual intervention with good operation stability. To demonstrate the application of the system, a method for the determination of four drugs, namely ibuprofen, diclofenac, naproxen and bezafibrate, was developed with enrichment factors of up to several hundreds. Detection of the drug residues down to the nM-scale was found possible and the method was found suitable for the detection of ibuprofen in the waste water of a hospital in Hanoi.     

Calibration of the complex matrix effects on the sampling of polycyclic aromatic hydrocarbons in milk samples using solid phase microextraction

Solid phase microextraction (SPME), a simple, fast and promising sampling technique, has been widely used for complex sample analysis. However, complex matrices could modify the absorption property of coatings as well as the uptake kinetics of analytes, eventually biasing the quantification results. In the current study, we demonstrated the feasibility of a developed calibration method for the analysis of polycyclic aromatic hydrocarbons (PAHs) in complex milk samples. Effects of the complex matrices on the SPME sampling process and the sampling conditions were investigated. Results showed that short exposure time (pre-equilibrium SPME, PE-SPME) could increase the lifetime of coatings, and the complex matrices in milk samples could significantly influence the sampling kinetics of SPME. In addition, the optimized sampling time, temperature and dilution factor for PAHs were 10 min, 85 °C and 20, respectively. The obtained LODs and LOQs of all the PAHs were 0.1–0.8 ng/mL and 1.4–4.7 ng/mL, respectively. Furthermore, the accuracy of the proposed PE-SPME method for milk sampling was validated by the recoveries of the studied compounds in two concentration levels, which ranged from 75% to 110% for all the compounds. Finally, the proposed method was applied to the screening of PAHs in milk samples.     

Synthesis and application of molecularly imprinted nanoparticles combined ultrasonic assisted for highly selective solid phase extraction trace amount of celecoxib from human plasma samples using design expert (DXB) software

In this work molecular imprinted nanoparticles (MINPs) was synthesized and applied for ultrasonic assisted solid phase extraction of celecoxib (CEL) from human plasma sample following its combination by HPLC–UV. The MINPs were prepared in a non-covalent approach using methacrylic acid as monomer, CEL as template, ethylene glycol dimethacrylate as cross-linker, and 2,2-azobisisobutyronitrile (AIBN) as the initiator of polymerization. pH, volume of rinsing and eluent solvent and amount of sorbent influence on response were investigated using factorial experimental design, while optimum point was achieved and set as 250 mg sorbent, pH 7.0, 1.5 mL washing solvent and 2 mL eluent by analysis of results according to design expert (DX) software. At above specified conditions, CEL in human plasma with complicated matrices with acceptable high recoveries (96%) and RSD% lower than 10% was quantified and estimated.The proposed MISPE-HPLC–UV method has linear responses among peak area and concentrations of CEL in the range of 0.2–2000 μg L⁻¹, with regression coefficient of 0.98. The limit of detection (LOD) and quantification (LOQ) based on three and ten times of the noise of HPLC peaks correspond to blank solution were 0.08 and 0.18 μg L⁻¹, respectively.     

Application of Graphene as a Sorbent for Simultaneous Preconcentration and Determination of Trace Amounts of Cobalt and Nickel in Environmental Water and Vegetable Samples

A new method using a column packed with graphene as adsorbent was developed for the preconcentration of trace amounts of cobalt (Co) and nickel (Ni) prior to their determinations by flame atomic absorption spectrometry. Several factors influencing the extraction efficiency of Co and Ni and their subsequent determinations, such as pH, amounts of the chelating agent, flow rates of sample and eluent solution, eluent type and its volume, breakthrough volume, and adsorption capacity were established. Under the optimum conditions, the calibration graphs were linear in the range of 4.0‐200.0 μg L^?1 and 5.0‐200.0 μg L^?1 with detection limits of 0.36 μg L^?1 and 0.51 μg L^?1 for Co and Ni, respectively. Good relative standard deviations for ten determinations of 100.0 μg L^?1 of Co and Ni were 3.2 and 3.6%, respectively. The results for determination of Co and Ni in tap water, river water, sea water, vegetable and spiked samples have demonstrated the accuracy and applicability of the proposed method. To validate the proposed method, three certified reference materials of environment water (GSBZ 50030‐94 and GSB 07‐1186‐2000) and tomato leaf (GSBZ 51001‐94) were analyzed, and the determined values were in good agreement with the certified values.     

Synthesis of α-aminonitriles using silica-bonded N-propylpiperazine sulfamic acid as a recyclable catalyst

<正>α-Aminonitriles were synthesized via a one-pot three-component condensation of aldehydes,amines,and trimethylsilyl cyanide using silica-bonded N-propylpiperazine sulfamic acid(SBPPSA) as a recyclable solid acid at room temperature.SBPPSA showed much the same efficiency when used in consecutive reaction runs.