Synthesis of salicylaldehyde-modified mesoporous silica and its application as a new sorbent for separation, preconcentration and determination of uranium by inductively coupled plasma atomic emission spectrometry

A new functionalized mesoporous silica (MCM-41) using salicylaldehyde was utilized for the separation, preconcentration and determination of uranium in natural water by inductively coupled plasma atomic emission spectrometry (ICP-AES).Experimental conditions for effective adsorption of trace levels of U(VI) were optimized. The preconcentration factor was 100 (1.0 mL of elution for a 100 mL sample volume). The analytical curve was linear in the range 2-1000 μg L⁻¹ and the detection limit was 0.5 ng mL⁻¹. The relative standard deviation (R.S.D.) under optimum conditions was 2.5% (n = 10). Common coexisting ions did not interfere with the separation and determination of uranium at pH 5. The sorbent exhibited excellent stability and its sorption capacity under optimum conditions has been found to be 10 mg of uranium per gram of sorbent. The method was applied for the recovery and determination of uranium in different water samples.     

Extraction and preconcentration of ultra trace amounts of beryllium from aqueous samples by nanometer mesoporous silica functionalized by 2,4-dihydroxybenzaldehyde prior to ICP OES determination

A new functionalized nanometer mesoporous silica (MCM-41) using 2,4-dihydroxybenzaldehyde (4-OHsal) was applied as an effective sorbent for solid phase extraction (SPE) of beryllium ions from aqueous solution followed by inductively coupled plasma optical emission spectrometric detection (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ion were investigated in batch method. In order to perform the batch mode of SPE, known amount of sorbent was added to a test tube containing sample solution buffered at pH 7.2. After manual shaking and centrifugation the aqueous phase was decanted and beryllium was desorbed by adding 1.0 mL of 1.0 mol L^?1 HNO₃ to the sedimented sorbent. The sorbent was separated by centrifugation and the concentration of beryllium in the supernatant was determined by ICP OES. The maximum sorption capacity of the modified MCM-41 was found to be 34 mg g^?1. The sorbent exhibited good stability, reusability and fast rate of equilibrium for sorption/desorption of beryllium ions. The present method was used for preconcentration and determination of beryllium for water samples. Under optimal conditions, the limit of detection (LOD) obtained was 0.3 ng L^?1. The accuracy of the procedure was evaluated by analysis of the certified reference material (NIST 1640).     

Solving the problem of packing equal and unequal circles in a circular container

In this paper we propose a Monotonic Basin Hopping approach and its population-based variant Population Basin Hopping to solve the problem of packing equal and unequal circles within a circular container with minimum radius. Extensive computational experiments have been performed both to analyze the problem at hand, and to choose in an appropriate way the parameter values for the proposed methods. Different improvements with respect to the best results reported in the literature have been detected.     

Development and validation of a capillary electrophoresis-indirect photometric detection method for the determination of the non-UV-absorbing 1,4-dideoxy-1,4-imino-D-arabinitol in active pharmaceutical ingredients,solutions and tablets using an internal standard

A high speed, selective, and robust capillary electrophoresis (CE) method with high capacity was developed and validated for determination of assay of 1,4-dideoxy-1,4-imino-D-arabinitol in active pharmaceutical ingredients, solutions, and tablets during the development work at preclinical and Phase I and II clinical studies. 1,4-Dideoxy-1,4-imino-D-arabinitol, tartrate has (almost) no UV absorption. Therefore, the developed CE method for quantification was based on indirect UV detection. A cation CE principle was chosen using an electrolyte at pH 4.0 containing dimethyldiphenylphosphonium hydroxide, which has a strong UV absorbance. The quantification was performed using internal standard technique, by which piperidine was used as internal standard. The method was validated. The validation results showed that the CE method was suitable for the assay (and dissolution) analysis.     

Determination of Trihalomethanes in Drinking Water by Dispersive Liquid–Liquid Microextraction then Gas Chromatography with Electron-Capture Detection

Dispersive liquid–liquid microextraction (DLLME) has been used for preconcentration of trihalomethanes (THMs) in drinking water. In DLLME an appropriate mixture of an extraction solvent (20.0 μL carbon disulfide) and a disperser solvent (0.50 mL acetone) was used to form a cloudy solution from a 5.00-mL aqueous sample containing the analytes. After phase separation by centrifugation the enriched analytes in the settled phase (6.5 ± 0.3 μL) were determined by gas chromatography with electron-capture detection (GC–ECD). Different experimental conditions, for example type and volume of extraction solvent, type and volume of disperser solvent, extraction time, and use of salt, were investigated. After optimization of the conditions the enrichment factor ranged from 116 to 355 and the limit of detection from 0.005 to 0.040 μg L⁻¹. The linear range was 0.01–50 μg L⁻¹ (more than three orders of magnitude). Relative standard deviations (RSDs) for 2.00 μg L⁻¹ THMs in water, with internal standard, were in the range 1.3–5.9% (n = 5); without internal standard they were in the range 3.7–8.6% (n = 5). The method was successfully used for extraction and determination of THMs in drinking water. The results showed that total concentrations of THMs in drinking water from two areas of Tehran, Iran, were approximately 10.9 and 14.1 μg L⁻¹. Relative recoveries from samples of drinking water spiked at levels of 2.00 and 5.00 μg L⁻¹ were 95.0–107.8 and 92.2–100.9%, respectively. Comparison of this method with other methods indicates DLLME is a very simple and rapid (less than 2 min) method which requires a small volume of sample (5 mL).     

Cumulative Residual q-Fisher Information and Jensen-Cumulative Residual χ2 Divergence Measures

In this work, we define cumulative residual q-Fisher (CRQF) information measures for the survival function (SF) of the underlying random variables as well as for the model parameter. We also propose q-hazard rate (QHR) function via q-logarithmic function as a new extension of hazard rate function. We show that CRQF information measure can be expressed in terms of the QHR function. We define further generalized cumulative residual χ2 divergence measures between two SFs. We then examine the cumulative residual q-Fisher information for two well-known mixture models, and the corresponding results reveal some interesting connections between the cumulative residual q-Fisher information and the generalized cumulative residual χ2 divergence measures. Further, we define Jensen-cumulative residual χ2 (JCR-χ2) measure and a parametric version of the Jensen-cumulative residual Fisher information measure and then discuss their properties and inter-connections. Finally, for illustrative purposes, we examine a real example of image processing and provide some numerical results in terms of the CRQF information measure.     

An integrated production and preventive maintenance planning model

We are given a set of items that must be produced in lots on a capacitated production system throughout a specified finite planning horizon. We assume that the production system is subject to random failures, and that any maintenance action carried out on the system, in a period, reduces the system’s available production capacity during that period. The objective is to find an integrated lot-sizing and preventive maintenance strategy of the system that satisfies the demand for all items over the entire horizon without backlogging, and which minimizes the expected sum of production and maintenance costs. We show how this problem can be formulated and solved as a multi-item capacitated lot-sizing problem on a system that is periodically renewed and minimally repaired at failure. We also provide an illustrative example that shows the steps to obtain an optimal integrated production and maintenance strategy.     

碱性溶液中电聚酪胺-铜草酸盐纳米复合物修饰铜电极电催化甲醇氧化(英文)

A polytyramine-copper oxalate nanocomposite modified copper(PTCOxNMC) electrode prepared by electropolymerization was examined for electrocatalytic activity towards the oxidation of methanol in alkaline solution using cyclic voltammetry and impedance spectroscopy. The prepared PTCOxNMC electrode showed a significantly high response for adsorbed methanol oxidation. The effects of various parameters such as potential scan rate and methanol concentration on the electrocatalytic oxidation at the surface of the PTCOxNMC electrode were investigated. Spectrometry techniques such as Fourier transform infrared spectroscopy and scanning electron microscopy were used to determine the surface physical characteristics of the modified electrode and revealed that the polytyramine-copper oxalate nanocomposite particles were highly dispersed on the surface of the copper electrode with a narrow size up to 40 nm. The very high current density obtained for the catalytic oxidation may have resulted from the high electrode surface area caused by modification with the poly-tyramine-copper oxalate nanocomposite.     

A new simple sensitive differential pulse polarographic method for the determination of acrylamide in aqueous solution

A new simple sensitive differential pulse polarographic (DPP) method was investigated for the determination of acrylamide (AA) directly in a neutral aqueous solution. The AA showed a well-defined and well-resolved peak in pure aqueous LiCl at −1.84 V in the potential range from −1.6 V to −1.97 V at nitrogen pressure of 0.5 kg cm⁻². Among the various electrolytes studied, the AA showed good DPP response in the presence of LiCl and tetra methyl ammonium iodide, while it showed poor response in the presence of tetra butyl ammonium hydroxide and tetra butyl ammonium bromide due to their strong adsorption on the surface of electrode which hindered its reduction. The effect of LiCl concentration, the cyclic voltammetric response and the drop time study showed that AA exhibited an irreversible adsorptive electrochemical behavior. The good electrochemical response in pure aqueous medium suggested that hydrogen bonding might be involved which may favor the electrode reaction. Under optimized conditions, the peak current was linear in the entire concentration range from 0.2 mg L⁻¹ to 20 mg L⁻¹ with the correlation coefficient of R² = 0.9998. The method showed good reproducible results with R.S.D. of 0.3% (n = 16). The detection limit (LOD) was 27 μg L⁻¹. The influence of various interfering agents was also studied. The method was applied successfully for the quantification of AA in water samples without any interference effect from alkali metals.     

Application of fractional factorial design and Doehlert matrix in the optimization of experimental variables associated with the ultrasonic-assisted acid digestion of chocolate samples for aluminum determination by atomic absorption spectrometry

A simple and rapid method based on ultrasound energy is described for the determination of aluminum (AI) in complex matrixes of chocolate and candy samples by electrothermal atomic absorption spectrometry. The optimization strategy was carried out using multivariate methodologies. Five variables (temperature of the ultrasonic bath; exposure time to ultrasound energy; volumes of 2 acid mixtures, HNO3-H2SO4-H2O2 (1 + 1 + 1) and HNO3-H2O2 (1 + 1); and sample mass) were considered as factors in the optimization process. Interactions between analytical factors and their optimal levels were investigated using fractional factorial and Doehlert matrix designs. Validation of the ultrasonic-assisted acid digestion procedure was performed against standard reference materials, milk powder (SRM 8435) and wheat flour (SRM 1567a). The proposed procedure allowed Al determination with a detection limit of 2.3 microg/L (signal-to-noise = 3) and a precision, calculated as relative standard deviation, of 2.2% for a set of 10 measurements of certified samples. The recovery of Al by the proposed procedure was close to 100%, and no significant difference at the 95% confidence level was found between determined and certified values of Al. The proposed procedure was applied to the determination of Al in chocolate and candy samples. The results indicated that cocoa-based chocolates have higher contents of Al than milk- and sugar-based chocolates and candies.