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A simple and sensitive double injection/single detector flow injection analysis (FIA) method is proposed for the simultaneous kinetic determination of ascorbic acid (AA) and uric acid (UA). This method is based upon the difference between the rates of the AA and UA reactions with Fe 3 + in the presence of 1, 10-phenanthroline (phen). The absorbance of Fe 2 + /1, 10-phenanthroline (Fe-phen) complex obtained as the product was measured spectrophotometrically at 510 nm. To reach a good accuracy in the differential kinetic determination via the mathematical manipulations of the transient signals, different criteria were considered in the selection of the optimum conditions. The multi criteria decision making (MCDM) approach was applied for the selection of the optimum conditions. The importance weights of the evaluation criteria were determined using the analytic hierarchy process, entropy method, and compromised weighting (CW). The experimental conditions (alternatives) were ranked by the technique for order preference by similarity to an ideal solution. Under the selected optimum conditions, the obtained analytical signals were linear in the ranges of 0.50–5.00 and 0.50–4.00 mg L − 1 for AA and UA, respectively. The 3σ detection limits were 0.07 mg L − 1 for AA and 0.12 mg L − 1 for UA. The relative standard deviations for four replicate determinations of AA and UA were 2.03% and 3.30% respectively. The method was also applied for the analysis of analytes in the blood serum, Vitamine C tablets, and tap water with satisfactory results. [ABSTRACT FROM AUTHOR]

The performance of the Nano-magnetite Fe 3 O 4 impregnated onto walnut shell (Fe 3 O 4 -WNS), which possessed the adsorption features of walnut shell and the magnetic property of Fe 3 O 4 , was investigated for the elimination of the methyl violet and Rhodamine 6G from contaminated aqueous solutions. The effects of different experimental variables on the removal efficiency of the cited dyes were examined. Then these variables were used as the inputs to generate linear and non-linear models such as the multiple linear regression, random forest, and artificial neural network to predict the removal efficiency of these dye species at different experimental conditions. The validation studies of these models were performed using the test set, which was not present in the modeling procedure. It was found that ANN had a higher ability to predict the adsorption process under different experimental conditions, and could be applied for the development of an automated dye wastewater removal plant. Also the maximum adsorption capacity (q max ) indicated that the q max value for Fe 3 O 4 -WNS for removal of cationic dyes was comparable or better than that for some reported adsorbents. Also it should be cited that exhausted Fe 3 O 4 -WNS was regenerated using dishwashing liquid, and reused for removal of the cited dye species from aqueous solutions. [ABSTRACT FROM AUTHOR]

In this study, the photo-decolorization of a mixture of methylene blue (MB) and methyl orange (MO) was investigated using Ag–ZnO multipods. The photo-catalyst used, ZnO multipods, was successfully synthesized. The surface of ZnO microstructure was modified by deposition of different amounts of Ag nanoparticles (Ag NPs) using the photo-reduction method. The as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–Vis and atomic absorption spectroscopy. The photo-catalytic efficiency of Ag–ZnO is mainly controlled by the amount of Ag NPs deposited on the ZnO surface. The results obtained suggest that Ag–ZnO containing 6.5% Ag NPs, has the highest photo-catalytic performance in the simultaneous photo-degradation of dyes at a shorter time. [ABSTRACT FROM AUTHOR]

In this work, a flow injection analysis (FIA) method was introduced for the determination of trace amounts of thiourea in tap water. This method is based upon the inhibition effect of thiourea on the reaction between meta-cresol purple (MCP) and potassium bromate catalyzed by bromide ions in a sulfuric acid medium. In the presence of thiourea, an induction period appears in the reaction system, and as a result, the absorbance of MCP increases at 525 nm in the FIA manifold. The chemical and FIA variables are studied and optimized using the univariate and Simplex optimization methods. Under the optimum conditions, thiourea can be determined in the range of 0.100–13.0 μg mL −1 . The limit of detection (3 σ ) for thiourea was found to be 0.0310 μg mL −1 . The relative standard deviations (RSDs) for six replicate determinations of 0.500, 5.00, and 12.0 μg mL −1 of thiourea were 4.0%, 1.8%, and 1.2%, respectively. The proposed method was also applied for the determination of thiourea in orange juice and orange peel samples with recoveries in the range of 98.0–101%. The analytical speed of the method was calculated to be about 120 sample per hour. [ABSTRACT FROM AUTHOR]

A five-coordinated Fe(III) complex with the distorted trigonal bipyramidal configuration was synthesized by reactions of FeCl3•6H2O and 2-(2'-hydroxyphenyl)oxazoline (Hphox) as a bidentate ON donor oxazoline ligand. Complex [Fe(phox)2Cl] was fully characterized, including by single-crystal X-ray structure analysis. DFT calculations were accompanied with experimental results in order to obtain a deeper insight into the electronic structure and vibrational normal modes of complex. Oxidation of sulfides to sulfoxides in one-step was conducted by this complex as catalyst using urea hydrogen peroxide (UHP) in mixture of CH2Cl2/CH3OH (1:1) under air at room temperature. The results show that using this system in oxidation of sulfides, sulfoxides are obtained as the main products, together with variable amounts of sulfones (≼13%), depending on the nature of the substrate. [ABSTRACT FROM AUTHOR]

Abstract: A rapid, simple, accurate, and highly selective spectrophotometric method is proposed for the determination of periodate in water samples. This method is based on the reaction of methylene green with periodate in the presence of iodide. The decrease in the absorbance of methylene green is used to monitor the reaction spectrophotometrically at 613nm. Under the optimum conditions, periodate could be determined in the concentration range 0.18–6.0μgmL−1. The detection limit for the method is 0.010μgmL−1. The influence of various foreign species was studied, and it was found that iodate did not interfere with the determination even in the presence of 200-fold of periodate. The relative standard deviations for six replicate determinations of 0.30, 0.50, 1.0, 1.5, 4.0, and 5.5μgmL−1 of periodate were 3.33, 2.0, 1.6, 1.33, 0.50, and 0.55%, respectively. The proposed method was applied to the determination of periodate in water samples and indirect determination of ethylene glycol in antifreeze and glycerol in vegetable oil via malaprade reaction, and satisfactory results were obtained. [Copyright &y& Elsevier]

Abstract: This paper describes a new, simple, sensitive, and selective catalytic–kinetic-spectrophotometric method for the determination of trace amounts of oxalate in vegetable and water samples. The method is based upon the catalytic effect of oxalate on the oxidation of crystal violet (CV) by dichromate in sulfuric acid media. The reaction was followed by measuring the decrease in absorbance of CV at 630nm (λ max of CV). The dependence of sensitivity on the reaction variables was studied and discussed. Under the optimum conditions, a fixed time procedure was used to obtain a linear calibration curve in the oxalate concentration ranges of 0.20–5.5μgmL−1 of oxalate. The calculated detection limit was 0.050μgmL−1. The relative standard deviations for ten replicate determinations of 0.40, 1.8, and 2.5μgmL−1 of oxalate were 6.0%, 2.5%, and 1.8%, respectively. The effect of the presence of various species commonly associated with real samples was also investigated. The proposed method was successfully applied for the determination of oxalate in vegetable and spiked water samples. [Copyright &y& Elsevier]

Abstract: A new, simple and sensitive kinetic spectrophotometric method with no need for removing of interfering substances is proposed for the determination of thiocyanate ion in biological and water samples. The procedure is based on the inhibiting effect of thiocyanate on the sodium periodate–potassium bromide–meta cresol purple (MCP) system in acidic media. The induction period of the reaction is proportional to the SCN− concentration. The decolorization of meta cresol purple by the reaction products was used to monitor the reaction spectrophotometrically at 525nm. Under optimum conditions, thiocyanate can be determined in the range of 0.02–0.8μgml−1 with a 3σ detection limit of 5ngml−1. The relative standard deviations for 10 replicate determinations of 0.060, 0.10 and 0.50μgml−1 thiocyanate are 3.7, 2.4 and 1.0%, respectively. This method has been successfully used to the determination of thiocyanate content in smokers and non-smokers saliva and spiked water sample. [Copyright &y& Elsevier]

Abstract: A simple, sensitive and selective spectrophotometric method for the simultaneous determination of Co(II) and Pd(II) using partial least square (PLS) calibration and H-point standard addition method is described. The method is based on the complex formation of Co(II) and Pd(II) with 4-(2-pyridylazo) resorcinol (PAR) in acidic media and in the presence of sodium dodecyl sulfate (SDS) as a micellizing agent. Acidic media and the presence of a micellar system improve selectivity and sensitivity, respectively. By applying PLS calibration, Co(II) and Pd(II) can be determined in the range of 0.20–2.0 and 0.40–4.0μgml−1, respectively. The relative errors of prediction for the determination of Co(II) and Pd(II) in the 10 prediction samples were 1.69 and 1.72%, respectively. The results of applying H-point standard addition method show that Co(II) and Pd(II) can be determined simultaneously with concentration ratio of Co(II) to Pd(II) varying between 7:1 and 1:8 in the mixed samples. Both proposed methods (PLS and HPSAM) were applied to the determination of Co(II) and Pd(II) in several alloy solutions with satisfactory results. [Copyright &y& Elsevier]

Abstract: A simple, novel and sensitive spectrophotometric method was described for the simultaneous determination of cobalt, nickel and palladium. The method is based on the complex formation of Co, Ni and Pd with 1-(2-pyridylazo)-2-naphtol (PAN) in Tween-80 micellar media. All factors affecting on the sensitivity were optimized and the linear dynamic range for determination of Co, Ni and Pd was found. The experimental calibration matrix was designed by measuring the absorbance over the range of 520–700nm for 21 samples of 0.10–1.0, 0.050–0.50 and 0.050–4.0μgml−1 of Co, Ni and Pd, respectively. The partial least square (PLS) modeling based on singular value decomposition (SVD) was used for the multivariate calibration of the spectrophotometric data. The direct orthogonal signal correction was used for pre-processing of data matrices and the prediction results of model, with and without using direct orthogonal signal correction, were statistically compared. The effects of various anions and cations on selectivity of the method were investigated. The proposed method was successfully applied to the determination of Co, Ni and Pd in water and alloy samples. [Copyright &y& Elsevier]

A flow injection (FI) system is described for the sequential determination of periodate and iodate based on their reaction with iodide at pH 3.5. Two sample plugs were injected into the same carrier stream sequentially. One injection is for the iodate determination and the other for the sum of iodate and periodate determination. For iodate determination, molybdate solution buffered at pH of 3.5 was used for selective masking of periodate. The influences of reagent concentrations were studied by a univariable method and the influence of FI manifolds was studied using univariable and simplex method. Periodate and iodate can be determined in the range of 0.050–5.0 and 0.050–10 μg/ml, respectively. The 3σ limit of detection was 0.030 and 0.050 μg/ml for periodate and iodate, respectively. The proposed method has been applied for the sequential determinations of periodate and iodate in water samples. [Copyright &y& Elsevier]

A simple and efficient flow-injection method was used with good results to determine periodate and iodate in water. The method is based on the reaction of periodate or iodate with pyrogallol red in sulfuric acid media. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of pyrogallol red at 470 nm. The chemical and FIA variables were established using the univariate and simplex optimization methods. The calibration curve was linear over the concentration ranges of 0.8–73.0 and 2.0–100.0 μM for IO4− and IO3−, respectively. The detection limits were 0.7 and 1.0 μM for IO4− and IO3−, respectively. The sample throughput was 20±5 h−1. The influence of potential interfering ions in the determination of the anions was tested. The relative standard deviations for 4.20 and 5.73 μM periodate and iodate were 1.8 and 2.2%, respectively. [ABSTRACT FROM AUTHOR]

[Display omitted] • Methylene blue and Crystal violet removal studies using magnetic biosorbents prepared from Heracleum Persicum waste. • The quasi-second-order kinetic model best showed the methylene blue and crystalline violet data in the binary system. • The extended Langmuir multicomponent model better fit the methylene blue and crystal violet experimental data in binary aqueous solution. • RF has a higher predictive ability than ANN due to its better statistical parameters. Synthetic dyes can be hazardous to the ecosystem, even at low concentrations in the effluent. In this research, the Heracleum persicum stems-Fe3O4 (MHPS) adsorbent performance for the removal of crystal violet (CV) and methylene blue (MB) from binary aqueous solutions was investigated in a batch method under the influence of different parameters. In addition, predictive models for the adsorption process were developed using machine learning techniques such as artificial neural networks and random forests. ANN and RF models achieved high R2 values of 0.9501 and 0.9797 for CV, 0.9471, and 09,834 for MB, respectively, and obtained low MSE values of 0.07107 and 0.03405 for CV, 0.09933, and 0.02908 for MB. The proposed adsorbent is cheap and eco-friendly and, on the other hand, is easily collected by the magnetic field. The adsorbent was characterized by applying FESEM-EDX, FESEM, BET, and FTIR. Various isotherm and kinetics models for the simultaneous adsorption of CV and MB were investigated in aqueous solutions. The adsorption isotherm and kinetics studies explain that the extended Langmuir model and pseudo-second-order models are best suited for CV and MB in the binary solution. The exothermic adsorption was achieved in the temperature range of 5–45 °C. [ABSTRACT FROM AUTHOR]

Achieving specific selectivity and high sensitivity for the colorimetric recognition of copper(II) ions in aqueous media over a complex background of potentially competing metal ions is inherently challenging in sensor development. Thus, a novel azo–azomethine receptor ( L ) based on the combination of 2-amino-3-(5-bromo-2-hydroxybenzylamino)maleonitrile and azo-coupled salicylaldehyde scaffold has been designed and synthesized for the naked-eye and rapid detection of Cu 2+ ion at trace level in a wide pH range. Accordingly, the devised chemosensor distinguished Cu 2+ from other metal ions by distinct color change from light yellow to light brown without any expensive equipment. The binding stoichiometry between Cu 2+ and L has been investigated using Job’s plot and MALDI-TOF mass analysis. Remarkably, the current sensor can detect Cu 2+ ions even at 1.07 μM level, which is lower than the World Health Organization (WHO) permissible level (30 μM) in drinking water. Furthermore, sensor L was successfully utilized in the preparation of test strips for the detection of copper(II) ions from aqueous environment. [ABSTRACT FROM AUTHOR]

[Display omitted] • The use of Gypsophila aretioides stems as a bio-sorbent to remove the crystal violet (CV) dye. • The bio-sorbent is cheap, simple, minimize excess sludge and eco-friendly. • The column breakthrough curves were fitted by the Thomas and Yoon-Nelson models. • The batch and fixed-bed adsorptions were evaluated by the random forest model. • After five times of regeneration, the removal percentage was high with both methods. In this work, the Gypsophila aretioides (GYP-A) stem is used as a biosorbent to remove crystal violet (CV) by the static and dynamic systems from aqueous solutions; the biosorbent is interesting in green chemistry and, on the other hand, cheaper than activated carbon and does not have the limitation of industrialization. The effects of different operating parameters such as pH(3–9), biosorbent dosage(0.4–1.8 mg/L), and initial concentration of CV(100–250 mg/L) and time for the batch method and the bed height, inlet CV concentration(75–250 mg/L), and flow rate(3–8) on the breakthrough curves for the continuous method is investigated. The result of CV adsorption onto GYP-A using the batch method indicates that the model fits Freundlich > Temkin > Langmuir > R-D, and R2 equal 0.9953, 0.9847, 0.9161, 0.7909 were obtained for isotherm model, respectively. A pseudo-second-order model (R2 = 0.9995–0.9997) is recommended to describe the adsorption kinetics. The Thomas and Yoon-Nelson models were analyzed to study the adsorption kinetics. The random forest model shows an excellent ability to predict the parameters involved in the CV adsorption process with appropriate accuracy and useable for large data, robust against noise; it can be very effective in selecting important variables. [ABSTRACT FROM AUTHOR]

• Determination of nitroaniline isomers in binary mixtures by four spectrophotometric methods. • Similar precision and accuracy of CC and RD methods compared to PLS and PCR methods. • Selection of best pair of wavelengths and divisor in proposed methods was studied. • No need to computer programs or sophisticated equipment in suggested methods. In the present work, four simple and economic spectrophotometric methods, namely constant center (CC), ratio difference (RD), H-point standard addition method (HPSAM), and ratio H-point standard addition method (RHPSAM) were employed for the simultaneous determination of meta and para -nitroaniline with severely overlapping spectra without unitizing the preliminary physical separation techniques. In each method, the parameters affecting the resolution of the spectra were optimized to determine the cited isomers in a binary mixture with a high accuracy. Under the optimized conditions, the results obtained showed that from cited methods used, the CC and RD methods have the least errors in determination of the concentration of highly spectral overlapping species. The mean percentage recovery values for the binary mixture of meta- and para -nitroaniline were found to be 95.98 and 98.78 using the RD method, and 101.85 and 100.23 using the CC method, respectively. For comparison of the powerful multivariate methods including the principal component regression (PCR) and partial least squares (PLS) were also applied. The mean percentage recovery values for the binary mixtures of the cited isomers were found to be 101.62 and 101.47 using the PCR method, and 101.00 and 101.36 using the PLS method, respectively. A statistical comparison of the methods demonstrated that there was no significant difference between the RD, CC, PCR, and PLS methods and the reported HPLC method regarding both accuracy and precision. The proposed methods have an admissible precision and accuracy for determination of the two isomers in their binary mixtures in tap water as a real sample. [ABSTRACT FROM AUTHOR]

[Display omitted] • Three novel curcumin-fused aldohexose compounds 3 (a-c) were synthesized. • The compounds have been property characterized and further used in a series of biological in vivo and in vitro assays. • All compounds inhibited α-Amy and α-Gls by mixed and competitive mechanisms, respectively. • The intrinsic fluorescence of α-Amy was quenched by the interaction with compounds 1 and 3b through a dynamic quenching mechanism. • Molecular docking and molecular dynamics (MD) simulations indicated that all compounds mainly interacted with amino acid residues located in the active site of proteins. • In-vivo studies confirmed the plasma glucose diminution by administration compound 3b compared to the positive control. Curcumin (bis-α,β-unsaturated β-diketone) plays an important role in the prevention of numerous diseases, including diabetes. Curcumin, as an enzyme inhibitor, has ideal structural properties including hydrophobic nature, flexible backbone, and several available hydrogen bond (H-bond) donors and acceptors. In this study, curcumin-fused aldohexose derivatives 3 (a-c) were synthesized and used as influential agents in the treatment of diabetes with inhibitory properties against two carbohydrate-hydrolyzing enzymes α-glucosidase (α-Gls) and α-amylase (α-Amy) which are known to be significant therapeutic targets for the reduction of postprandial hyperglycemia. These compounds were isolated, purified, and then spectrally characterized via FT-IR, Mass, 1H, and 13C NMR, which strongly confirmed the targeted product's formation. Also, their inhibitory properties against α-Gls and α-Amy were evaluated spectroscopically. The Results indicated that all compounds strongly inhibited α-Amy and α-Gls by mixed and competitive mechanisms, respectively. The intrinsic fluorescence of α-Amy was quenched by the interaction with compounds 1 and 3b through a dynamic quenching mechanism, and the 1 and 3b /α-Amy complexes were spontaneously formed, mainly driven by the hydrophobic interaction and hydrogen bonding. Fourier transform infrared spectra (FT-IR) comprehensively verified that the binding of compounds 1 and 3b to α-Amy would change the conformation and microenvironment of α-Amy, thereby inhibiting the enzyme activity. Docking and molecular dynamics (MD) simulations showed that all compounds interacted with amino acid residues located in the active pocket site of the proteins. In vivo studies confirmed the plasma glucose diminution after the administration of compound 3b to Wistar rats. Accordingly, the results of the current work may prompt the scientific communities to investigate the possibility of compound 3b application in the clinic. [ABSTRACT FROM AUTHOR]