A New Sensitive Fluorescence Sensor and Photocatalyst for Determination and Degradation of Sodium Valproate Using g-C3N4@Fe3O4@CuWO4 Nanocomposite and FCCD Optimization.

In this research, carbon nitride nanocomposite coupled with Fe3O4 and CuWO4 was thermally synthesized and characterized by different techniques, including SEM, TEM, XRD, EDX, and FTIR. Due to sodium valproate's luminescence quenching of this nanocomposite, a reliable, accurate, sensitive, selective, and fast-acting sodium valproate assay was proposed. Optimization of this fluorescent sensor was carried out by the FCCD approach. In the optimum conditions, the plot of sodium valproate concentration versus nanocomposite fluorescence emission showed a linear response (R2 = 0.9918), with a range of 0-0.55 µM, the limit of detection (S/N = 3) equal to 0.85 nM and limit of qualification equal to 2.82 nM. Photocatalytic activity of g-C3N4@Fe3O4@CuWO4 (40%) nanocomposite exhibited a good potency to sodium valproate degradation. Active species of degradation including superoxide radicals, holes, and hydroxyl radicals were investigated using ammonium oxalate, benzoquinone, and 2-propanol to identify the mechanism of photodegradation action. The activity of benzoquinone in the photocatalytic process led to a reduction in the rate of analyte degradation, which indicates the prominent role of superoxide radicals compared to other species in the degradation process. The degradation rate of the analyte using the Fenton reagent was found to be around two times more than in the Fenton reagent-free process. The possible mechanism for the fluorescence sensor and photocatalytic degradation reaction was also discussed.

Application of response surface methodology for optimization of ionic liquid-based dispersive liquid-liquid microextraction of cadmium from water samples.

A new, rapid, and simple method for the determination of cadmium in water samples was developed using ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) coupled to flame atomic absorption spectrometry (FAAS). In the proposed approach, 2-(5-boromo-2-pyridylazo)-5-(diethyamino) phenol was used as a chelating agent and 1-hexyl-3-methylimidazolium bis(trifluoro methylsulfonyl)imide and acetone were selected as extraction and dispersive solvents, respectively. Sample pH, concentration of chelating agent, amount of ionic liquid (extraction solvent), disperser solvent volume, extraction time, salt effect, and centrifugation speed were selected as interested variables in IL-DLLME process. The significant variables affecting the extraction efficiency were determined using a Placket-Burman design. Thereafter, the significant variables were optimized using a Box-Behnken design and the quadratic model between the dependent and the independent variables was built. The optimum experimental conditions obtained from this statistical evaluation included: pH: 6.7; concentration of chelating agent: 1.1 10(-) (3) mol L(-1); and ionic liquid: 50.0 mg. Under the optimum conditions, the preconcentration factor obtained was 100. Calibration graph was linear in the range of 0.2-60 µg L(-1) with correlation coefficient of 0.9992. The limit of detection was 0.06 µg L(-) (1), which is lower than other reported approaches applied to the determination of cadmium using FAAS. The relative SD (n = 8) was 2.4%. The proposed method was successfully applied to the determination of trace amounts of cadmium in the real water samples with satisfactory results.

Silica gel-polyethylene glycol as a new adsorbent for solid phase extraction of cobalt and nickel and determination by flame atomic absorption spectrometry.

In this paper a novel solid phase extraction method to determine Co(II) and Ni(II) using silica gel-polyethylene glycol (Silica-PEG) as a new adsorbent is described. The method is based on the adsorption of cobalt and nickel ions in alkaline media on polyethylene glycol-silica gel in a mini-column, elution with nitric acid and determination by flame atomic absorption spectrometry. The adsorption conditions such as NaOH concentration, sample volume and amount of adsorbent were optimized in order to achieve highest sensitivity. The calibration graph was linear in the range of 0.5-200.0ngmL(-1) for Co(II) and 2.0-100.0ngmL(-1) for Ni(II) in the initial solution. The limit of detection based on 3S(b) was 0.37ngmL(-1) for Co(II) and 0.71ngmL(-1) for Ni(II). The relative standard deviations (R.S.D.) for ten replicate measurements of 40ngmL(-1) of Co(II), and Ni(II) were 3.24 and 3.13%, respectively. The method was applied to determine Co(II) and Ni(II) in black tea, rice flour, sesame seeds, tap water and river water samples.

Simultaneous spectrophotometric determination of iron and vanadium by H-point standard addition method and partial least squares regression in micellar medium.

Simultaneous determination of total iron and vanadium by H-point standard addition method (HPSAM) and partial least squares (PLS) is described. Gallic acid (GA) in a cationic micellar solution of CTAB was used for determination of iron and vanadium in different oxidation states at pH 5. The presence of a micellar system enables total iron and vanadium to be determined with improved sensitivities. The total relative standard error for applying the PLS method to 15 synthetic samples in the ranges 0.20-15.00 mug ml(-1) iron and 0.20-8.00 mug ml(-1) vanadium was 2.2%. The results of applying the H-point standard addition method showed that iron and vanadium can be determined simultaneously with the concentration ratios of iron to vanadium from 10:1 to 1:20 in the mixed sample. Both HPSAM and PLS methods showed suitable abilities to resolve accurately overlapped absorption spectra of the compounds. Both proposed methods were successfully applied to the determination of Fe and V in several synthetic alloy solutions.

Simultaneous determination of Fe(II) and Fe(III) by kinetic spectrophotometric H-point standard addition method.

The H-point standard addition method (HPSAM) for simultaneous determination of Fe(II) and Fe(III) is described. The method is based on the difference in the rate of complex formation of iron in two different oxidation states with Gallic acid (GA) at pH 5. Fe(II) and Fe(III) can be determined in the range of 0.02-4.50 mug ml(-1) and 0.05-5.00 mug ml(-1), respectively, with satisfactory accuracy and precision in the presence of other metal ions, which rapidly form complexes with GA under working conditions. The proposed method was successfully applied for simultaneous determination of Fe(II) and Fe(III) in several environmental and synthetic samples with different concentration ratios of Fe(II) and Fe(III).