In this work, the nickel-aluminum layered double hydroxide （Ni-Al LDH） with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbent for the selective separation and pre-concentration of...In this work, the nickel-aluminum layered double hydroxide （Ni-Al LDH） with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbent for the selective separation and pre-concentration of mefenamic acid prior to quantification by UV detection at λmax ？ 286 nm. Extraction procedure is based on the adsorption of mefenamate anions on the Ni-Al（NO3？ ） LDH and/or their exchange with LDH interlayer NO3？ anions. The effects of several parameters such as cations and interlayer anions type in LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent and co-existing ions on the extraction were investigated and optimized. Under the optimum conditions, the calibration graph was linear within the range of 2-1000 mg/L with a correlation coefficient of 0.9995. The limit of detection and relative standard deviation were 0.6 mg/L and 0.84% （30 mg/L, n ？ 6）, respectively. The presented method was successfully applied to determine of mefenamic acid in human serum and pharmaceutical wastewater samples.展开更多
In this research,an eco-friendly magnetic adsorbent based on Fe_(3)O_(4)/salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method.The crystalline and morphological characterization of...In this research,an eco-friendly magnetic adsorbent based on Fe_(3)O_(4)/salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method.The crystalline and morphological characterization of the prepared nanocomposite was performed by field emission scanning electron microscopy,X-ray diffraction,and Fourier transform infrared spectroscopy.The nanocomposite was employed as a magnetic solid-phase extraction agent for separation of Cd(II)ions from synthetic solutions.Some experimental factors affecting the extraction efficiency were investigated and optimized.Following elution with acetic acid(pH 3.5),the pre-concentrated analyte was quantified by flame atomic absorption spectrometry.In optimal conditions,a linear calibration graph was achieved in the concentration range of 0.2–30 ng·mL^(−1) with a determination coefficient(R^(2))of 0.9953.The detection limit,the enhancement factor,inter-and intra-day relative standard deviations(for six consecutive extractions at the concentration level of 10 ng·mL^(−1))were 0.04 ng·mL^(−1),100,2.38%and 1.52%,respectively.To evaluate the accuracy of the method,a certified reference material(NIST SRM 1643e)was analyzed,and there was a good agreement between the certified and the measured values.It was successfully utilized to determine cadmium in industrial wastewater samples and the attained relative recovery values were between 96.8%and 103.2%.展开更多
基金support from the Research Council of Azarbaijan Shahid Madani University (ASMU,Iran)
文摘In this work, the nickel-aluminum layered double hydroxide （Ni-Al LDH） with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbent for the selective separation and pre-concentration of mefenamic acid prior to quantification by UV detection at λmax ？ 286 nm. Extraction procedure is based on the adsorption of mefenamate anions on the Ni-Al（NO3？ ） LDH and/or their exchange with LDH interlayer NO3？ anions. The effects of several parameters such as cations and interlayer anions type in LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent and co-existing ions on the extraction were investigated and optimized. Under the optimum conditions, the calibration graph was linear within the range of 2-1000 mg/L with a correlation coefficient of 0.9995. The limit of detection and relative standard deviation were 0.6 mg/L and 0.84% （30 mg/L, n ？ 6）, respectively. The presented method was successfully applied to determine of mefenamic acid in human serum and pharmaceutical wastewater samples.
基金The financial support of the research council of Azarbaijan Shahid Madani University(Grant No.ASMU/98372-19)is acknowledged.
文摘In this research,an eco-friendly magnetic adsorbent based on Fe_(3)O_(4)/salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method.The crystalline and morphological characterization of the prepared nanocomposite was performed by field emission scanning electron microscopy,X-ray diffraction,and Fourier transform infrared spectroscopy.The nanocomposite was employed as a magnetic solid-phase extraction agent for separation of Cd(II)ions from synthetic solutions.Some experimental factors affecting the extraction efficiency were investigated and optimized.Following elution with acetic acid(pH 3.5),the pre-concentrated analyte was quantified by flame atomic absorption spectrometry.In optimal conditions,a linear calibration graph was achieved in the concentration range of 0.2–30 ng·mL^(−1) with a determination coefficient(R^(2))of 0.9953.The detection limit,the enhancement factor,inter-and intra-day relative standard deviations(for six consecutive extractions at the concentration level of 10 ng·mL^(−1))were 0.04 ng·mL^(−1),100,2.38%and 1.52%,respectively.To evaluate the accuracy of the method,a certified reference material(NIST SRM 1643e)was analyzed,and there was a good agreement between the certified and the measured values.It was successfully utilized to determine cadmium in industrial wastewater samples and the attained relative recovery values were between 96.8%and 103.2%.
