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1.
A nanocomposite composed of graphene oxide and magnetite (Fe3O4) was coated with the ionic liquid (IL) 1,3-didecyl-2-methylimidazolium chloride and used to capture and separate hemin from serum samples. The critical parameters affecting the extraction of analyte, such as pH, surfactant and adsorbent amounts, and desorption conditions were studied and optimized. Following magnetic separation and desorption with a 5:1 mixture of acetic acid and acetone, hemin (an iron porphyrin complex) was quantified by FAAS of iron. Under optimum conditions, the enrichment factor was 96. The calibration curve was linear in the 4.8 to 730 μg L?1 concentration range, the limit of detection was 3.0 μg L?1, and the relative standard deviations (RSDs) for single-sorbent repeatability and sorbent-to-sorbent reproducibility were less than 3.9 % and 10.2 % (n = 5), respectively. The adsorbent displayed adsorption capacity as high as 200 mg g?1, indicating IL-coated Fe3O4/GO to be a good sorbent for the adsorption of hemin. The method was validated by determining serum hemin in the presence of a large excess (480-fold) of Fe3+ without considerable interference. The results compare well to those obtained with a commercial hemin assay kit. The results show that this method can be successfully applied to the enrichment and determination of hemin in acid digested serum samples of breast cancer patients.
Graphical abstract Fe3O4/GO nanocomposites were coated with the ionic liquid 1,3-didecyl-2-methylimidazolium chloride and used as the sorbent for the separation and preconcentration of hemin from blood serum samples prior to determination using by flame AAS.
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2.
In the present study, the ?5-(4-dimethylaminobenzylidene)rhodanin-modified SBA-15? was applied as stable solid sorbent for the separation and preconcentration of trace amounts of cobalt ions in aqueous solution. SBA-15 was modified by ?5-(4-dimethylaminobenzylidene)rhodanin reagent. The sorption of Co2+ ions was done onto modified sorbent in the pH range of 6.8–7.9 and desorption occurred in 5.0 mL of 3.0 mol L?1 HNO3. The results exhibit a linear dynamic range from 0.01 to 6.0 mg L?1 for cobalt. Intra-day (repeatability) and inter-day (reproducibility) for 10 replicated determination of 0.06 mg L?1 of cobalt was ±1.82% and ?±1.97%?. Detection limit was 4.2 µg L?1 (3Sb, n = 5) and preconcentration factor was 80. The effects of the experimental parameters, including the sample pH, flow rates of sample and eluent solution, eluent type and interference ions were studied for the preconcentration of Co2+. The proposed method was applied for the determination of cobalt in standard samples, water samples and agricultural products.  相似文献   

3.
Nanocrystalline MnO2, synthesized by alcoholic hydrolysis of KMnO4, has been studied as a sorbent for removal of americium from low level liquid waste solutions. The synthesized MnO2 was found to have BET surface area of 230 m2 g?1. Am(III) was found to be sorbed by MnO2 quantitatively within 15 min at pH 5. The sorption was found to be more than 90 % at as low a pH as 1.2 and reached to near 100 % at all pH values above pH 3.0 There was no effect of ionic strength (0.01–1.0 M NaCl, CaCl2) on the sorption suggesting the sorption following inner sphere complexation mechanism at all the pH values. Adsorption isotherm studies were carried out using Eu(III) as a chemical analogue of Am(III). These studies showed the isotherm data to follow Langmuir adsorption isotherm.  相似文献   

4.
In this study, a new Cr(III)-imprinted polymer (Cr(III)-IIP) is prepared from CrCl3·6H2O, methacrylic acid functional monomer, ethyleneglycoldimethacrylate cross-linking agent, 2,2?-azobisisobutyronitrile radical initiator and 2,2-(azanediylbis (ethane-2,1-diyl))bis(isoindoline-1,3-dione) ligand. To obtain the maximum adsorption capacity, the optimum condition was studied through pH, type and concentration of eluent, IIP weight, sample volume as well as the adsorption and desorption times. The Cr(III) ion content was determined via flame atomic absorption spectrometer. In optimum conditions, the adsorption capacity of the IIP for Cr(III) was obtained to be 74.65 mg g?1, using 50 mg of IIP and the initial pH solution of 3.0. Both the adsorption and desorption times for quantitative analyses of Cr(III) ions were 15 and 5 min; respectively. After elution of the adsorbed ions by 3 mL of 4 mol L?1 HNO3 aqueous solution, the established IIP-based SPE procedure provides a reasonable pre-concentration factor of 100. The IIP-based pre-concentration method provides a low detection limit of 1.7 µg L?1 with good repeatability (RSD?=?3.22%). Reusability studies confirmed that synthesis IIP is reusable and recoverable up to six cycles. According to the selectivity experiments, it was concluded that the prepared sorbent possesses more affinity toward Cr(III) ions than other ions such as Al3+, Pb2+, Cu2+, Mn2+, Fe2+, Zn2+, and Ni2+ ions. To evaluate the potential applicability of the proposed separation method, the pre-concentration and determination of trace amounts of Cr(III) were performed successfully in food samples with complex matrices, a bestial sample (i.e. cow liver) and an herbal product (i.e., broccoli) as real samples.  相似文献   

5.
Adsorption behavior of uranyl and thorium ions from synthetic radioactive solutions onto functionalized silica as sorbent has been investigated. The effect of contact time, initial concentration of radioactive solutions, sorbent mass, pH value and temperature on the adsorption capacity of the sorbent was investigated. Negative values of Gibbs free energy of adsorption suggested the spontaneity of the adsorption process on both functionalized silica with –NH2 groups and with –SH groups. Positive values obtained for ΔH° indicates that the adsorption is an endothermic process. The adsorption isotherms were better fitted by Freundlich model and the adsorption kinetic was well described by the pseudo-second order equation. Desorption studies indicated that the most favorable desorptive reagents for UO2 2+ is HNO3 1 M and for Th4+ is EDTA 1 M solutions.  相似文献   

6.
Chemical sensors relying on graphene-based materials have been widely used for electrochemical determination of metal ions and have demonstrated excellent signal amplification. This study reports an electrochemically reduced graphene oxide (ERGO)/mercury film (HgF) nanocomposite-modified pencil graphite electrode (PGE) prepared through successive electrochemical reduction of graphene oxide (GO) sheets and an in situ plated HgF. The ERGO-PG-HgFE, in combination with dimethylglyoxime (DMG) and square-wave adsorptive cathodic stripping voltammetry (SW-AdCSV), was evaluated for the determination of Ni2+ in tap and natural river water samples. A single-step electrode pre-concentration approach was employed for the in situ Hg-film electroplating, metal-chelate complex formation, and non-electrolytic adsorption at –0.7 V. The current response due to nickel-dimethylglyoxime [Ni(II)-DMG2] complex reduction was studied as a function of experimental paratmeters including the accumulation potential, accumulation time, rotation speed, frequency and amplitude, and carefully optimized for the determination of Ni2+ at low concentration levels (μg?L?1) in pH 9.4 of 0.1 M NH3–NH4Cl buffer. The reduction peak currents were linear with the Ni2+ concentration between 2 and 16?μg?L?1. The limits of detection and quantitation were 0.120?±?0.002?µg?L?1 and 0.401?±?0.007?µg?L?1 respectively, for the determination of Ni2+ at an accumulation time of 120?s. The ERGO-PG-HgFE further demonstrated a highly selective stripping response toward Ni2+ determination compared to Co2+. The electrode was found to be sufficiently sensitive to determine metal ions in water samples at 0.1?µg?L?1, well below the World Health Organization standards.  相似文献   

7.
A selective, simple and fast dispersive micro solid phase extraction method using magnetic graphene oxide (GO) as an efficient sorbent has been developed for the extraction, separation and speciation analysis of chromium ions. The method is based on different adsorption behaviour of Cr(VI) and Cr(III) species onto magnetic GO in aqueous solutions which allowed the selective separation and extraction of Cr(VI) in the pH range of 2.0–3.0. The retained Cr(VI) ions by the sorbent were eluted using 0.5 mL of 0.5 mol L?1 nitric acid solution in methanol and determined by ?ame atomic absorption spectrometry. Total chromium content was determined after the oxidation of Cr(III) to Cr(VI) by potassium permanganate. All effective parameters on the performance of the extraction process were thoroughly investigated and optimised. Under the optimised conditions, the method exhibited a linear dynamic range of 0.5–50.0 µg L?1 with a detection limit of 0.1 µg L?1 and pre-concentration factor of 200. The relative standard deviations of 3.8% and 4.6% (n = 8) were obtained at 25.0 µg L?1 level of Cr(VI) for intra- and inter-day analysis, respectively. The method was successfully applied to the speciation and determination of Cr(VI) and Cr(III) in environmental water samples.  相似文献   

8.
In the present work, titanium dioxide nanowires (TNWs) were synthesised via hydrothermal method. Insertion of ZnFe2O4 nanoparticles to the surface of TNWs was done by sol gel combustion synthesis of the nanoparticles in the presence of the nanowires. The surface of prepared magnetic TNWs was modified by p-phenylendiamine and then it was used in preconcentration of Cu2+ ion prior to their determination by flame atomic absorption spectroscopy. The sorbent was characterised by Fourier transform infrared spectra, EDX, FE-SEM and VSM techniques. We investigated and optimised various parameters influencing the preconcentration efficiency, such as the media pH, adsorbent quantity, contact time, sample volume and elution conditions. Under optimum conditions, the analytical performance of the method was evaluated. The calibration curve was found to be linear from 10.0 to 150 μg L?1 (R2 = 0.996). Calculated limit of detection was 0.43 μg L?1 (n = 5). The estimated relative standard deviation was 2.50% (n = 5). Moreover, the maximum adsorption capacity of the sorbent was 51.5 mg g?1 and preconcentration factor was 125. Capability of developed method was proved by applying it for preconcentration of Cu2+ ion from food and water samples.  相似文献   

9.
A surface molecular imprinting technology was developed to adsorb Ce(III) ions that showed much higher adsorption affinity and selectivity for than for other metal ions. The batch adsorption process was studied with respect to effects of pH value, residence time, temperature, and initial concentration of Ce(III) ion. The maximum adsorption capacity is 43 mg g?1 at an initial Ce(III) concentration of 300 mg L?1 and at a sorbent dosage of 1.0 g L?1. A Langmuir isotherm fits the experimental data. The imprinted sorbent exhibits a much higher separation and selectivity for the target imprinted ion than the non-imprinted polymer. Cerium ion can be desorbed with 1M hydrochloric acid solution which is also proven by scanning electron microoscopy and X-ray diffraction experiments. The limit of detection is 37 ng mL?1. The sorbent has been applied to the determination of trace cerium in different environmental samples with satisfactory results.  相似文献   

10.
In the present work, synthesis of polymer wrapped flower-like MgAl layered double hydroxide was done through condensation of 1,4 phenylenediamine and resorcinol by p-formaldehyde. The nanocomposite was characterised with X-ray diffraction analysis, fourier transform infrared spectroscopy, thermogravimetric analysis and field emission scanning electron microscopy techniques and employed for effective adsorption of Cr(VI) from aqueous solution prior to flame atomic absorption spectrometer determination. Optimum level of effective parameters (pH, reaction time and adsorbent dosage) and their interaction was determined by response surface methodology. To investigate applicability of method for trace heavy metal adsorption, the method was employed for preconcentration of Cr(VI) in water samples. At the optimum conditions, pH = 4.5, shaking time of 15 min and adsorbent dosage of 20 mg, analytical performance of the method was evaluated and results showed that calibration curve is linear in the concentration range of 2–100 μg L?1. Moreover, limit of detection was 0.22 µg L?1 and relative standard deviation of six replicate experiments at initial concentration of 0.1 mg L?1 was 3.3%. Isotherm study showed that Freundlich model can better describe adsorption behaviour as well as the sorbent showed the adsorption capacity of 62.5 mg g?1. Moreover, thermodynamic study revealed that chromate adsorption was spontaneous and followed the endothermic path. Regeneration of sorbent was performed using 1.0 mol L?1 of NaOH solution. The sorbent was employed for Cr(VI) determination from food additives and seawater samples.  相似文献   

11.
Attapulgite modified with 2-hydroxy-1-naphthaldehyde was prepared and applied to the separation, preconcentration and determination of Cu(II) in aqueous solutions by inductively coupled plasma optical emission spectrometry. Experimental conditions for effective adsorption of trace levels of Cu(II) were optimized using batch and column procedures. The optimum pH value for the separation of Cu(II) on the newly sorbent was 4.0 and complete elution of Cu(II) from the sorbent surface was carried out using 2 mL of 0.01 mol L?1 HCl. The adsorption capacity for Cu(II) was 25.13 mg g?1. The detection limits of the method defined by IUPAC were found to be 0.24 μg L?1 with enrichment factor of 150. The method has been applied to the determination of Cu(II) in certified reference materials and natural water samples with satisfactory results.  相似文献   

12.
A novel Fe3O4/graphene/polypyrrole nanocomposite has been successfully synthesised via a simple chemical method and applied as a new magnetic solid-phase extraction (MSPE) sorbent for the separation and pre-concentration of trace amounts of Pt (IV) in environmental samples followed by flame atomic absorption spectrometric (FAAS) detection. The nanocomposite has been characterised by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infrared (FTIR) spectroscopy. Seven important parameters, affecting the extraction efficiency of Pt (IV), including pH, adsorption time, desorption solvent type and concentration, desorption time, elution volume and sample volume, were investigated. Under the optimised conditions, the calibration graph was linear in the range of 50–1500 μg L?1 (R = 0.993). The detection limit and pre-concentration factor (PF) for Pt (IV) were found to be 16 μg L?1 and 112.5, respectively. Under the optimised solid-phase extraction (SPE) conditions, the adsorption isotherm and the adsorption capacity of the nanocomposite for Pt (IV) were studied. Pt (IV) adsorption equilibrium data were fitted well to the Langmuir isotherm and the maximum adsorption capacity of the magnetic sorbent was calculated from the Langmuir isotherm model as 416.7 mg g?1. The precision of the method was studied as intraday and interday variations. A relative standard deviation percentage (RSD%) value less than 3.0 indicates that the method is precise. Also, the accuracy of the method was tested by the analysis of the standard reference material (NIST SRM 2556) and by recovery measurements on spiked real samples. It was also shown that the optimised method was suitable for the analysis of trace amounts of Pt (IV) in roadside soil, tap water and wastewater samples.  相似文献   

13.
In this research, nickel ferrite (NiFe2O4) magnetic nanoparticles were synthesised by a simple method and applied as sorbent for magnetic solid-phase extraction of trace amounts of Au(III) from water samples. Detection in this technique was performed by flame atomic absorption spectrometry. The effects of sample pH, amount of sorbent, extraction time, desorption solvent and its volume on the extraction process were optimised. The effects of interfering ions on the recovery of the analyte were also evaluated in model solutions. The best results were obtained at pH 6.5 with 5 mL of eluent solution (0.1 mol L?1 sodium thiosulphate) and an extraction time of 30 min. Under optimal conditions, the sorption capacity was 34.6 mg g?1. Also, enhancement factor (for 100 mL of sample solution) was found to be 19.3. The calibration graph was linear in the range of 4.4–800.0 µg L?1 gold concentration and the limit of detection was 1.32 µg L?1. The relative standard deviation of the method (for n = 8) was 1.57%. The method was successfully applied to the extraction of Au(III) from water samples.  相似文献   

14.
We report on the synthesis of Fe3O4-functionalized metal-organic framework (m-MOF) composite from Zn(II) and 2-aminoterephthalic acid by a hydrothermal reaction. The magnetic composite is iso-reticular and was characterized by FTIR, X-ray diffraction, SEM, magnetization, and TGA. The m-MOF was then applied as a sorbent for the solid-phase extraction of trace levels of copper ions with subsequent quantification by electrothermal AAS. The amount of sorbent applied, the pH of the sample solution, extraction time, eluent concentration and volume, and desorption time were optimized. Under the optimum conditions, the enrichment factor is 50, and the sorption capacity of the material is 2.4 mg g?1. The calibration plot is linear over the 0.1 to 10 μg L?1 Cu(II) concentration range, the relative standard deviation is 0.4 % at a level of 0.1 μg L?1 (for n?=?10), and the detection limit is as low as 73 ng L?1. We consider this magnetic MOF composite to be a promising and highly efficient material for the preconcentration of metal ions.
Figure
Magnetic metal-organic frameworks was synthesized and used as a new sorbent for lead adsorption with detection by electrothermal atomic absorption spectrometry.  相似文献   

15.
Porous microspheres of magnesium oxide were synthesized by calcination of precursor obtained via hydrothermal method. A sample of microsphere was characterized by transmission electron microscopy, scanning electron microscopy–energy dispersion spectroscopy, X-ray diffraction, thermogravimetric analysis, N2 adsorption–desorption isotherms, and BET surface area. The average pore size and surface area of the microsphere were found to be 9.0 nm and 83.1 m2 g?1, respectively. The performance of sorbent was investigated in a continuous adsorption system. Iodine adsorption on sorbent was studied by varying temperature of adsorption column, sorbent calcination temperature and initial concentration of iodine. The capacity of sorbent increased by ~25 % when calcination temperature was raised from 350 to 500 °C. The maximum iodine adsorption capacity of sorbent was found to be 196 mg g?1 using Langmuir isotherm. These results indicate the microspherical form of MgO to be effective sorbent to capture iodine vapor from off-gas stream.  相似文献   

16.
A magnetic molecularly imprinted polymer (MMIP) was fabricated and used as the sorbent for the MMIP-dispersive solid-phase microextraction of fenitrothion prior its determination by high-performance liquid chromatography equipped with an ultraviolet detector. The MMIP was prepared using functionalized Fe3O4 nanoparticles as the magnetic supporter. Methacrylic acid, ethylene glycol dimethacrylate and fenitrothion were used as the functional monomer, the cross-linker and the template, respectively. The properties of the resultant MMIP were evaluated using X-ray diffraction spectroscopy, Fourier transform infrared spectroscopy and scanning electron microscopy. The sorbent exhibited high selectivity and affinity toward fenitrothion compared to other organophosphate pesticides with the maximum adsorption capacity of 31.5 mg g?1. The effective variables on the extraction were optimized by univariable and MultiSimplex methods. The calibration curve exhibited linearity over the concentration range of 0.3–50.0 μg L?1 with the limit of detection of 0.1 μg L?1. The relative standard deviations at 10.0 μg L?1 level of FNT (n = 5) for intra- and inter-day assays were 1.6 and 3.1%, respectively. The proposed method was successfully used for the determination of trace amounts of FNT in food and water samples.  相似文献   

17.
A composite of aminosilane-grafted TiO2 (TA) and graphene oxide (GO) was prepared via a hydrothermal process. The TiO2/graphene oxide-based (TA/GO) anode was investigated in an ionic liquid electrolyte (0.7 M lithium bis(trifluoromethanesulfonyl)imide (LiNTf2)) in ionic liquid (N-methyl-N-propylpyrrolidinium bis(trifluoromethanesulfonyl)imide (MPPyrNTf2)) at room temperature and in sulfolane (1 M lithium hexafluorophosphate (LiPF6) in tetramethylene sulfolane (TMS)). Scanning and transmission electron microscopy (SEM and TEM) observations of the anode materials suggested that the electrochemical intercalation/deintercalation process in the ionic liquid electrolyte with vinylene carbonate (VC) leads to small changes on the surface of TA/GO particles. The addition of VC to the electrolyte (0.7 M LiNTf2 in MPPyrNTf2 + 10 wt.% VC) considerably increases the anode capacity. Electrodes were tested at different current regimes in the range 5–50 mA g?1. The capacity of the anode, working at a low current regime of 5 mA g?1, was ca. 245 mA g?1, while a current of 50 mA g?1 resulted in a capacity of 170 mA g?1. The decrease in anode capacity with increasing current rate was interpreted as the result of kinetic limits of electrode operation. A much lower capacity was observed for the system TA/GO│1 M LiPF6 in TMS + 10 wt.% VC│Li.  相似文献   

18.
In this study, the use of the organic fraction of municipal solid waste as an abundant and low-cost raw material for producing activated carbon was investigated. For this purpose, ZnCl2 was used as a chemical activation agent and the carbonization process took place at 800 °C in N2 atmosphere. Seven sorbents were prepared by chemical activation (pyrolysis under N2 atmosphere at temperature of 800 °C after impregnation with ZnCl2) with different ratios of ZnCl2. The optimum ratio of organic fraction of municipal solid waste to ZnCl2 was inspected via methylene blue number and iodine number (ASTM Designation: D4607–94). The results showed that the adsorbent with 60 % ZnCl2/raw material was the most appropriate one with a satisfactory adsorption capacity, 112.4 mg g?1 for methylene blue and 134.0 mg g?1 for iodine. In addition, the structural analysis of this sorbent was performed using FT-IR, BET surface area, SEM–EDX and thermal analysis. Application of this sorbent to remove Cr(VI) from wastewater was studied to find an adsorption capacity of 66.7 mg g?1. The experimental adsorption equilibrium data were fitted to Langmuir adsorption model with an acceptable adsorption capacity of 66.7 mg g?1.  相似文献   

19.
A novel graphene oxide/bentonite composite (GO/bentonite) was synthesized and then characterized through powder X-ray diffraction, fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, and energy dispersive spectroscopy. Adsorption achieved equilibrium within 10 min. Moreover, U(VI) adsorption on GO/bentonite was highly dependent on solution pH and independent of ionic strength. These characteristics suggested that inner-sphere surface complexes of U(VI) formed on GO/bentonite. The adsorption of U(VI) from aqueous solution on GO/bentonite was fitted to the pseudo-second-order and Freundlich isotherm models. The maximum sorption capacity of GO/bentonite was 234.19 mg g?1 under neutral pH at 303 K. GO/bentonite is a potentially powerful adsorbent for the efficient removal of U(VI) from aqueous solutions.  相似文献   

20.
Silica gel surface was chemically functionalized by reaction the silanol from the silica surface with 3-chloropropyltrimethoxysilane followed by reaction with Sulfasalazine. This new sorbent has been used for the preconcentration of low levels of U(VI) ions from an aqueous phase. Parameters involved in extraction efficiency such as pH, weight of the sorbent, volume of sample and eluent were optimized in batch and column methods prior to determination by spectrophotometry using arsenazo(III) reagent. The results showed that U(VI) ions can be sorbed at pH range of 5.0–6.0 in a minicolumn and quantitative recovery of U(VI) (>98.0?±?1.6%) was achieved by stripping with 2.5 mL of 0.1 mol L?1 HCl. The sorption capacity of the functionalized silica gel was 1.15 mmol g?1 of U(VI). A linear calibration graph was obtained over the concentration range of 0.02–27.0 μg mL?1 with a limit of detection of 1 μg L?1 in treatment with 1000 mL of the U(VI) solution in which the preconcentration factor was as high as 400. The method was employed to the preconcentration of U(VI) ions from spiked ground water and synthetic sea water samples.  相似文献   

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