A new liquid-liquid microextraction method based on the solidification of floating organic drops coupled with gas chromatography was developed for the determination of trace benzene, toluene and xylene（BTX） in water...A new liquid-liquid microextraction method based on the solidification of floating organic drops coupled with gas chromatography was developed for the determination of trace benzene, toluene and xylene（BTX） in water samples. In the microextraction procedure, a microdrop of n-decanol was delivered to the surface of the analytes’ solution, and stirred for a desired time. Following the absolute extraction, the sample vial was cooled in an ice bath for 10 min. The solidified n-decanol was then transferred into a plastic tube and melted naturally; and 1 μL of it was injected into gas chromatography for analysis. Factors relevant to the extraction efficiency were studied and optimized. The optimal experimental conditions were： 15 μL of n-decanol as extractive solvent, 30 mL of solution containing analytes, no salt, the stirring rate 400 r/min, the extraction temperature 30 °C, and the extraction time 30 min. Under those optimized conditions, the detection limit（LOD） of analytes was in a range of 0.05―0.10 ng/mL by the developed method. A good linearity（r0.99） in a calibration range of 0.01―100 μg/mL was obtained. The recoveries of the real samples at different spiked levels of BTX were in the range from 92.2% to 103.4%.展开更多
In the present work, a ultrasound-assisted emulsification dispersive liquid-liquid microextraction based on solidification of floating organic droplet method has been developed as a sample preparation method prior to ...In the present work, a ultrasound-assisted emulsification dispersive liquid-liquid microextraction based on solidification of floating organic droplet method has been developed as a sample preparation method prior to flame atomic absorption spectrometry determination of trace amounts of gold in the standard, wastewater and river water samples. In the proposed method, 1-dodecanol and 5-(4-dimethylamino-benzylidene) were used as extraction solvent and chelating agent, respectively. Several factors that may be affected on the ex-traction process, such as type and volume of the extraction solvent, ionic strength, pH of the aqueous solu-tion, extraction temperature and extraction time were studied and optimized. Under the best experimental conditions, the calibration curve exhibited linearity over the range of 8.0 ng●mL-1- 3.0 μg●mL-1 with a correlation coefficient of 0.9978 and detection limit based on three times the standard deviation of the blank signal was 1.5 ng●mL-1. Eight replicate determinations of 0.2 and 1.0 μg●mL-1 of gold gave a mean absorbance of 0.051 and 0.253 with relative standard deviations of ±2.3% and ±1.5%, respectively. Finally, the developed method was successfully applied to the extraction and determination of gold ions in a silica ore, wastewater, river water and standard samples and satisfactory results were obtained.展开更多
A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floatin...A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop（DLLME-SFO） followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient（r） of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.展开更多
A simple and efficient liquid-phase microextraction(LPME)technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction(USAE-SFODME)combined with flame atomic absorpt...A simple and efficient liquid-phase microextraction(LPME)technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction(USAE-SFODME)combined with flame atomic absorption spectrometry,for the extraction and determination of trace copper in water samples.1-(2-Pyridylazo)-2-naphthol(PAN)was used as chelating agent.Microextraction efficiency factors(including extraction solvent type,extraction volume,time,temperature,and pH),the amount of the chelating agent,and salt effect were investigated and optimized.Under the optimum extraction conditions,figures of merit of the proposed method were evaluated.The calibration graph was linear in the range of 20–600 mg·L^(–1)with a detection limit of 0.76 mg·L^(–1).The relative standard deviation(R.S.D)for ten replicate measurements of 20 and 400 mg·L^(–1)of copper was 3.83%and 2.65%,respectively.Finally,the proposed method was applied to tap water,river water,and sea water,and accuracy was assessed through the analysis of certified reference water or recovery experiments.展开更多
基金Supported by the National Natural Science Foundation of China(No.21105088)the Program for Science and Technology Projects of the Education Department of Fujian Province,China(No.JA10211)
文摘A new liquid-liquid microextraction method based on the solidification of floating organic drops coupled with gas chromatography was developed for the determination of trace benzene, toluene and xylene（BTX） in water samples. In the microextraction procedure, a microdrop of n-decanol was delivered to the surface of the analytes’ solution, and stirred for a desired time. Following the absolute extraction, the sample vial was cooled in an ice bath for 10 min. The solidified n-decanol was then transferred into a plastic tube and melted naturally; and 1 μL of it was injected into gas chromatography for analysis. Factors relevant to the extraction efficiency were studied and optimized. The optimal experimental conditions were： 15 μL of n-decanol as extractive solvent, 30 mL of solution containing analytes, no salt, the stirring rate 400 r/min, the extraction temperature 30 °C, and the extraction time 30 min. Under those optimized conditions, the detection limit（LOD） of analytes was in a range of 0.05―0.10 ng/mL by the developed method. A good linearity（r0.99） in a calibration range of 0.01―100 μg/mL was obtained. The recoveries of the real samples at different spiked levels of BTX were in the range from 92.2% to 103.4%.
文摘In the present work, a ultrasound-assisted emulsification dispersive liquid-liquid microextraction based on solidification of floating organic droplet method has been developed as a sample preparation method prior to flame atomic absorption spectrometry determination of trace amounts of gold in the standard, wastewater and river water samples. In the proposed method, 1-dodecanol and 5-(4-dimethylamino-benzylidene) were used as extraction solvent and chelating agent, respectively. Several factors that may be affected on the ex-traction process, such as type and volume of the extraction solvent, ionic strength, pH of the aqueous solu-tion, extraction temperature and extraction time were studied and optimized. Under the best experimental conditions, the calibration curve exhibited linearity over the range of 8.0 ng●mL-1- 3.0 μg●mL-1 with a correlation coefficient of 0.9978 and detection limit based on three times the standard deviation of the blank signal was 1.5 ng●mL-1. Eight replicate determinations of 0.2 and 1.0 μg●mL-1 of gold gave a mean absorbance of 0.051 and 0.253 with relative standard deviations of ±2.3% and ±1.5%, respectively. Finally, the developed method was successfully applied to the extraction and determination of gold ions in a silica ore, wastewater, river water and standard samples and satisfactory results were obtained.
基金supported by the Natural Science Foundation of Hebei(No.B2010000657)
文摘A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop（DLLME-SFO） followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient（r） of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.
文摘A simple and efficient liquid-phase microextraction(LPME)technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction(USAE-SFODME)combined with flame atomic absorption spectrometry,for the extraction and determination of trace copper in water samples.1-(2-Pyridylazo)-2-naphthol(PAN)was used as chelating agent.Microextraction efficiency factors(including extraction solvent type,extraction volume,time,temperature,and pH),the amount of the chelating agent,and salt effect were investigated and optimized.Under the optimum extraction conditions,figures of merit of the proposed method were evaluated.The calibration graph was linear in the range of 20–600 mg·L^(–1)with a detection limit of 0.76 mg·L^(–1).The relative standard deviation(R.S.D)for ten replicate measurements of 20 and 400 mg·L^(–1)of copper was 3.83%and 2.65%,respectively.Finally,the proposed method was applied to tap water,river water,and sea water,and accuracy was assessed through the analysis of certified reference water or recovery experiments.
