A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe（II）-ferrozine complex was reacted with cetyltrimethylammonium bromide （CTAB...A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe（II）-ferrozine complex was reacted with cetyltrimethylammonium bromide （CTAB） to form a Fe（II）-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 ~tg/L. The detection limit of this method reached 0.19 ktg/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation （n = 7） was 1.9% for samples containing 10 ~g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student＇s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.展开更多
A simple and sensitive high performance liquid chromatography-chemical vapour generation-atom fluorescent spectrometry （HPLC-CVG-AFS） method was developed and validated for simultaneous determination mercury species...A simple and sensitive high performance liquid chromatography-chemical vapour generation-atom fluorescent spectrometry （HPLC-CVG-AFS） method was developed and validated for simultaneous determination mercury species in Su-He-Xiang-Wan （SHXW） and in tissues of rats, respectively. The species of mercury were separated by a Venusil MP-C 18 （5μm, 150 mm×4.6 ram） column with the optimized mobile phase containing 5% （w/v） acetonitrile, 0.01 mol/L L-cysteine and 0.06 moL/L ammonium acetate. The tissues of rats were freeze-dried after giving the medicine for 10 d, and then added into the solution containing 10% （w/v） HC1, 1% （w/v） sulfocarbamide and 0.15% （w/v） KC1 for increasing extraction rate. The resolutions of Hg2＋, MeHg and EtHg were 1.5 and 2.9, respectively. The detection limits of Hg2＋, MeHg and EtHg were 2.0, 1.0 and 0.9 ng/mL, respectively. The relative standard deviation （RSD） of inter- and intra-day precisions ranged from 1.56% to 2.86%. The recovery rates of three different adding level were 87%-101% （n=6）, and the RSDs were smaller than 8.2%. The results show that no MeHg and EtHg were detected in rat tissues. Only soluble mercury （Hg2＋） was determined for the mercury species of SHXW in rat tissues.展开更多
[Objective]The aim was to find a way to measure the cholesterol content in deserted oil.[Method]Dual-wavelength spectrophotometry method was used for the determination of cholesterol in edible oil.630 nm and 720 nm we...[Objective]The aim was to find a way to measure the cholesterol content in deserted oil.[Method]Dual-wavelength spectrophotometry method was used for the determination of cholesterol in edible oil.630 nm and 720 nm were set as target band and reference band in this method,respectively.The result was compared to liquid chromatography method.[Result]The relative standard deviation(RSD)was at 1.26% and recovery was between 101.9% and 110.7%.Linear range was 8.0-40.0 μg/ml.The tested result was close to the result of liquid chromatography.[Conclusion]It was proved that this method was easy,fast and accurate.The disturbance of sitosterol was eliminated without isolation.It can be used for fast identification of the authenticity of waste fat.展开更多
In order to measure the flow velocity of carbon particle suspension perpendicular to the receiving axis of ultrasound transducer, the standard deviation of photoacoustic Doppler frequency spectrum is used to estimate ...In order to measure the flow velocity of carbon particle suspension perpendicular to the receiving axis of ultrasound transducer, the standard deviation of photoacoustic Doppler frequency spectrum is used to estimate the bandwidth broadening, and the spectrum standard deviation is calculated by an auto-correlation method. A 532 nm pulsed laser with the repetition rate of 20 Hz is used as a pumping source to generate photoacoustic signal. The photoacoustic signals are detected using a focused PZT ultrasound transducer with the central frequency of 10 MHz. The suspension of carbon particles is driven by a syringe pump. The complex photoacoustic signal is calculated by Hilbert transformation from time domain signal before auto-correlation. The standard deviation of the Doppler bandwidth broadening is calculated by averaging the auto-correlation results of several individual A scans. The feasibility of the proposed method is demonstrated by measuring the spectrum standard deviation of the transversal carbon particle flow from 5.0 mm/s to 8.4 mrn/s. The experimental results show that the auto-correlation result is approximately linearly distributed within the measuring range.展开更多
An analytical method for quantifying biomarker compounds of the sterane and the hopane existing in saturated hydrocarbons has been established by using comprehensive two-dimensional gas chromatography-flame ionization...An analytical method for quantifying biomarker compounds of the sterane and the hopane existing in saturated hydrocarbons has been established by using comprehensive two-dimensional gas chromatography-flame ionization detector(GC×GC-FID) with optimized operating parameters. The new method achieves the quantification by using a GC×GC-FID system which is able to completely separate steranes from hopanes. The data obtained by the new method are of good repeatability and reliability. Compared with the original data, the relative standard deviations(RSDs) of 12 reference compounds are less than 5%. The RSDs of the quantitative results of the biomarkers based on seven separate analyses are also less than 5%. Compared with the traditional method of gas chromatography-mass spectrometry(GC-MS), the new method has a number of advantages, such as common internal standards(ISs), high resolution, no co-eluting peak, and no interference caused by diagnostic ion peaks. The new method provides petroleum geologists with an effective and scientific means in future researches.展开更多
基金Supported by State Key Laboratory of Marine Environmental Science(MEL)Funds(No.MELRI1001)
文摘A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe（II）-ferrozine complex was reacted with cetyltrimethylammonium bromide （CTAB） to form a Fe（II）-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 ~tg/L. The detection limit of this method reached 0.19 ktg/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation （n = 7） was 1.9% for samples containing 10 ~g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student＇s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.
基金Projects(20875104, 21075138) supported by the National Natural Science Foundation of China
文摘A simple and sensitive high performance liquid chromatography-chemical vapour generation-atom fluorescent spectrometry （HPLC-CVG-AFS） method was developed and validated for simultaneous determination mercury species in Su-He-Xiang-Wan （SHXW） and in tissues of rats, respectively. The species of mercury were separated by a Venusil MP-C 18 （5μm, 150 mm×4.6 ram） column with the optimized mobile phase containing 5% （w/v） acetonitrile, 0.01 mol/L L-cysteine and 0.06 moL/L ammonium acetate. The tissues of rats were freeze-dried after giving the medicine for 10 d, and then added into the solution containing 10% （w/v） HC1, 1% （w/v） sulfocarbamide and 0.15% （w/v） KC1 for increasing extraction rate. The resolutions of Hg2＋, MeHg and EtHg were 1.5 and 2.9, respectively. The detection limits of Hg2＋, MeHg and EtHg were 2.0, 1.0 and 0.9 ng/mL, respectively. The relative standard deviation （RSD） of inter- and intra-day precisions ranged from 1.56% to 2.86%. The recovery rates of three different adding level were 87%-101% （n=6）, and the RSDs were smaller than 8.2%. The results show that no MeHg and EtHg were detected in rat tissues. Only soluble mercury （Hg2＋） was determined for the mercury species of SHXW in rat tissues.
基金Supported by National Quality Inspection Bureau(KJ092102,2009QK146)
文摘[Objective]The aim was to find a way to measure the cholesterol content in deserted oil.[Method]Dual-wavelength spectrophotometry method was used for the determination of cholesterol in edible oil.630 nm and 720 nm were set as target band and reference band in this method,respectively.The result was compared to liquid chromatography method.[Result]The relative standard deviation(RSD)was at 1.26% and recovery was between 101.9% and 110.7%.Linear range was 8.0-40.0 μg/ml.The tested result was close to the result of liquid chromatography.[Conclusion]It was proved that this method was easy,fast and accurate.The disturbance of sitosterol was eliminated without isolation.It can be used for fast identification of the authenticity of waste fat.
基金supported by the Joint Funds of the National Natural Science Foundation of China(No.U1204612)the Natural Science Foundation of He’nan Educational Committee(No.13A416180)
文摘In order to measure the flow velocity of carbon particle suspension perpendicular to the receiving axis of ultrasound transducer, the standard deviation of photoacoustic Doppler frequency spectrum is used to estimate the bandwidth broadening, and the spectrum standard deviation is calculated by an auto-correlation method. A 532 nm pulsed laser with the repetition rate of 20 Hz is used as a pumping source to generate photoacoustic signal. The photoacoustic signals are detected using a focused PZT ultrasound transducer with the central frequency of 10 MHz. The suspension of carbon particles is driven by a syringe pump. The complex photoacoustic signal is calculated by Hilbert transformation from time domain signal before auto-correlation. The standard deviation of the Doppler bandwidth broadening is calculated by averaging the auto-correlation results of several individual A scans. The feasibility of the proposed method is demonstrated by measuring the spectrum standard deviation of the transversal carbon particle flow from 5.0 mm/s to 8.4 mrn/s. The experimental results show that the auto-correlation result is approximately linearly distributed within the measuring range.
文摘An analytical method for quantifying biomarker compounds of the sterane and the hopane existing in saturated hydrocarbons has been established by using comprehensive two-dimensional gas chromatography-flame ionization detector(GC×GC-FID) with optimized operating parameters. The new method achieves the quantification by using a GC×GC-FID system which is able to completely separate steranes from hopanes. The data obtained by the new method are of good repeatability and reliability. Compared with the original data, the relative standard deviations(RSDs) of 12 reference compounds are less than 5%. The RSDs of the quantitative results of the biomarkers based on seven separate analyses are also less than 5%. Compared with the traditional method of gas chromatography-mass spectrometry(GC-MS), the new method has a number of advantages, such as common internal standards(ISs), high resolution, no co-eluting peak, and no interference caused by diagnostic ion peaks. The new method provides petroleum geologists with an effective and scientific means in future researches.
