Trace analysis of volatile organic compounds(VOCs) during wildfires is imperative for environmental and health risk assessment. The use of gas sampling devices mounted on unmanned aerial vehicles(UAVs) to chemically s...Trace analysis of volatile organic compounds(VOCs) during wildfires is imperative for environmental and health risk assessment. The use of gas sampling devices mounted on unmanned aerial vehicles(UAVs) to chemically sample air during wildfires is of great interest because these devices move freely about their environment, allowing for more representative air samples and the ability to sample areas dangerous or unreachable by humans. This work presents chemical data from air samples obtained in Davis, CA during the most destructive wildfire in California's history-the 2018 Camp Fire – as well as the deployment of our sampling device during a controlled experimental fire while fixed to a UAV. The sampling mechanism was an in-house manufactured micro-gas preconcentrator(μPC) embedded onto a compact battery-operated sampler that was returned to the laboratory for chemical analysis. Compounds commonly observed in wildfires were detected during the Camp Fire using gas chromatography mass spectrometry(GC–MS), including BTEX(benzene, toluene, ethylbenzene, m + p-xylene, and o-xylene), benzaldehyde, 1,4-dichlorobenzene, naphthalene, 1,2,3-trimethylbenzene and 1-ethyl-3-methylbenzene. Concentrations of BTEX were calculated and we observed that benzene and toluene were highest with average concentrations of 4.7 and 15.1 μg/m^(3), respectively. Numerous fire-related compounds including BTEX and aldehydes such as octanal and nonanal were detected upon experimental fire ignition, even at a much smaller sampling time compared to samples taken during the Camp Fire. Analysis of the air samples taken both stationary during the Camp Fire and mobile during an experimental fire show the successful operation of our sampler in a fire environment.展开更多
A rapid and simple preconcentration step applying packed-fiber solid-phase extraction columns has been investigated to vitamin B12. The extraction performance of the new method was investigated preliminarily on vitami...A rapid and simple preconcentration step applying packed-fiber solid-phase extraction columns has been investigated to vitamin B12. The extraction performance of the new method was investigated preliminarily on vitamin functional drink. The analysis used a reversed-phase C18 column, with a photo-diode array detector at 220 nm. The samples were preconcentrated with packed-fiber solid-phase extraction columns. Good linearity was observed in vitamin functional drink. The repeatability of extraction performance, expressed as relative standard deviations, was from 3.5% to 4.3%. The limit of detection （LOD） is 5 ng mL^-1 （S/N = 3）. Finally, the method had been applied for the determination of vitamin B12 in vitamin functional drink.展开更多
The unstable state of nitrite results in its very low concentration in seawater, which is below the limit of detection （LOD） of conventional techniques of analysis. Some sensitivity-enhanced methods have been propos...The unstable state of nitrite results in its very low concentration in seawater, which is below the limit of detection （LOD） of conventional techniques of analysis. Some sensitivity-enhanced methods have been proposed for the determination of nitrite at nanomolar level to illustrate the role of nitrite in the marine nitrogen cycle. However, most of previous reports are not widely accepted, because of their complexity and cost equipment or intensive labor requirement. In this study, a simple automatic system for the determination of nanomolar level nitrite using on-line preconcentration with spectrophotometric detection was described..An Oasis HLB cartridge was adopted to quantitatively enrich the pink-colored azo compound, formed from nitrite via Griess reaction. The cartridge was rinsed with water and ethanol （volume fraction is 55%, the same below）, in turn, then eluted by an eluent containing 50% ethanol and 0.25 M（mol/dm^3） H2SO4, and determined at 543 nm with a 2 cm path-length flow cell. Under the optimized experimental conditions, the calibration curve showed a good linearity in the range of 1.4 85.7 aM, and the LOD （3a） was estimated to be 0.5 nM. The relative standard deviations of 7 measurements were 4.0% and 1.0% for the samples spiked at 7.1 and 28.6 nM, respectively. The recoveries for the different natural water samples were between 92.2%-108.4%. Each HLB cartridge could be reused for at least 50 times. As compared with other SPE methods, the advantages of this method included the free of interference from salinity variation and less sample consuming. The results of the application of the proposed method to natural water showed good agreement with liquid waveguide capillary cell detection method.展开更多
Nano-TiO2 was employed for the separation and preconcentration of thallium.It was found that the adsorption ratio of thallium ions was more than 98% at pH 4.5 and the desorption ratio reached 99% under microwave irrad...Nano-TiO2 was employed for the separation and preconcentration of thallium.It was found that the adsorption ratio of thallium ions was more than 98% at pH 4.5 and the desorption ratio reached 99% under microwave irradiation for 3 min at 350 W.The adsorption equilibrium was well described by the Langmuir isotherm model with a maximum adsorption capacity of 4.09 mg/g[（20±0.1） °C].The nano-TiO2 was successfully applied to the determination of element thallium in the certified reference material polymetallic nodule and water samples.展开更多
This article focuses on iodine determination by microwave plasma torch atomic emission spectrometry （MPT-AES） coupled with online preconcentration vapor generation method. A new desolvation device, multistrand Nafio...This article focuses on iodine determination by microwave plasma torch atomic emission spectrometry （MPT-AES） coupled with online preconcentration vapor generation method. A new desolvation device, multistrand Nafion dryer, was used as the substitute for condenser desolvation system. Some experimental conditions, such as preconcentration time, acidity of sample solution, rinsing solution acidity and dynamic linear range were investigated and optimized. The new desolvation system eliminates the problem of decreasing emission intensity of I（I） 206.238 nm line with the increase of working time on a conventional condenser desolvation system, thus greatly improving the reproducibility.展开更多
Molybdenum（ Ⅵ ） is a biologically essential trace element and its role in an extremely wide variety of systems has been reported. Most common methods often fail to determine trace Mo （ Ⅵ ） in the analysis of mol...Molybdenum（ Ⅵ ） is a biologically essential trace element and its role in an extremely wide variety of systems has been reported. Most common methods often fail to determine trace Mo （ Ⅵ ） in the analysis of molybdenum-containing samples, due to limitations such as inadequate detection limits and matrix interference, which make the direct determinations impossible. To solve this problem, various approaches are employed to concentrate and separate Mo（ Ⅵ ） to detectable levels. Concentration and separation methods play a main role in the analysis of trace Mo（Ⅵ）. Therefore, many separation and preconcentration procedures have been developed for the determination of Mo （ Ⅵ ）.展开更多
A rapid method for the extraction and monitoring of nanogram level of Pbz＋ and Cuz＋ ions using uniform silanized mesopor （SBA-15） functionalized with aminobenzenesulfonamide groups and flame atomic absorption spec...A rapid method for the extraction and monitoring of nanogram level of Pbz＋ and Cuz＋ ions using uniform silanized mesopor （SBA-15） functionalized with aminobenzenesulfonamide groups and flame atomic absorption spectrometry （FAAS） is presented. Aminobenzenesulfonamide functionalized SBA-15 was synthesized according to procedure in the literature and the presence of organic groups in the silica framework was demonstrated by FT-IR spectra. The functionalized product showed the BET surface area 110 mZ/g and pore diameter 5. l nm, based on adsorption-desorption of N2 at 77 K. The effect of several variables such as （amount of adsorbent, stirring time, pH and presence of other ions in the medium） has been studied. Lead and copper were completely extracted at pH greater than 3 after stirring for 10 min. The maximum capacity of the adsorbent was found to be 191.3 ＋ 1.4 and 155.0 ＋ 1.0 ~xg of lead and copper ions/mg functionalized SBA-15, respectively. The preconcentration factor of the method was found to be 200. The detection limit of the technique was 3.4 and 0.4 ng/mL for Pb2＋ and Cuz＋, respectively. The applications of this methodology for real samples were examined by various water type, black tea and pepper samples.展开更多
A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements...A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements. The analytical performances of the prospsed method for determining Cd, Cu and Mn were studied. The analytes were preconcentrated with a thiol resin(Type 190, produced by Nankai University, China) whose active group is -SH. The elements to be determined were preconcentrated onto the column for 60 s and then rinsed with deionized water and eluted with 30 μL of 1 mol/L HCl. The graphite furnace atomic absorption spectrometry(GFAAS) determination of the concentrated analyte was carried out in parallel with the next preconcentration cycle. Enrichment factors 41, 22 and 20 and detection limits(3 σ , n =10) 0.36, 3.8 and 7.0 ng/L for Cd, Cu and Mn, respectively, along with a sampling frequency of 20 h -1 , were obtained with a 60 s loading time at a sample flow rate of 3.5 mL/min. The analytical results for a number of water samples show that the flow-injection semi-online column preconcentration can not only eliminate the effect of some concomitant elements, such as Li, Na, K, Ca and Mg, on the determination of the analyte, but also enhance the sensitivity.展开更多
The online flow injection preconcentration and electrothermal atomic absorption spectrometry method were used for the determination of trace nickel in electrolytic manganese samples by sorption on a conical minicolumn...The online flow injection preconcentration and electrothermal atomic absorption spectrometry method were used for the determination of trace nickel in electrolytic manganese samples by sorption on a conical minicolumn packed with activated carbon at pH 9.0. The nickel was eluted from the minicolumn with 10%(v/v) nitric acid. An enrichment factor of 190-fold for a sample volume of 10mL was obtained. The detection limit (DL) of nickel with the use of the preconcentration method was 13ng·g -1in the original solid sample. The precision for 10 replicate determinations at 150ng·g -1 nickel concentration was 5.2% relative standard deviation (RSD). The calibration graph was linear with a correlation coefficient of r=0.9996 up to concentration of 660ng·g -1 nickel.展开更多
A novel micelle to solvent stacking on-line sample preconcentration technique in capillary zone electrophoresis（MSS-CZE） has been developed to determine the strychnine and brucine in traditional Chinese medicine pre...A novel micelle to solvent stacking on-line sample preconcentration technique in capillary zone electrophoresis（MSS-CZE） has been developed to determine the strychnine and brucine in traditional Chinese medicine preparations.The optimal running buffer was 30 mmol/L H_3PO_4 containing 20%acetonitrile at pH 4.0.The sample matrix was 8 mmol/L H_3PO_4 containing 5 mmol/L sodium dodecyl sulfate（SDS） at pH 3.0.The established MSS-CZE method afforded more than 50-fold improvements in concentration sensitivity compared with typical CZE-UV analysis.The calibration curve was linear in the range from 0.2 to 15.0μg/ mL for both strychnine and brucine,with correlation coefficients of 0.9984 and 0.9976,respectively.The limits of detection（5/ N = 3：1） for strychnine and brucine were 0.02 and 0.05μg/mL,respectively.The MSS-CZE method has been successfully applied to the analysis of strychnine and brucine in Chinese medicinal preparations.展开更多
Solidified floating organic drop microextraction(SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine(CBZ)in human plasma and ur...Solidified floating organic drop microextraction(SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine(CBZ)in human plasma and urine samples.Parameters that affect the extraction efficiency such as the type and volume of extraction solvent,ionic strength,sodium hydroxide concentration,stirring rate,sample volume and extraction time,were investigated and optimized.Under the optimum conditions(extraction solvent,40μL of 1-undecanol;sodium hydroxide concentration,1 mol/L;temperature,50℃;stirring speed,400 r/min;sample volume,8 mL;sodium chloride concentration,3%(w/v)and extraction time,60 min)the calibration curve was found to be linear in the mass concentration range of 0.4-700.0μg/L.The limit of detection(LOD)was 0.1μg/L and the relative standard deviation(RSD)for six replicate extraction and determination of carbamazepine at 100μg/L level was found to be 4.1%.The method was successfully applied to the determination of CBZ in human plasma and urine samples.展开更多
The present work dealt with the preconcentration of rare earth elements in Saghand ore(Yazd province,Iran)which was achieved by Humphrey spiral using orthogonal optimization method after scrubbing the sample at 45%sol...The present work dealt with the preconcentration of rare earth elements in Saghand ore(Yazd province,Iran)which was achieved by Humphrey spiral using orthogonal optimization method after scrubbing the sample at 45%solid pulp density for 30 min.The pulp was diluted and was fed to a Humphrey spiral for upgrading.The process parameters considered were feed size,feed solids and feed rate,and Taguchi’s L9(34)orthogonal array(OA)was selected for optimization of the process.The results show that the feed rate and feed size were more significant than the other operation parameters of the process.It was also found that under optimal conditions,the concentrate grade of rare earth elements increased from2860 10 6to 6050 10 6and recovery reached to 58%.展开更多
Thiosemicarbazide-grafted multi-walled carbon nanotubes were prepared and employed to investigate the pre-concentration of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） from aqueous solution prior to their determination by ICP-OES....Thiosemicarbazide-grafted multi-walled carbon nanotubes were prepared and employed to investigate the pre-concentration of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） from aqueous solution prior to their determination by ICP-OES. The resulting material was characterized by FT-IR, TGA and SEM. Various factors influencing the separation and pre-concentration were investigated. The enrichment factor typically is 60. Under optimized experimental conditions, the maximum adsorption capacities of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） were found to be 1.98, 10.94, 3.69 mg/g, and the relative standard deviations are 〈 3.5% （n = 6）. The new adsorbent shows superior reusability and stability. The procedure was successfully applied to the determination of trace quantities of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） in water samples.展开更多
In a flow injection separation and precon-centration system incorporating a microcolumn,the adsorption behavior(effect of pH,kinetic adsorption capacity)of metal ions Cu^(²+),Cr+,Mn^(²+),Ni2+,La^(³+),Eu...In a flow injection separation and precon-centration system incorporating a microcolumn,the adsorption behavior(effect of pH,kinetic adsorption capacity)of metal ions Cu^(²+),Cr+,Mn^(²+),Ni2+,La^(³+),Eu^(³+),Ca^(³+),Mo(V)and W(V)on TiO_(2)powder with different crystal structure and particle diameter was studied an d compared.In addition,the mechanism of the adsorption of metal ions on TiO_(2)powder was explored.The results show that crystal structure and particle diameter of the TiO_(2)powder will definitely afect the adsorption capacity of metals on it.展开更多
A novel electroanalytical method. oscillographic chronopotentiometry with high and low frequency current. is presented in this paper. With this method, the sensitivity or almost all kinds of oscillographic chronopoten...A novel electroanalytical method. oscillographic chronopotentiometry with high and low frequency current. is presented in this paper. With this method, the sensitivity or almost all kinds of oscillographic chronopotentiometry can be: enhanced about one order.展开更多
Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions wer...Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions were preconcentrated on the column filled with 8 hydroxyquinoline 5 sulfonic acid cellulose filter and analysed by ICP AES after being eluted with dilute HNO 3. In the given pH range, alkali and alkaline earth metal ions can be separated as matrix elements; a high concentration factor is obtained and the eluates can be measured without interference. The usefulness of the method is shown by the control analyses of standard reference materials. [WT5FZ]展开更多
A new method for the determination of trace non-rare earth elements in high purity rare earth oxides by ICP-AES with preconcentration on an active carbon-silica gel microcolumn in a flow injection system is described ...A new method for the determination of trace non-rare earth elements in high purity rare earth oxides by ICP-AES with preconcentration on an active carbon-silica gel microcolumn in a flow injection system is described in this paper. Experimental parameters such as pH, flow rate,reagent concentration,length of reaction coil,eluent acidity,etc. were optimized. In the buffer solution of NH3. H2O/NH4Cl at pH 4. 6,Al,Cr,Cu,Fe, Pb, V and Zn can be preconcentrated and then eluted with 4. 5 mol/L nitric acid utilizing stop-flow technique. The enrichment factors were in range of 8. 1￣12. 6 with detection limits of μg/m level ,and the RSD with metals at μg/g level were 2. 3￣5. 0% (n= 7). The method proposed can reduce the matrix interference effectively , and has been applied to the determination of non-rare earth metals atμg/g level in high purity Eu2O3 with satisfactory results.展开更多
An adsorbent calix[4]arene carboxylic acid was employed as the adsorption material for on-line flow in jection（FI） micro-column preconcentration coupled with flame atomic absorption spectrometry（FAAS） determinatio...An adsorbent calix[4]arene carboxylic acid was employed as the adsorption material for on-line flow in jection（FI） micro-column preconcentration coupled with flame atomic absorption spectrometry（FAAS） determination of trace heavy metals（Cu, Pb, Co, Ni and Cd）. Parameters such as the pH, loading time and flow rate of sample, and the concentration, volume and flow rate of eluent were optimized. The enrichment factors are 50.0, 56.5, 11.6, 12.1 and 19.1 for Cu, Pb, Co, Ni, and Cd, respectively, and a sample throughput of 20 h–1 was obtained. The limits of de tection for Cu, Pb, Co, Ni, and Cd were in a range of 1.56―3.91 μg/L, and the relative standard deviations（RSDs） were less than 2.76%（n=7）. Furthermore, the proposed method was successfully applied to the determination of Cu, Pb, Co, Ni, and Cd in certified reference materials and various water samples.展开更多
A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by C...A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.展开更多
A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast a...A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast adsorption of chromium (VI) on the high surface area nanometer-size TiO2 (anatase) powders, which prepared by a sol-gel method from hydrolysis of TiCI4 and (ii) the quantitative and reproducible elution of Cr (VI) by 2. 0 mol. L-1 HCI. A mini-column system for preconcentration is developed, Cr(VI)on the mini-column is eluted and merged with a stream water and DPCB (1, 5-diphenylcarbazide ) as the chromogenic reagent. The Proposed system permits throughputs of 6 sample h--l (0. 001 μg mL-1 Cr(VI) ) or 20 sample h-1 (0. 1 μg mL-1Cr (VI) . The preconcentration factor is 55. The detection limit is 0. 8 ng·mL-1 Cr(VI). The reproducibility is satisfactory with a relative standard deviation of less than 3. 35% (0. Of μg'mL-1Cr (VI), n = 5).展开更多
基金supported by NIH award U01 EB0220003-01[CED,NJK]the NIH National Center for Advancing Translational Sciences(NCATS)through grant UL1 TR000002[CED,NJK]+1 种基金NIH award 1P30ES023513-01A1[CED,NJK]NIH award UG3-OD023365[CED,NJK]。
文摘Trace analysis of volatile organic compounds(VOCs) during wildfires is imperative for environmental and health risk assessment. The use of gas sampling devices mounted on unmanned aerial vehicles(UAVs) to chemically sample air during wildfires is of great interest because these devices move freely about their environment, allowing for more representative air samples and the ability to sample areas dangerous or unreachable by humans. This work presents chemical data from air samples obtained in Davis, CA during the most destructive wildfire in California's history-the 2018 Camp Fire – as well as the deployment of our sampling device during a controlled experimental fire while fixed to a UAV. The sampling mechanism was an in-house manufactured micro-gas preconcentrator(μPC) embedded onto a compact battery-operated sampler that was returned to the laboratory for chemical analysis. Compounds commonly observed in wildfires were detected during the Camp Fire using gas chromatography mass spectrometry(GC–MS), including BTEX(benzene, toluene, ethylbenzene, m + p-xylene, and o-xylene), benzaldehyde, 1,4-dichlorobenzene, naphthalene, 1,2,3-trimethylbenzene and 1-ethyl-3-methylbenzene. Concentrations of BTEX were calculated and we observed that benzene and toluene were highest with average concentrations of 4.7 and 15.1 μg/m^(3), respectively. Numerous fire-related compounds including BTEX and aldehydes such as octanal and nonanal were detected upon experimental fire ignition, even at a much smaller sampling time compared to samples taken during the Camp Fire. Analysis of the air samples taken both stationary during the Camp Fire and mobile during an experimental fire show the successful operation of our sampler in a fire environment.
基金supported by Jiangsu Science and Technology Department(No.BG2007044)Jiangsu Preventive Medicine Foundation(No.Y2006025).
文摘A rapid and simple preconcentration step applying packed-fiber solid-phase extraction columns has been investigated to vitamin B12. The extraction performance of the new method was investigated preliminarily on vitamin functional drink. The analysis used a reversed-phase C18 column, with a photo-diode array detector at 220 nm. The samples were preconcentrated with packed-fiber solid-phase extraction columns. Good linearity was observed in vitamin functional drink. The repeatability of extraction performance, expressed as relative standard deviations, was from 3.5% to 4.3%. The limit of detection （LOD） is 5 ng mL^-1 （S/N = 3）. Finally, the method had been applied for the determination of vitamin B12 in vitamin functional drink.
基金The National High Technology Research and Development Program of China under contract Nos 2006AA09Z174 and 2007AA061501the National Natural Science Foundation of China under contract No. 40521003
文摘The unstable state of nitrite results in its very low concentration in seawater, which is below the limit of detection （LOD） of conventional techniques of analysis. Some sensitivity-enhanced methods have been proposed for the determination of nitrite at nanomolar level to illustrate the role of nitrite in the marine nitrogen cycle. However, most of previous reports are not widely accepted, because of their complexity and cost equipment or intensive labor requirement. In this study, a simple automatic system for the determination of nanomolar level nitrite using on-line preconcentration with spectrophotometric detection was described..An Oasis HLB cartridge was adopted to quantitatively enrich the pink-colored azo compound, formed from nitrite via Griess reaction. The cartridge was rinsed with water and ethanol （volume fraction is 55%, the same below）, in turn, then eluted by an eluent containing 50% ethanol and 0.25 M（mol/dm^3） H2SO4, and determined at 543 nm with a 2 cm path-length flow cell. Under the optimized experimental conditions, the calibration curve showed a good linearity in the range of 1.4 85.7 aM, and the LOD （3a） was estimated to be 0.5 nM. The relative standard deviations of 7 measurements were 4.0% and 1.0% for the samples spiked at 7.1 and 28.6 nM, respectively. The recoveries for the different natural water samples were between 92.2%-108.4%. Each HLB cartridge could be reused for at least 50 times. As compared with other SPE methods, the advantages of this method included the free of interference from salinity variation and less sample consuming. The results of the application of the proposed method to natural water showed good agreement with liquid waveguide capillary cell detection method.
基金Supported by the Excellent Talents Project(No.2009R30)Innovation Team Project(No.2007T053)of the Education Department of Liaoning Province,China
文摘Nano-TiO2 was employed for the separation and preconcentration of thallium.It was found that the adsorption ratio of thallium ions was more than 98% at pH 4.5 and the desorption ratio reached 99% under microwave irradiation for 3 min at 350 W.The adsorption equilibrium was well described by the Langmuir isotherm model with a maximum adsorption capacity of 4.09 mg/g[（20±0.1） °C].The nano-TiO2 was successfully applied to the determination of element thallium in the certified reference material polymetallic nodule and water samples.
基金the Key Project for Science and Technology Development of Jilin Province, China(No.20010306-1)the China’s Post-doctoral Science Fund(No.20040350561).
文摘This article focuses on iodine determination by microwave plasma torch atomic emission spectrometry （MPT-AES） coupled with online preconcentration vapor generation method. A new desolvation device, multistrand Nafion dryer, was used as the substitute for condenser desolvation system. Some experimental conditions, such as preconcentration time, acidity of sample solution, rinsing solution acidity and dynamic linear range were investigated and optimized. The new desolvation system eliminates the problem of decreasing emission intensity of I（I） 206.238 nm line with the increase of working time on a conventional condenser desolvation system, thus greatly improving the reproducibility.
基金Supported by the Natural Science Foundation of Henan Province(No.0511020500).
文摘Molybdenum（ Ⅵ ） is a biologically essential trace element and its role in an extremely wide variety of systems has been reported. Most common methods often fail to determine trace Mo （ Ⅵ ） in the analysis of molybdenum-containing samples, due to limitations such as inadequate detection limits and matrix interference, which make the direct determinations impossible. To solve this problem, various approaches are employed to concentrate and separate Mo（ Ⅵ ） to detectable levels. Concentration and separation methods play a main role in the analysis of trace Mo（Ⅵ）. Therefore, many separation and preconcentration procedures have been developed for the determination of Mo （ Ⅵ ）.
基金the Islamic Azad University, Shahre Rey Branch, for the support
文摘A rapid method for the extraction and monitoring of nanogram level of Pbz＋ and Cuz＋ ions using uniform silanized mesopor （SBA-15） functionalized with aminobenzenesulfonamide groups and flame atomic absorption spectrometry （FAAS） is presented. Aminobenzenesulfonamide functionalized SBA-15 was synthesized according to procedure in the literature and the presence of organic groups in the silica framework was demonstrated by FT-IR spectra. The functionalized product showed the BET surface area 110 mZ/g and pore diameter 5. l nm, based on adsorption-desorption of N2 at 77 K. The effect of several variables such as （amount of adsorbent, stirring time, pH and presence of other ions in the medium） has been studied. Lead and copper were completely extracted at pH greater than 3 after stirring for 10 min. The maximum capacity of the adsorbent was found to be 191.3 ＋ 1.4 and 155.0 ＋ 1.0 ~xg of lead and copper ions/mg functionalized SBA-15, respectively. The preconcentration factor of the method was found to be 200. The detection limit of the technique was 3.4 and 0.4 ng/mL for Pb2＋ and Cuz＋, respectively. The applications of this methodology for real samples were examined by various water type, black tea and pepper samples.
文摘A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements. The analytical performances of the prospsed method for determining Cd, Cu and Mn were studied. The analytes were preconcentrated with a thiol resin(Type 190, produced by Nankai University, China) whose active group is -SH. The elements to be determined were preconcentrated onto the column for 60 s and then rinsed with deionized water and eluted with 30 μL of 1 mol/L HCl. The graphite furnace atomic absorption spectrometry(GFAAS) determination of the concentrated analyte was carried out in parallel with the next preconcentration cycle. Enrichment factors 41, 22 and 20 and detection limits(3 σ , n =10) 0.36, 3.8 and 7.0 ng/L for Cd, Cu and Mn, respectively, along with a sampling frequency of 20 h -1 , were obtained with a 60 s loading time at a sample flow rate of 3.5 mL/min. The analytical results for a number of water samples show that the flow-injection semi-online column preconcentration can not only eliminate the effect of some concomitant elements, such as Li, Na, K, Ca and Mg, on the determination of the analyte, but also enhance the sensitivity.
文摘The online flow injection preconcentration and electrothermal atomic absorption spectrometry method were used for the determination of trace nickel in electrolytic manganese samples by sorption on a conical minicolumn packed with activated carbon at pH 9.0. The nickel was eluted from the minicolumn with 10%(v/v) nitric acid. An enrichment factor of 190-fold for a sample volume of 10mL was obtained. The detection limit (DL) of nickel with the use of the preconcentration method was 13ng·g -1in the original solid sample. The precision for 10 replicate determinations at 150ng·g -1 nickel concentration was 5.2% relative standard deviation (RSD). The calibration graph was linear with a correlation coefficient of r=0.9996 up to concentration of 660ng·g -1 nickel.
基金supported by the Natural Science Foundations of Hebei(NoB2010000657)
文摘A novel micelle to solvent stacking on-line sample preconcentration technique in capillary zone electrophoresis（MSS-CZE） has been developed to determine the strychnine and brucine in traditional Chinese medicine preparations.The optimal running buffer was 30 mmol/L H_3PO_4 containing 20%acetonitrile at pH 4.0.The sample matrix was 8 mmol/L H_3PO_4 containing 5 mmol/L sodium dodecyl sulfate（SDS） at pH 3.0.The established MSS-CZE method afforded more than 50-fold improvements in concentration sensitivity compared with typical CZE-UV analysis.The calibration curve was linear in the range from 0.2 to 15.0μg/ mL for both strychnine and brucine,with correlation coefficients of 0.9984 and 0.9976,respectively.The limits of detection（5/ N = 3：1） for strychnine and brucine were 0.02 and 0.05μg/mL,respectively.The MSS-CZE method has been successfully applied to the analysis of strychnine and brucine in Chinese medicinal preparations.
文摘Solidified floating organic drop microextraction(SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine(CBZ)in human plasma and urine samples.Parameters that affect the extraction efficiency such as the type and volume of extraction solvent,ionic strength,sodium hydroxide concentration,stirring rate,sample volume and extraction time,were investigated and optimized.Under the optimum conditions(extraction solvent,40μL of 1-undecanol;sodium hydroxide concentration,1 mol/L;temperature,50℃;stirring speed,400 r/min;sample volume,8 mL;sodium chloride concentration,3%(w/v)and extraction time,60 min)the calibration curve was found to be linear in the mass concentration range of 0.4-700.0μg/L.The limit of detection(LOD)was 0.1μg/L and the relative standard deviation(RSD)for six replicate extraction and determination of carbamazepine at 100μg/L level was found to be 4.1%.The method was successfully applied to the determination of CBZ in human plasma and urine samples.
基金the deputy director of Research and Development in Atomic Energy of Iran for financial support as well as Nuclear Science and Technology Research Institute for technical support
文摘The present work dealt with the preconcentration of rare earth elements in Saghand ore(Yazd province,Iran)which was achieved by Humphrey spiral using orthogonal optimization method after scrubbing the sample at 45%solid pulp density for 30 min.The pulp was diluted and was fed to a Humphrey spiral for upgrading.The process parameters considered were feed size,feed solids and feed rate,and Taguchi’s L9(34)orthogonal array(OA)was selected for optimization of the process.The results show that the feed rate and feed size were more significant than the other operation parameters of the process.It was also found that under optimal conditions,the concentrate grade of rare earth elements increased from2860 10 6to 6050 10 6and recovery reached to 58%.
文摘Thiosemicarbazide-grafted multi-walled carbon nanotubes were prepared and employed to investigate the pre-concentration of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） from aqueous solution prior to their determination by ICP-OES. The resulting material was characterized by FT-IR, TGA and SEM. Various factors influencing the separation and pre-concentration were investigated. The enrichment factor typically is 60. Under optimized experimental conditions, the maximum adsorption capacities of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） were found to be 1.98, 10.94, 3.69 mg/g, and the relative standard deviations are 〈 3.5% （n = 6）. The new adsorbent shows superior reusability and stability. The procedure was successfully applied to the determination of trace quantities of Cd（Ⅱ）, Cu（Ⅱ） and Pb（Ⅱ） in water samples.
文摘In a flow injection separation and precon-centration system incorporating a microcolumn,the adsorption behavior(effect of pH,kinetic adsorption capacity)of metal ions Cu^(²+),Cr+,Mn^(²+),Ni2+,La^(³+),Eu^(³+),Ca^(³+),Mo(V)and W(V)on TiO_(2)powder with different crystal structure and particle diameter was studied an d compared.In addition,the mechanism of the adsorption of metal ions on TiO_(2)powder was explored.The results show that crystal structure and particle diameter of the TiO_(2)powder will definitely afect the adsorption capacity of metals on it.
基金The authors gratefully acknowedge the financial support from the National Natural Scicllcc Foundation of China Nat
文摘A novel electroanalytical method. oscillographic chronopotentiometry with high and low frequency current. is presented in this paper. With this method, the sensitivity or almost all kinds of oscillographic chronopotentiometry can be: enhanced about one order.
基金Supported by the National Natural Science Foundation of China
文摘Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions were preconcentrated on the column filled with 8 hydroxyquinoline 5 sulfonic acid cellulose filter and analysed by ICP AES after being eluted with dilute HNO 3. In the given pH range, alkali and alkaline earth metal ions can be separated as matrix elements; a high concentration factor is obtained and the eluates can be measured without interference. The usefulness of the method is shown by the control analyses of standard reference materials. [WT5FZ]
文摘A new method for the determination of trace non-rare earth elements in high purity rare earth oxides by ICP-AES with preconcentration on an active carbon-silica gel microcolumn in a flow injection system is described in this paper. Experimental parameters such as pH, flow rate,reagent concentration,length of reaction coil,eluent acidity,etc. were optimized. In the buffer solution of NH3. H2O/NH4Cl at pH 4. 6,Al,Cr,Cu,Fe, Pb, V and Zn can be preconcentrated and then eluted with 4. 5 mol/L nitric acid utilizing stop-flow technique. The enrichment factors were in range of 8. 1￣12. 6 with detection limits of μg/m level ,and the RSD with metals at μg/g level were 2. 3￣5. 0% (n= 7). The method proposed can reduce the matrix interference effectively , and has been applied to the determination of non-rare earth metals atμg/g level in high purity Eu2O3 with satisfactory results.
基金Supported by the Fund of State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemi-stry, Chinese Academy of Sciences(No.RERU2011006)
文摘An adsorbent calix[4]arene carboxylic acid was employed as the adsorption material for on-line flow in jection（FI） micro-column preconcentration coupled with flame atomic absorption spectrometry（FAAS） determination of trace heavy metals（Cu, Pb, Co, Ni and Cd）. Parameters such as the pH, loading time and flow rate of sample, and the concentration, volume and flow rate of eluent were optimized. The enrichment factors are 50.0, 56.5, 11.6, 12.1 and 19.1 for Cu, Pb, Co, Ni, and Cd, respectively, and a sample throughput of 20 h–1 was obtained. The limits of de tection for Cu, Pb, Co, Ni, and Cd were in a range of 1.56―3.91 μg/L, and the relative standard deviations（RSDs） were less than 2.76%（n=7）. Furthermore, the proposed method was successfully applied to the determination of Cu, Pb, Co, Ni, and Cd in certified reference materials and various water samples.
文摘A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.
文摘A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast adsorption of chromium (VI) on the high surface area nanometer-size TiO2 (anatase) powders, which prepared by a sol-gel method from hydrolysis of TiCI4 and (ii) the quantitative and reproducible elution of Cr (VI) by 2. 0 mol. L-1 HCI. A mini-column system for preconcentration is developed, Cr(VI)on the mini-column is eluted and merged with a stream water and DPCB (1, 5-diphenylcarbazide ) as the chromogenic reagent. The Proposed system permits throughputs of 6 sample h--l (0. 001 μg mL-1 Cr(VI) ) or 20 sample h-1 (0. 1 μg mL-1Cr (VI) . The preconcentration factor is 55. The detection limit is 0. 8 ng·mL-1 Cr(VI). The reproducibility is satisfactory with a relative standard deviation of less than 3. 35% (0. Of μg'mL-1Cr (VI), n = 5).
