A new method for determining the kinetic order and activation energy for atom formation in electrothermal atomic absorption spec-trometry is proposed. The assumption of first order kinetics for atom formation and the ...A new method for determining the kinetic order and activation energy for atom formation in electrothermal atomic absorption spec-trometry is proposed. The assumption of first order kinetics for atom formation and the steady-state approximation which appeared in the previous models is avoided in the proposed method. The kinetic parameters for atom formation of Li have been obtained, and the effect of the amount of analysed sample, ashing temperature, atomization temperature, heating rate, gas flow and tube surface on the atomization of Li has also been investigated.展开更多
[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision ...[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision departments. [Methods] The lead content in lime-preserved eggs was measured by the microwave digestion and flame atomic absorption spectroscopy. [Results] The method had a correlation coefficient of r2=0.998 in the injection concentration range of 0-4 mg/L. The detection limit of the method was 0.008 2 mg/kg. In the range of 0.2 to 1.0 mg/kg addition concentration, the recovery rate of the method was 92.5%-108.0%, and the relative standard deviation(RSD) was <5%. [Conclusions] This method is accurate and reliable, simple and efficient, and is suitable for the detection of lead in lime-preserved eggs.展开更多
[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by co...[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by combined flame atomic absorption spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-0.8 mg/L for Cr and 0-0.8 mg/L for Zn, the detection limits of Cr and Zn was 0.0025 mg/L and 0.002 3 mg/L, respectively. Recoveries of 102.4%-103.2% for Cr and 97.7%-98.3% for Zn were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of Cr and Zn in soil samples.展开更多
[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with H...[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with HNO3-HSO4 (5:1) and determining Cd in the samples by a flame atomic absorption spectrophotometer. [Results] The Cd contents in squil a were 1.0-2.0 mg/kg, and the recoveries of Cd were 86%-109%, and the relative standard deviations were 0-6%. [Conclusion] The method is simple and rapid with strong operability, good reproducibility and high ac-curacy.展开更多
In the study, the contents of 5 trace elements including Fe, Cu, Mg, Mn and Ca were directly analyzed by flame atomic absorption spectroscopy in Gu- oshangye. The sample was subjected to microwave digestion with HNO3 ...In the study, the contents of 5 trace elements including Fe, Cu, Mg, Mn and Ca were directly analyzed by flame atomic absorption spectroscopy in Gu- oshangye. The sample was subjected to microwave digestion with HNO3 and H2O2, and detected by the standard curve method. The results showed that Guoshangye contained abundant trace elements which rates of these trace elements were in the curacy and satisfactory. were necessary for human. The recovery range of 96%-103%. The method is ac-展开更多
[Objective] This study aimed to analyze the contents of trace elements in potatoes from different production areas in Qinghai Province. [Method] By flame atomic absorption spectrometry (FAAS), the contents of variou...[Objective] This study aimed to analyze the contents of trace elements in potatoes from different production areas in Qinghai Province. [Method] By flame atomic absorption spectrometry (FAAS), the contents of various trace elements in potatoes were determined. [Result] Potatoes contain abundant trace elements such as Cu, Zn, Fe, Mn, Ca, K and Mg. To be specific, the contents of Ca, K and Mg were relatively high. [Conclusion] By using FAAS, the relative standard deviation was 1.17%-2.75% and the recovery rate was 97%-99.5%, indicating accurate and reli-able results with high precision.展开更多
A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction ( CPE ). 1-( 2-Pyr...A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction ( CPE ). 1-( 2-Pyridylazo ) -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu ( Ⅱ ). This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.展开更多
Cloud point extraction (CPE) with Tergitol TMN-6 was applied for the extraction of trace amounts of palladium (Pd(Ⅱ)), platinum (Pt(Ⅳ)), and gold (Au(Ⅲ)) in the soil of industrial sewage. Ammonium pyrolysine dithio...Cloud point extraction (CPE) with Tergitol TMN-6 was applied for the extraction of trace amounts of palladium (Pd(Ⅱ)), platinum (Pt(Ⅳ)), and gold (Au(Ⅲ)) in the soil of industrial sewage. Ammonium pyrolysine dithiocarbamate (APDC) was adopted as the chelating agent prior to CPE and then was detected by atomic absorption spectrometry (AAS). Different parameters such as the concentration of surfactants, chelating agent and salt, sample pH, equilibration temperature and time, centrifugation time and rates, and the effect of foreign ions were studied. Under optimum conditions, the low limits of detections are 1.4, 2.8 and 1.2 ng·ml^-1 and the enrichment factors are 21, 12, and 24 for Pd(Ⅱ), Pt(Ⅳ), and Au(Ⅲ, respectively. The relative standard deviations vary from 0.6% to 1.0% (n=11). All correlation coefficients of the calibration curves are >0.9960. The proposed method was successfully applied for the determination of Pd(Ⅱ), Pt(Ⅳ), and Au(Ⅲ) in the real soil of industrial sewage samples.展开更多
A method was developed for the determination of total arsenic concentration in less than ng/ml level by decomposition of organoarsenicals using photo -oxidation combined with in situ trapping of arsenic hydride on a p...A method was developed for the determination of total arsenic concentration in less than ng/ml level by decomposition of organoarsenicals using photo -oxidation combined with in situ trapping of arsenic hydride on a palladium coated graphite tube with subsequent atomization and detection by AAS. The organoarsenicals include monomethylarsenic, dimethylarsenic, arsenobetaine, arsenocholine, o -aminobenzenarsenate and p -aminobenzenarsenate. The method is simple and sensitive. Detection limit was obtained from different arsenic compounds over the range from 0. 058 to 0.063 ng/ml as As (based on three times of the standard deviation of 10 blank measurements) and the relative standard deviations for ten replicate measurements were from 2.0 to 3.8%. The calibration curves of arsenic compounds including inorganic and organic arsenicals were linear over the range from 0.1 to 3.0 ng/ml as As. The recommended method has been applied to the determination of total arsenic in tap and lake water samples at ng/ml levels.展开更多
Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions wher...Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions where the combination of a pyrolytic coating graphitetube and fast raising temperature were used and the temperature was stable, the signal peak shapescould be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curvemethod.展开更多
A new method based on the cloud point extraction(CPE) for separation and preconcentration of nickel(Ⅱ) and its subsequent determination by graphite furnace atomic absorption spectrometry(GFAAS) was proposed, 8-...A new method based on the cloud point extraction(CPE) for separation and preconcentration of nickel(Ⅱ) and its subsequent determination by graphite furnace atomic absorption spectrometry(GFAAS) was proposed, 8-hydroxyquinoline and Triton X-100 were used as the ligand and surfactant respectively. Nickel(Ⅱ) can form a hy-drophobic complex with 8-hydroxyquinoline, the complex can be extracted into the small volume surfactant rich phase at the cloud point temperature(CPT) for GFAAS determination. The factors affecting the cloud point extraction, such as pH, ligand concentration, surfactant concentration, and the incubation time were optimized. Under the optimal conditions, a detection limit of 12 ng/L and a relative standard deviation(RSD) of 2.9% were obtained for Ni(Ⅱ) determination. The enrichment factor was found to be 25. The proposed method was successfully applied to the determination of nickel(Ⅱ) in certified reference material and different types of water samples and the recovery was in a range of 95%―103%.展开更多
In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption ...In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity (R^2=0.9992) over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.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 method for the determination of trace mercury in water samples by hydride generation atomic absorption spectrophotometry after cloud point extraction was proposed in the present work. The effects of pH, concentratio...A method for the determination of trace mercury in water samples by hydride generation atomic absorption spectrophotometry after cloud point extraction was proposed in the present work. The effects of pH, concentration of surfactant, and equilibration time on cloud point extraction were discussed. The enhancement factor of 20 and the detection limit of 0.039 μg/L were obtained for mercury with relative standard deviation of 4.8% (n = 11).展开更多
A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water s...A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.展开更多
The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry (FAAS) were investigated. It was found that boric acid as a matrix modifier obviously e...The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry (FAAS) were investigated. It was found that boric acid as a matrix modifier obviously eliminated silicate interference. Under the optimum operating conditions, the determination results of iron in layered crystal sodium disilicate and sodium silicate samples by FAAS were satisfactory. The linear range of calibration curve is 0-10.5 μg.mL^-1, the relative standard deviation of method is 1.2%-2.2%, the recovery of added iron is 96.0%- 101%, the sensitivity is 0.19 μg.mL^-l and the detection limit is 77 ng.mL^-1. The effect of the determination of iron of the standard curve method, standard addition calibration and colorimetry method was the same, but the first has the merits of rapid sample preparation, reduced contamination risks and fast analysis.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
The adsorption behavior of multiwalled carbon nanotubes (MWNTs) toward heavy elements has been investigated systemically, and a new method has been developed for the determination of trace elements in water samples ...The adsorption behavior of multiwalled carbon nanotubes (MWNTs) toward heavy elements has been investigated systemically, and a new method has been developed for the determination of trace elements in water samples based on preconcentration with mini-column packed with MWNTs prior to its determination by flame atomic absorption spectrometry (FAAS) The recommended parameters of proposed method influencing the preconcentration of the analytes, such as pH of the sample, sample flow rate and volume, elute solution and interfering ions, have been used. Under the optimized conditions, the calibration graphs were linear with the correlation coefficient range 0.9981-0.9995. According to the results, the metals were found 0.019-0.051, 0.011-0.031, 0.00-0.081, 0.00-0.0002, 0.007-0.0925, 0.00-0.0104 μg/L in water samples for Pb, Mn, Zn, Cd, Fe, Cu respectively. The percentage relative standard deviation (%RSD) for five replicate samples were 〈 5% in all cases. The method has been successfully applied to the determination of trace elements in some environmental samples with satisfactory results.展开更多
While engineered nanoparticles are widely used and maybe eventually released into the environment,natural nanoparticles are also commonly found in the Earth system.Nanoparticles may critically affect the geochemical m...While engineered nanoparticles are widely used and maybe eventually released into the environment,natural nanoparticles are also commonly found in the Earth system.Nanoparticles may critically affect the geochemical migration of associated elements and pose potential threats to the ecological environment.It is necessary to establish an accurate and reliable method for measuring the concentration of nanoparticles.AAS is one of the most commonly used methods for the concentration determination of nanoparticles.However,till now,there has been no systematic report on how experimental variables affect AAS measurements.In this study,we used gold nanoparticles(AuNPs) as an example and studied the influences of a list of factors on the concentration determination of AuNPs by AAS,including digestion method,ionization interference,acidic medium,background correction method,and organic matter.We demonstrate that all these factors may have varying degrees of influence on the measured gold concentrations.When the gold colloid is digested at room temperature for more than 8 h or at 60℃ for more than 2 h,and the system contains a low concentration of organic matter,AAS can accurately measure the AuNP concentration at ppm-level.The deuterium lamp background deduction method is not recommended to use for samples with lower gold concentrations.展开更多
文摘A new method for determining the kinetic order and activation energy for atom formation in electrothermal atomic absorption spec-trometry is proposed. The assumption of first order kinetics for atom formation and the steady-state approximation which appeared in the previous models is avoided in the proposed method. The kinetic parameters for atom formation of Li have been obtained, and the effect of the amount of analysed sample, ashing temperature, atomization temperature, heating rate, gas flow and tube surface on the atomization of Li has also been investigated.
文摘[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision departments. [Methods] The lead content in lime-preserved eggs was measured by the microwave digestion and flame atomic absorption spectroscopy. [Results] The method had a correlation coefficient of r2=0.998 in the injection concentration range of 0-4 mg/L. The detection limit of the method was 0.008 2 mg/kg. In the range of 0.2 to 1.0 mg/kg addition concentration, the recovery rate of the method was 92.5%-108.0%, and the relative standard deviation(RSD) was <5%. [Conclusions] This method is accurate and reliable, simple and efficient, and is suitable for the detection of lead in lime-preserved eggs.
基金Supported by Key Fund of Guangxi Academy of Agricultural Sciences(2014JZ01 and2013YZ07)~~
文摘[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by combined flame atomic absorption spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-0.8 mg/L for Cr and 0-0.8 mg/L for Zn, the detection limits of Cr and Zn was 0.0025 mg/L and 0.002 3 mg/L, respectively. Recoveries of 102.4%-103.2% for Cr and 97.7%-98.3% for Zn were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of Cr and Zn in soil samples.
基金Supported by Science and Technology Planning Project of Zhejiang Province(2015C32001)Special Fund for Research Institutes from Science and Technology Department of Zhejiang Province(2016F30021)Natural Science Foundation of China(21407127)~~
文摘[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with HNO3-HSO4 (5:1) and determining Cd in the samples by a flame atomic absorption spectrophotometer. [Results] The Cd contents in squil a were 1.0-2.0 mg/kg, and the recoveries of Cd were 86%-109%, and the relative standard deviations were 0-6%. [Conclusion] The method is simple and rapid with strong operability, good reproducibility and high ac-curacy.
基金Supported by the Research Project for Postgraduate Students of Minzu University of China in 2015Scientific and Technological Cooperation Planning Project of Guizhou Province(QKJ LH[2015]7265)~~
文摘In the study, the contents of 5 trace elements including Fe, Cu, Mg, Mn and Ca were directly analyzed by flame atomic absorption spectroscopy in Gu- oshangye. The sample was subjected to microwave digestion with HNO3 and H2O2, and detected by the standard curve method. The results showed that Guoshangye contained abundant trace elements which rates of these trace elements were in the curacy and satisfactory. were necessary for human. The recovery range of 96%-103%. The method is ac-
文摘[Objective] This study aimed to analyze the contents of trace elements in potatoes from different production areas in Qinghai Province. [Method] By flame atomic absorption spectrometry (FAAS), the contents of various trace elements in potatoes were determined. [Result] Potatoes contain abundant trace elements such as Cu, Zn, Fe, Mn, Ca, K and Mg. To be specific, the contents of Ca, K and Mg were relatively high. [Conclusion] By using FAAS, the relative standard deviation was 1.17%-2.75% and the recovery rate was 97%-99.5%, indicating accurate and reli-able results with high precision.
基金the Analysis and Testing Foundation of Zhejiang Province(No 04045)
文摘A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction ( CPE ). 1-( 2-Pyridylazo ) -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu ( Ⅱ ). This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.
基金supported by the National Natural Science Foundation of China(No.20961012)the Medical Neurobiology Key Laboratory of Kunming University of Science and Technology,Basic and Applied Research Project in Yunnan Province(No.2008ZC082M)+3 种基金the Analysis and Testing Foundation of Kunming University of Science and Technology(No.2010121)Innovation Fund for Smalland Medium Technology Based Firms(No.11C26215305936)Natural and Science Foundation of Yunnan Province(No.2010ZC027)Focus Fund of Department of Education in Yunnan Province(No.2010Z016)
文摘Cloud point extraction (CPE) with Tergitol TMN-6 was applied for the extraction of trace amounts of palladium (Pd(Ⅱ)), platinum (Pt(Ⅳ)), and gold (Au(Ⅲ)) in the soil of industrial sewage. Ammonium pyrolysine dithiocarbamate (APDC) was adopted as the chelating agent prior to CPE and then was detected by atomic absorption spectrometry (AAS). Different parameters such as the concentration of surfactants, chelating agent and salt, sample pH, equilibration temperature and time, centrifugation time and rates, and the effect of foreign ions were studied. Under optimum conditions, the low limits of detections are 1.4, 2.8 and 1.2 ng·ml^-1 and the enrichment factors are 21, 12, and 24 for Pd(Ⅱ), Pt(Ⅳ), and Au(Ⅲ, respectively. The relative standard deviations vary from 0.6% to 1.0% (n=11). All correlation coefficients of the calibration curves are >0.9960. The proposed method was successfully applied for the determination of Pd(Ⅱ), Pt(Ⅳ), and Au(Ⅲ) in the real soil of industrial sewage samples.
文摘A method was developed for the determination of total arsenic concentration in less than ng/ml level by decomposition of organoarsenicals using photo -oxidation combined with in situ trapping of arsenic hydride on a palladium coated graphite tube with subsequent atomization and detection by AAS. The organoarsenicals include monomethylarsenic, dimethylarsenic, arsenobetaine, arsenocholine, o -aminobenzenarsenate and p -aminobenzenarsenate. The method is simple and sensitive. Detection limit was obtained from different arsenic compounds over the range from 0. 058 to 0.063 ng/ml as As (based on three times of the standard deviation of 10 blank measurements) and the relative standard deviations for ten replicate measurements were from 2.0 to 3.8%. The calibration curves of arsenic compounds including inorganic and organic arsenicals were linear over the range from 0.1 to 3.0 ng/ml as As. The recommended method has been applied to the determination of total arsenic in tap and lake water samples at ng/ml levels.
文摘Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions where the combination of a pyrolytic coating graphitetube and fast raising temperature were used and the temperature was stable, the signal peak shapescould be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curvemethod.
基金Supported by the National Natural Science Foundation of China(No.20075009)
文摘A new method based on the cloud point extraction(CPE) for separation and preconcentration of nickel(Ⅱ) and its subsequent determination by graphite furnace atomic absorption spectrometry(GFAAS) was proposed, 8-hydroxyquinoline and Triton X-100 were used as the ligand and surfactant respectively. Nickel(Ⅱ) can form a hy-drophobic complex with 8-hydroxyquinoline, the complex can be extracted into the small volume surfactant rich phase at the cloud point temperature(CPT) for GFAAS determination. The factors affecting the cloud point extraction, such as pH, ligand concentration, surfactant concentration, and the incubation time were optimized. Under the optimal conditions, a detection limit of 12 ng/L and a relative standard deviation(RSD) of 2.9% were obtained for Ni(Ⅱ) determination. The enrichment factor was found to be 25. The proposed method was successfully applied to the determination of nickel(Ⅱ) in certified reference material and different types of water samples and the recovery was in a range of 95%―103%.
基金Project supported by the Hi-Tech Research and Development Program (863) of China (No.2006AA06Z424)Personal Innovation Foundation of Universities in Henan Province (No.[2005]-126)+1 种基金Youth Science Foundation of Henan Normal University (No.2004005)Natural Science Foundation of Henan Province (No.072300460010).
文摘In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity (R^2=0.9992) over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.
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.
文摘A method for the determination of trace mercury in water samples by hydride generation atomic absorption spectrophotometry after cloud point extraction was proposed in the present work. The effects of pH, concentration of surfactant, and equilibration time on cloud point extraction were discussed. The enhancement factor of 20 and the detection limit of 0.039 μg/L were obtained for mercury with relative standard deviation of 4.8% (n = 11).
文摘A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.
文摘The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry (FAAS) were investigated. It was found that boric acid as a matrix modifier obviously eliminated silicate interference. Under the optimum operating conditions, the determination results of iron in layered crystal sodium disilicate and sodium silicate samples by FAAS were satisfactory. The linear range of calibration curve is 0-10.5 μg.mL^-1, the relative standard deviation of method is 1.2%-2.2%, the recovery of added iron is 96.0%- 101%, the sensitivity is 0.19 μg.mL^-l and the detection limit is 77 ng.mL^-1. The effect of the determination of iron of the standard curve method, standard addition calibration and colorimetry method was the same, but the first has the merits of rapid sample preparation, reduced contamination risks and fast analysis.
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The adsorption behavior of multiwalled carbon nanotubes (MWNTs) toward heavy elements has been investigated systemically, and a new method has been developed for the determination of trace elements in water samples based on preconcentration with mini-column packed with MWNTs prior to its determination by flame atomic absorption spectrometry (FAAS) The recommended parameters of proposed method influencing the preconcentration of the analytes, such as pH of the sample, sample flow rate and volume, elute solution and interfering ions, have been used. Under the optimized conditions, the calibration graphs were linear with the correlation coefficient range 0.9981-0.9995. According to the results, the metals were found 0.019-0.051, 0.011-0.031, 0.00-0.081, 0.00-0.0002, 0.007-0.0925, 0.00-0.0104 μg/L in water samples for Pb, Mn, Zn, Cd, Fe, Cu respectively. The percentage relative standard deviation (%RSD) for five replicate samples were 〈 5% in all cases. The method has been successfully applied to the determination of trace elements in some environmental samples with satisfactory results.
基金supported by Guizhou Provincial Science and Technology Foundation (Qian Sci.Co.ZK[2021] No.198)Doctoral Research Startup Project in 2017 of Guizhou Normal University in China+1 种基金the B-type Strategic Priority Program of the Chinese Academy of Sciences (Grant No.XDB41000000)the National Natural Science Foundation of China (41872046,41173074 and 42063008)。
文摘While engineered nanoparticles are widely used and maybe eventually released into the environment,natural nanoparticles are also commonly found in the Earth system.Nanoparticles may critically affect the geochemical migration of associated elements and pose potential threats to the ecological environment.It is necessary to establish an accurate and reliable method for measuring the concentration of nanoparticles.AAS is one of the most commonly used methods for the concentration determination of nanoparticles.However,till now,there has been no systematic report on how experimental variables affect AAS measurements.In this study,we used gold nanoparticles(AuNPs) as an example and studied the influences of a list of factors on the concentration determination of AuNPs by AAS,including digestion method,ionization interference,acidic medium,background correction method,and organic matter.We demonstrate that all these factors may have varying degrees of influence on the measured gold concentrations.When the gold colloid is digested at room temperature for more than 8 h or at 60℃ for more than 2 h,and the system contains a low concentration of organic matter,AAS can accurately measure the AuNP concentration at ppm-level.The deuterium lamp background deduction method is not recommended to use for samples with lower gold concentrations.