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
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
On-line ion-exchange separation and preconcentration were combined with flow-injection hydride generation atomic absorption spectrometry (HGAAS) to determine ultra-trace amounts of antimony in water samples. Antimony(...On-line ion-exchange separation and preconcentration were combined with flow-injection hydride generation atomic absorption spectrometry (HGAAS) to determine ultra-trace amounts of antimony in water samples. Antimony(Ⅲ) was preconcentrated on a micro-column packed with CPG-8Q chelating ion-exchanger using time-based sample loading and eluted by 4 mol l^(-1) HCl directly into the hydride generation AAS system. A detection limit (3σ) of 0.0015μg l^(-1) Sb(Ⅲ) was obtained on the basis of a 20 fold enrichment and with a sampling frequency of 60h^(-1). The precision was 1.0% r.s.d.(n=11) at the 0.5μg l^(-1) Sb(Ⅲ) level. Recoveries for the analysis of antimony in tap water, snow water and sea water samples were in the range 97-102%.展开更多
A continuous phosphine (PH3) generation was developed and applied to the sensitive detection of phosphorus by ICP-AES. Phosphate ion in aqueous solution was converted to phosphine by passing the sample solution throug...A continuous phosphine (PH3) generation was developed and applied to the sensitive detection of phosphorus by ICP-AES. Phosphate ion in aqueous solution was converted to phosphine by passing the sample solution through an incandescent copper silica-tube. Detection limit is 2 ng/mL. The relative standard deviation is 4.2% for 20 ng/mL. The method is rapid and simple with low contamination and high sensitivity.展开更多
A sensitive atomic spectrometric method for the redox speciation analysis of Sb in water is described. The proposed method is based on the selective generation of stibine from Sb(III) in a continuous flow system usi...A sensitive atomic spectrometric method for the redox speciation analysis of Sb in water is described. The proposed method is based on the selective generation of stibine from Sb(III) in a continuous flow system using non-dispersive atomic fluorescence spectrometry for detection. The effects of the HCI concentration on the fluorescence intensities of Sb(III) and Sb(V) were investigated. The results indicated that atomic fluorescence emission due to Sb(V) can constructively interfere with the determination of Sb(III). For the determination of Sb(III), four compounds were tested as masking agents to inhibit the generation of stibine from Sb(V). The effects of the concentrations of the masking agents and of HC1 on the fluorescence signals from Sb(III) and Sb(V) were studied. The results indicated that citric acid and NaF can successfully suppress hydride generation from Sb(V). To evaluate the developed methodology and the influence of the matrix, the recovery of Sb(III) from natural water that was spiked with different Sb(III) and Sb(V) concentrations was tested.展开更多
A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS) with selective electrochemical reduction. The d...A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS) with selective electrochemical reduction. The determination of inorganic arsenic species is based on the fact that As(Ⅲ) shows significantly higher absorbance at low electrolytic currents than As(Ⅴ) in 0.3 mol·L^-1 H2SO4. The electrolytic current used for the determination of As(Ⅲ) without considerable interferences of As(Ⅴ) was 0.4 A, whereas the current for the determination of As(Ⅲ) and As(Ⅴ) was 1.2 A. For equal concentrations of As(Ⅲ) and As(Ⅴ) in a sample, the interferences of As(Ⅴ) during the As(Ⅲ) determination were smaller than 5%. The absorbance for As(Ⅴ) could be calculated by subtracting that for As(Ⅲ) measured at 0.4 A from the total absorbance for As(Ⅲ) and As(Ⅴ) measured at 1.2 A, and then the concentration of As(Ⅴ) can be obtained by its calibration curve at 1.2 A. The methodology developed provided the detection limits of 0.3 and 0.6 ng·mL^-1 for As(Ⅲ) and As(Ⅴ), respectively. The relative standard deviations were of 3.5% for 20 ng·mL^-1 As(Ⅲ) and 3.2% for 20 ng·mL^-1 As(Ⅴ). The method was successfully applied to determination of soluble inorganic arsenic species in Chinese medicine.展开更多
An innovative method for the ultrasensitive detection of mercury by solution anode glow discharge atomic emission spectroscopy(SAGD-AES) coupled with hydride generation(HG) was first investigated.In this method,the me...An innovative method for the ultrasensitive detection of mercury by solution anode glow discharge atomic emission spectroscopy(SAGD-AES) coupled with hydride generation(HG) was first investigated.In this method,the mercury vapor generated by the HG was transmitted to the SAGD through the miniature hollow tungsten tube for excitation and detected by a miniaturized spectrograph.A thorough parametric evaluation of the HG and SAGD system was performed,including the type and concentration of ca rrier acid,He flow rate,concentrations of NaBH4,discha rge current and discharge gap.Under optimal operating conditions,the detection limit for Hg^(2+) achieved 0.03 μg/L,with a relative standard deviation of 1.1% at the Hg^(2+) concentration of 5 μg/L.Moreover,the correlation coefficient of the calibration curve was 0.9996 in the range between 0.1 and 10 μg/L.The accuracy and practicability of HG-SAGD-AES were verified by measuring GBW09101 b(human hair),GBW10029(fish),soil and rice samples.The results showed good agreement with the certified values and values from direct mercury analyzer(DMA).展开更多
Flue gas from coal combustion contains significant amounts of volatile selenium (Se). The capture of Se in the flue gas desulfurization (FGD) scrubber unit has resulted in a generation of metal-laden residues. It ...Flue gas from coal combustion contains significant amounts of volatile selenium (Se). The capture of Se in the flue gas desulfurization (FGD) scrubber unit has resulted in a generation of metal-laden residues. It is important to determine Se speciation to understand the environmental impact of its disposal. A simple method has been developed for selective inorganic Se(IV), Se(VI) and organic Se determination in the liquid-phase FGD residues by hydride generation atomic fluorescence spectrometry (AFS). It has been determined that Se(IV), Se(VI) and organic Se can be accurately determined with detection limits (DL) of 0.05, 0.06 and 0.06 μg/L, respectively. The accuracy of the proposed method was evaluated by analyzing the certified reference material, NIST CRM 1632c, and also by analyzing spiked tap-water samples. Analysis indicates that the concentration of Se is high in FGD liquid residues and primarily exists in a reduced state as selenite (Se(IV)). The toxicity of Se(IV) is the strongest of all Se species. Flue gas desulfurization residues pose a serious environmental risk.展开更多
A novel adsorbent was developed by coating yttrium hydroxide precipitate layer on cellulose fibre. This material takes up ca. 98% of 5 μg·L 1 As(Ⅲ) and As(V) at low pH (pH〈7), while a favorable selectivi...A novel adsorbent was developed by coating yttrium hydroxide precipitate layer on cellulose fibre. This material takes up ca. 98% of 5 μg·L 1 As(Ⅲ) and As(V) at low pH (pH〈7), while a favorable selectivity for As(V) was achieved within pH 11--12. In practice, a mini-column packed with Y(OH)3 precipitate layer coated cellulose fibre particles was incorporated into a sequential injection system for selective uptake of arsenate at pH 11.5. The retained arsenate was afterwards recovered with 50μL of 0.8 mol.L l NaOH solution as eluent, followed by hydride generation in a reaction medium of 2.0 mol·L-1 HCl and 1.0% NaBH4 solution (W/V, in 0.5% NaOH) after pre-reduction of arsenate to arsenite by KI-ascorbic acid (5%, W/V), with detection by atomic fluorescence spec- trometry. Total inorganic arsenic was quantitatively taken up at pH 6.0 by following the same procedure and arsenic speciation was performed by difference. With a sample volume of 1.0 mL, an enrichment factor of 16.4 was derived with a detection limit of 17 ng.L-1 within a linear range of 0.05--2.0μg.L ]. A relative standard deviation (RSD) of 2.6% (0.5 μg·L-1, n= 11) was achieved. The procedure was validated by analyzing arsenic in a certified refer- ence material GBW 09101 (human hair), and speciation process requires no organic solvents, thus Y(OH)3 coated of inorganic arsenic in natural water samples. The entire cellulose fibre provides a green adsorbent.展开更多
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On-line ion-exchange separation and preconcentration were combined with flow-injection hydride generation atomic absorption spectrometry (HGAAS) to determine ultra-trace amounts of antimony in water samples. Antimony(Ⅲ) was preconcentrated on a micro-column packed with CPG-8Q chelating ion-exchanger using time-based sample loading and eluted by 4 mol l^(-1) HCl directly into the hydride generation AAS system. A detection limit (3σ) of 0.0015μg l^(-1) Sb(Ⅲ) was obtained on the basis of a 20 fold enrichment and with a sampling frequency of 60h^(-1). The precision was 1.0% r.s.d.(n=11) at the 0.5μg l^(-1) Sb(Ⅲ) level. Recoveries for the analysis of antimony in tap water, snow water and sea water samples were in the range 97-102%.
文摘A continuous phosphine (PH3) generation was developed and applied to the sensitive detection of phosphorus by ICP-AES. Phosphate ion in aqueous solution was converted to phosphine by passing the sample solution through an incandescent copper silica-tube. Detection limit is 2 ng/mL. The relative standard deviation is 4.2% for 20 ng/mL. The method is rapid and simple with low contamination and high sensitivity.
文摘A sensitive atomic spectrometric method for the redox speciation analysis of Sb in water is described. The proposed method is based on the selective generation of stibine from Sb(III) in a continuous flow system using non-dispersive atomic fluorescence spectrometry for detection. The effects of the HCI concentration on the fluorescence intensities of Sb(III) and Sb(V) were investigated. The results indicated that atomic fluorescence emission due to Sb(V) can constructively interfere with the determination of Sb(III). For the determination of Sb(III), four compounds were tested as masking agents to inhibit the generation of stibine from Sb(V). The effects of the concentrations of the masking agents and of HC1 on the fluorescence signals from Sb(III) and Sb(V) were studied. The results indicated that citric acid and NaF can successfully suppress hydride generation from Sb(V). To evaluate the developed methodology and the influence of the matrix, the recovery of Sb(III) from natural water that was spiked with different Sb(III) and Sb(V) concentrations was tested.
基金Project supported by the National Natural Science Foundation of China (No. 20173004).
文摘A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry (EcHG-AAS) with selective electrochemical reduction. The determination of inorganic arsenic species is based on the fact that As(Ⅲ) shows significantly higher absorbance at low electrolytic currents than As(Ⅴ) in 0.3 mol·L^-1 H2SO4. The electrolytic current used for the determination of As(Ⅲ) without considerable interferences of As(Ⅴ) was 0.4 A, whereas the current for the determination of As(Ⅲ) and As(Ⅴ) was 1.2 A. For equal concentrations of As(Ⅲ) and As(Ⅴ) in a sample, the interferences of As(Ⅴ) during the As(Ⅲ) determination were smaller than 5%. The absorbance for As(Ⅴ) could be calculated by subtracting that for As(Ⅲ) measured at 0.4 A from the total absorbance for As(Ⅲ) and As(Ⅴ) measured at 1.2 A, and then the concentration of As(Ⅴ) can be obtained by its calibration curve at 1.2 A. The methodology developed provided the detection limits of 0.3 and 0.6 ng·mL^-1 for As(Ⅲ) and As(Ⅴ), respectively. The relative standard deviations were of 3.5% for 20 ng·mL^-1 As(Ⅲ) and 3.2% for 20 ng·mL^-1 As(Ⅴ). The method was successfully applied to determination of soluble inorganic arsenic species in Chinese medicine.
基金the Instrument Development Project of the Chinese Academy of Sciences(No.YZ201539)the National Natural Science Foundation of China(No.21175145)Shanghai Technical Platform for Testing on Inorganic Materials(No.19DZ2290700)。
文摘An innovative method for the ultrasensitive detection of mercury by solution anode glow discharge atomic emission spectroscopy(SAGD-AES) coupled with hydride generation(HG) was first investigated.In this method,the mercury vapor generated by the HG was transmitted to the SAGD through the miniature hollow tungsten tube for excitation and detected by a miniaturized spectrograph.A thorough parametric evaluation of the HG and SAGD system was performed,including the type and concentration of ca rrier acid,He flow rate,concentrations of NaBH4,discha rge current and discharge gap.Under optimal operating conditions,the detection limit for Hg^(2+) achieved 0.03 μg/L,with a relative standard deviation of 1.1% at the Hg^(2+) concentration of 5 μg/L.Moreover,the correlation coefficient of the calibration curve was 0.9996 in the range between 0.1 and 10 μg/L.The accuracy and practicability of HG-SAGD-AES were verified by measuring GBW09101 b(human hair),GBW10029(fish),soil and rice samples.The results showed good agreement with the certified values and values from direct mercury analyzer(DMA).
基金supported by the National Natural Science Foundation of China (No.90410018)the Shanxi Nature Science Foundation (No.20051017)+1 种基金the Shanxi Returned Scholar Research Project (No.2005-21)the Programfor Changjiang Scholars and Innovative Research Team at University in MOE,China (No.IRT0517)
文摘Flue gas from coal combustion contains significant amounts of volatile selenium (Se). The capture of Se in the flue gas desulfurization (FGD) scrubber unit has resulted in a generation of metal-laden residues. It is important to determine Se speciation to understand the environmental impact of its disposal. A simple method has been developed for selective inorganic Se(IV), Se(VI) and organic Se determination in the liquid-phase FGD residues by hydride generation atomic fluorescence spectrometry (AFS). It has been determined that Se(IV), Se(VI) and organic Se can be accurately determined with detection limits (DL) of 0.05, 0.06 and 0.06 μg/L, respectively. The accuracy of the proposed method was evaluated by analyzing the certified reference material, NIST CRM 1632c, and also by analyzing spiked tap-water samples. Analysis indicates that the concentration of Se is high in FGD liquid residues and primarily exists in a reduced state as selenite (Se(IV)). The toxicity of Se(IV) is the strongest of all Se species. Flue gas desulfurization residues pose a serious environmental risk.
文摘A novel adsorbent was developed by coating yttrium hydroxide precipitate layer on cellulose fibre. This material takes up ca. 98% of 5 μg·L 1 As(Ⅲ) and As(V) at low pH (pH〈7), while a favorable selectivity for As(V) was achieved within pH 11--12. In practice, a mini-column packed with Y(OH)3 precipitate layer coated cellulose fibre particles was incorporated into a sequential injection system for selective uptake of arsenate at pH 11.5. The retained arsenate was afterwards recovered with 50μL of 0.8 mol.L l NaOH solution as eluent, followed by hydride generation in a reaction medium of 2.0 mol·L-1 HCl and 1.0% NaBH4 solution (W/V, in 0.5% NaOH) after pre-reduction of arsenate to arsenite by KI-ascorbic acid (5%, W/V), with detection by atomic fluorescence spec- trometry. Total inorganic arsenic was quantitatively taken up at pH 6.0 by following the same procedure and arsenic speciation was performed by difference. With a sample volume of 1.0 mL, an enrichment factor of 16.4 was derived with a detection limit of 17 ng.L-1 within a linear range of 0.05--2.0μg.L ]. A relative standard deviation (RSD) of 2.6% (0.5 μg·L-1, n= 11) was achieved. The procedure was validated by analyzing arsenic in a certified refer- ence material GBW 09101 (human hair), and speciation process requires no organic solvents, thus Y(OH)3 coated of inorganic arsenic in natural water samples. The entire cellulose fibre provides a green adsorbent.