Water-soluble rare earth elements (WSREEs) of four typical soil profiles in China were determined by using a high-resolution inductively coupled plasma mass spectrometer. Results showed that the contents of WSREEs dec...Water-soluble rare earth elements (WSREEs) of four typical soil profiles in China were determined by using a high-resolution inductively coupled plasma mass spectrometer. Results showed that the contents of WSREEs decreased from upper layer to lower layer of soils in the southern part of China with a high rainfall and low pH but increased for soils in the northern part of China with a low rainfall and relatively higher pH. Contents of WSREEs in soils were lower than 100 μg kg-1 in most casest and varied greatly with both different soils and different layers of the same profile. The highest content was 2816.3 μg kg-1 but the lowest was 17.6 μg kg-1 only. The content of individual rare earth iement (REE) in the soil solution also varied greatly with the highest one ranging from 8.4 to 1373 μg kg-1 for Ce and the lowest one from 0.05to 4.48 μg kg-1 for Lu. The sum of WSREEs in the first soil layers ranged from 121.5 to 345.6 μg kg-1.Great variations existed among ratios of REEs extracted with water to the total REEs of soils, ranging from 0.02×10-3 to 13.2×10-3. But as the upper layer was considered, the ratio showed only a small difference,ranging from 0.79×10-3 to 1.69×10-3.展开更多
A novel ambient negative corona discharge ion source with mini line-cylinder electrodes is designed. The diameters of inner and outer electrode are 0.16 and 4 mm respectively. With a special assembly method, a perfect...A novel ambient negative corona discharge ion source with mini line-cylinder electrodes is designed. The diameters of inner and outer electrode are 0.16 and 4 mm respectively. With a special assembly method, a perfect coaxiality of the two electrodes is obtained. An injection system utilizing a temperature control technique, achieves a constant and stable concentration of the sample, which is critical to the experiment. The formulas of the corona onset voltage of line-cylinder electrodes are also introduced. The experiment results show that negative substances such as formic acid and acetic acid can be ionized under ambient conditions. When combined with micro electrical mechanical system fabricationprocess, the volume of the ion source can be reduced dramatically, but there is an undesirable surface discharge. To solve the surface discharge problem, an improved structure was designed and tested. The simplicity of the interface of the ion source makes it suitable for mass spectrometer, micro mass spectrometer, ion mobility spectrometer, and high-field asymmetric waveform ion mobility spectrometer applications.展开更多
For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluores...For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluorescence detection. Quinolone antibiotics were separated by Dionex OmniPac PAX-500 column with an eluent of 15 mmol/L H2SO4 and 35% methanol （v/v） at a flow-rate of 1.0 ml/min and detected with fluorescence with excitation and emission wave lengths of 347 ran and 420 ran respectively. The detection limits （S/N=3） of norfloxacin, ciprofloxacin and enoxacin were 50, 105 and 80 ng/ml respectively. The relative standard deviations of retention time, peak area and peak height were less than 1.1% and good linear relationship resulted. The developed method was applied to pharmaceutical formulations and biological fluids.展开更多
Aerosol samples of PM10 (particulate matter with aerodynamic diameters less than 10μm) and TSP (total suspended particles) were simultaneously collected from April 2001 to March 2002 at the top of Mount Baguan on the...Aerosol samples of PM10 (particulate matter with aerodynamic diameters less than 10μm) and TSP (total suspended particles) were simultaneously collected from April 2001 to March 2002 at the top of Mount Baguan on the downtown campus of Ocean University of China, Qingdao, China. The concentrations of Al, Fe, Mn, Cu, Pb and Zn were determined by means of inductively coupled plasma atomic emission spectrometry (ICP-AES). The monthly variability of the mass concentrations of aerosol particles and the concentrations of trace metals are presented and discussed. The distribution pattern of these metals in PM10 and TSP is also discussed. During the observation period, the mass concentration of PM10 at this site ranged from 13.80 to 306.42μgm-3 , while that of TSP ranged from 31.02 to 568.82μgm-3. Both PM10 and TSP reached their highest concentrations in springtime, while the lowest values occurred in summertime. The concentrations of crustal metals followed the same variation pattern, while those of anthropogenic metals did not. A closer examination led to the conclusion that anthropogenic metals are mainly from local sources. The average concentration ratios of anthropogenic metals in PM10 to TSP were higher than the average mass ratio of PM10 to TSP, suggesting that there was a higher proportion of anthropogenic metals on smaller particles although there were a few exceptions. For crustal metals, however, the metal concentration ratios were close to the particle mass ratio, indicating that the distribution of crustal metals was much more homogeneous on aerosol particles with different sizes. The correlation analysis indicated that Al, Fe and Mn were originated from similar sources and were mainly controlled by the particle mass, while Cu, Pb and Zn were predominated by local anthropogenic sources, with Pb and Zn having similar origins.展开更多
Digestion with aqua regia in a Carius tube and separation of Re with anion exchange resin is commonly employed for Re–Os dating of molybdenite and pyrite.However, the recovery of Re is extremely low when this routine...Digestion with aqua regia in a Carius tube and separation of Re with anion exchange resin is commonly employed for Re–Os dating of molybdenite and pyrite.However, the recovery of Re is extremely low when this routine anion exchange method is applied to galena,causing difficulty in Re–Os dating of galena. In this study,we investigated the mechanism of Re loss during sample preparation and tested a revised procedure for Re–Os dating of galena and sphalerite.展开更多
In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a stron...In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a [R+] [BiI4-] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called 搕hin-layer resin phase?or 搑esin phase? and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer抯 law over the concentration range 0.01ug/ml^1.20ug/ml of bismuthous(III). It has a molar absorptivity of 7.1×105 [L/mol穋m]. It indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the measurements of 0.5ug/ml Bi(III). The detection limit of Bismuthous(III) is 1.4×10-8mol/L. The method has applied to the analysis Bi(III) in environmental water samples.展开更多
A reliable method for detecting nanoparticles is necessary for the wide application of nanomaterials. Single particle-inductively coupled plasma mass spectrometry(SP-ICP-MS) was investigated to detect the size of gold...A reliable method for detecting nanoparticles is necessary for the wide application of nanomaterials. Single particle-inductively coupled plasma mass spectrometry(SP-ICP-MS) was investigated to detect the size of gold nanoparticles(Au NPs) in this work. Discrimination of particle signal and iterative algorithm were used to calculate the baseline of particle signal. Influence of dwell time was discussed and 3 ms was selected as dwell time for size detection. Different Au NPs standards(30, 60, 80 and 100 nm) and mixed samples(60 and 100 nm) were determined by SP-ICP-MS and the accuracy was confirmed with reference values. The particle size detection limit was 19 nm in ultrapure water(UP water) and 31 nm in 0.1 μg/L Au^(3+) solution. Stability of Au NPs in ultrapure water and natural water samples was investigated by detecting size variation of AuN Ps. The result shows that Au NPs are stable in aqueous environment for 6 d but degraded after 30 d.展开更多
文摘Water-soluble rare earth elements (WSREEs) of four typical soil profiles in China were determined by using a high-resolution inductively coupled plasma mass spectrometer. Results showed that the contents of WSREEs decreased from upper layer to lower layer of soils in the southern part of China with a high rainfall and low pH but increased for soils in the northern part of China with a low rainfall and relatively higher pH. Contents of WSREEs in soils were lower than 100 μg kg-1 in most casest and varied greatly with both different soils and different layers of the same profile. The highest content was 2816.3 μg kg-1 but the lowest was 17.6 μg kg-1 only. The content of individual rare earth iement (REE) in the soil solution also varied greatly with the highest one ranging from 8.4 to 1373 μg kg-1 for Ce and the lowest one from 0.05to 4.48 μg kg-1 for Lu. The sum of WSREEs in the first soil layers ranged from 121.5 to 345.6 μg kg-1.Great variations existed among ratios of REEs extracted with water to the total REEs of soils, ranging from 0.02×10-3 to 13.2×10-3. But as the upper layer was considered, the ratio showed only a small difference,ranging from 0.79×10-3 to 1.69×10-3.
基金ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China （No.60706030 and No.20827007）, the National High Technology Research and Development Plan of China （No.2007AA 04Z337） and the State Key Laboratory Fund （No.9140 C12040506060C12）.
文摘A novel ambient negative corona discharge ion source with mini line-cylinder electrodes is designed. The diameters of inner and outer electrode are 0.16 and 4 mm respectively. With a special assembly method, a perfect coaxiality of the two electrodes is obtained. An injection system utilizing a temperature control technique, achieves a constant and stable concentration of the sample, which is critical to the experiment. The formulas of the corona onset voltage of line-cylinder electrodes are also introduced. The experiment results show that negative substances such as formic acid and acetic acid can be ionized under ambient conditions. When combined with micro electrical mechanical system fabricationprocess, the volume of the ion source can be reduced dramatically, but there is an undesirable surface discharge. To solve the surface discharge problem, an improved structure was designed and tested. The simplicity of the interface of the ion source makes it suitable for mass spectrometer, micro mass spectrometer, ion mobility spectrometer, and high-field asymmetric waveform ion mobility spectrometer applications.
基金Project supported by the National Natural Science Foundation of China (Nos.20375035 and 20527005)the Natural Science Foundation of Zhejiang Province (No.Z404105), China
文摘For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluorescence detection. Quinolone antibiotics were separated by Dionex OmniPac PAX-500 column with an eluent of 15 mmol/L H2SO4 and 35% methanol （v/v） at a flow-rate of 1.0 ml/min and detected with fluorescence with excitation and emission wave lengths of 347 ran and 420 ran respectively. The detection limits （S/N=3） of norfloxacin, ciprofloxacin and enoxacin were 50, 105 and 80 ng/ml respectively. The relative standard deviations of retention time, peak area and peak height were less than 1.1% and good linear relationship resulted. The developed method was applied to pharmaceutical formulations and biological fluids.
基金supported by the National Natural Science Foundation of China(Grant No.49976020).
文摘Aerosol samples of PM10 (particulate matter with aerodynamic diameters less than 10μm) and TSP (total suspended particles) were simultaneously collected from April 2001 to March 2002 at the top of Mount Baguan on the downtown campus of Ocean University of China, Qingdao, China. The concentrations of Al, Fe, Mn, Cu, Pb and Zn were determined by means of inductively coupled plasma atomic emission spectrometry (ICP-AES). The monthly variability of the mass concentrations of aerosol particles and the concentrations of trace metals are presented and discussed. The distribution pattern of these metals in PM10 and TSP is also discussed. During the observation period, the mass concentration of PM10 at this site ranged from 13.80 to 306.42μgm-3 , while that of TSP ranged from 31.02 to 568.82μgm-3. Both PM10 and TSP reached their highest concentrations in springtime, while the lowest values occurred in summertime. The concentrations of crustal metals followed the same variation pattern, while those of anthropogenic metals did not. A closer examination led to the conclusion that anthropogenic metals are mainly from local sources. The average concentration ratios of anthropogenic metals in PM10 to TSP were higher than the average mass ratio of PM10 to TSP, suggesting that there was a higher proportion of anthropogenic metals on smaller particles although there were a few exceptions. For crustal metals, however, the metal concentration ratios were close to the particle mass ratio, indicating that the distribution of crustal metals was much more homogeneous on aerosol particles with different sizes. The correlation analysis indicated that Al, Fe and Mn were originated from similar sources and were mainly controlled by the particle mass, while Cu, Pb and Zn were predominated by local anthropogenic sources, with Pb and Zn having similar origins.
基金supported by the 12th Five-Year Plan Project of State Key Laboratory of Ore Deposit Geochemistry, Chinese Academy of Sciences (SKLODG-ZY125-09 SKLODGZY125-02)+1 种基金the National Natural Science Foundation of China (Nos. 41373064 41430315)
文摘Digestion with aqua regia in a Carius tube and separation of Re with anion exchange resin is commonly employed for Re–Os dating of molybdenite and pyrite.However, the recovery of Re is extremely low when this routine anion exchange method is applied to galena,causing difficulty in Re–Os dating of galena. In this study,we investigated the mechanism of Re loss during sample preparation and tested a revised procedure for Re–Os dating of galena and sphalerite.
文摘In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a [R+] [BiI4-] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called 搕hin-layer resin phase?or 搑esin phase? and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer抯 law over the concentration range 0.01ug/ml^1.20ug/ml of bismuthous(III). It has a molar absorptivity of 7.1×105 [L/mol穋m]. It indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the measurements of 0.5ug/ml Bi(III). The detection limit of Bismuthous(III) is 1.4×10-8mol/L. The method has applied to the analysis Bi(III) in environmental water samples.
基金Projects(21407182,21277175)supported by the National Natural Science Foundation of ChinaProject(20120162110019)supported by the Specialized Research Fund for the Doctoral Program of Higher Education of China
文摘A reliable method for detecting nanoparticles is necessary for the wide application of nanomaterials. Single particle-inductively coupled plasma mass spectrometry(SP-ICP-MS) was investigated to detect the size of gold nanoparticles(Au NPs) in this work. Discrimination of particle signal and iterative algorithm were used to calculate the baseline of particle signal. Influence of dwell time was discussed and 3 ms was selected as dwell time for size detection. Different Au NPs standards(30, 60, 80 and 100 nm) and mixed samples(60 and 100 nm) were determined by SP-ICP-MS and the accuracy was confirmed with reference values. The particle size detection limit was 19 nm in ultrapure water(UP water) and 31 nm in 0.1 μg/L Au^(3+) solution. Stability of Au NPs in ultrapure water and natural water samples was investigated by detecting size variation of AuN Ps. The result shows that Au NPs are stable in aqueous environment for 6 d but degraded after 30 d.
