The contents ofMg, Al, Si, Ti, Cr, Mn, Fe, Co, Cu, Ga, As, Se, Cd, Sb, Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS）. The sample was diss...The contents ofMg, Al, Si, Ti, Cr, Mn, Fe, Co, Cu, Ga, As, Se, Cd, Sb, Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS）. The sample was dissolved in HNO3 and HCI by microwave digestion. Most of the spectral interferences could be avoided by measuring in the high resolution mode. The matrix effects because of the presence of excess HC1 and nickel were evaluated. Correction for matrix effects was made using Sc, Rh and T1 as internal standards. The optimum conditions for the determination were tested and discussed. The detection limits range from 0.012 to 1.76 ~tg/g depending on the type of elements. The applicability of the proposed method is also validated by the analysis of high purity nickel reference material （NIST SRM 671）. The relative standard deviation （RSD） is less than 3.3%. Results for determination of trace elements in high purity nickel were presented.展开更多
The contents of Cr, Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method. The sample digestions were performed in closed microwave vessels with...The contents of Cr, Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method. The sample digestions were performed in closed microwave vessels with HNO3, HClO4 and FIE The optimum conditions for the determination were obtained. The applicability of the proposed method was validated by the analysis of coal fly ash reference material （NIST SRM 1633a）. The results show that most of the spectral interferences can be avoided by measuring in the high resolution mode （maximum mass resolution R=9 000）. The detection limit is from 0.05 to 0.21 μg/g, and the precision is fine with relative standard deviation less than 4.3%.展开更多
An analytical method, using sector field inductively coupled plasma mass spectrometry （SF-ICP-MS） for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in e...An analytical method, using sector field inductively coupled plasma mass spectrometry （SF-ICP-MS） for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in electrolytic manganese metal, was described. At the beginning, the samples were decomposed by HNO3 and H2504, and then analyzed by SF-ICP-MS. Most of the spectral interferences could be avoided by measuring in different mass resolution modes. The matrix effects due to the excess of sulfuric acid and Mn were evaluated. Correction of matrix effects was conducted by using the internal standard elements. The optimum condition for the determination was investigated and discussed. The detection limit is in the range of 0.001-0.169 gg/L. The current method is applied to the determination of trace impurities in electrolytic manganese metal. And experiments show that good results can be obtained much faster, more accurately and conveniently by current method.展开更多
An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+H...An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system(ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching,and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of0.9-37.5 ng/L, the relative standard deviation of each element is within 1.1%-4.8%, and the recovery of each element is 90%-108%.展开更多
OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain,which causes hypoxia or ischemia in some areas.This work aimed to quantify the minerals and heavy metals in Qishiwei Zhen...OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain,which causes hypoxia or ischemia in some areas.This work aimed to quantify the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro,analyze its effect on the types and abundance of intestinal flora,and study its mechanism on inflammation and apoptosis pathways as a treatment for cerebral ischemia.METHODS Microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS)were used to determine the minerals and heavy metals in 10 batches of Qishiwei Zhenzhu pill in vitro.With the use of the middle cerebral artery obstruction(MCAO)model,ICP-MS was applied to determine the content of minerals and heavy metals in hepatic portal vein blood,abdominal aortic blood,brain,liver,kidney,hair,urine and feces at different time periods.On this model,the ileum,cecum,and colon tissues were tested for intestinal pathology,and 16S rRNA was used for sequencing.Species taxonomy,αdiversity,and species microbial composition and structure analysis were also performed.Polymerase chain reaction and Western blotting were employed to determine the mRNA and protein expression of p38 MAPK,caspase-3,IL^(-1)βand TNF-αin the ischemic brain tissues of rats.RESULTS The average content of heavy metals in the 10 batches of Qishiwei Zhenzhu pill samples is in the descending order Hg>Cu>Pb.Significant differences in the metal elements are found among Qishiwei Zhenzhu pill from different manufacturers but not among the different batches of the same manufacturer.An extremely low content of heavy metals are absorbed into the blood or accumulated in the brain,liver,kidney,and other tissues.Stool is the main excretion route of minerals and heavy metals from Qishiwei Zhenzhu pill.This medicine helps repair the intestinal mucosa in MCAO rats.At the phylum level,it can regulate the abundance of Firmicutes and Proteobacteria in the intestinal flora of rats with cerebral ischemia.At the genus level,it can adjust the abundance of Escherichia Shigella.At the species level,it can adjust the abundance of Lactobacillus yoelii and Lactobacillus reuteri.Cluster classification results show that Qishiwei Zhenzhu pill can improve the intestinal flora of rats with cerebral ischemia,reduce the mRNA and protein expression of caspase-3 and IL^(-1)βin rat brain tissues,and have a tendency to decrease the mRNA expression of p38 MAPK and TNF-α.CONCLUSION Quantifying the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro will help improve their quality standards.Minerals and heavy metals are mainly excreted in feces,accumulate in extremely low levels in various tissues,and do not damage the intestinal mucosa.The effective material basis of Qishiwei Zhenzhu pill in treating cerebral ischemia may be related to their Li,Cr,and Cd elements.These pills can improve the environment of intestinal flora,and their mechanism of treatment for cerebral ischemia may be related to the down-regulation of IL^(-1)βinflammatory factor and inhibition of cell apoptosis.展开更多
In this paper,the determination of six heavy metal ions (arsenic,lead,cadmium,chromium,mercury and nickel) in the Chinese Herb by inductively coupled plasma-mass spectrometry (ICP-MS) was studied.The samples were dige...In this paper,the determination of six heavy metal ions (arsenic,lead,cadmium,chromium,mercury and nickel) in the Chinese Herb by inductively coupled plasma-mass spectrometry (ICP-MS) was studied.The samples were digested by nitric acid and hydrogen peroxide in a microwave oven.The Sc,Y,In,Bi were added as internal standards to eliminate the matrix interferences.The results show that most of the relative standard deviations of these trace elements were below 3.5%,the standard recoveries of these elements were in the range of 91%-107%,and the detection limits were in the range of 0.001-0.006 μg·L-1. This method is accurate,rapid,convenience,and can be applied to the determination of arsenic,lead,cadmium,chromium,mercury and nickel in Chinese Herb with good results.展开更多
Inductively coupled plasma mass spectrometry(ICP-MS) was used to determine the concentration of Pb in atmospheric particulate samples,and the enrichment factor was calculated.The causes of the results were also discus...Inductively coupled plasma mass spectrometry(ICP-MS) was used to determine the concentration of Pb in atmospheric particulate samples,and the enrichment factor was calculated.The causes of the results were also discussed.展开更多
Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pr...Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pressure and working temperature. The etching process of Si3N4 is studied by inductively coupled plasma (ICP) with a gas mixture of SF6 and O2. The influence of the technique parameters, such as ICP power, DC bias, gas composition, total flow rate, on the etching selectivity of Si3N4/EPG533 which is used as a mask layer and the etching rate of Si3N4 is studied, in order to get a better etching selectivity of Si3N4/EPG533 with a faster etching rate of Si3N4. The optimized process parameters of etching Si3N4 by ICP are obtained after a series of experiments and analysis. Under the conditions of total ICP power of 250 W, DC bias of 50W, total flow rate of 40 sccm and O2 composition of 30%, the etching selectivity of 2.05 can be reached when Si3N4 etching rate is 336 nm/min.展开更多
Concentration of heavy metals in blood and urine of rabbit after inhaling three different kinds of cigarette was studied through the animal passive smoking pattern. The samples were prepared by nitric acid solution di...Concentration of heavy metals in blood and urine of rabbit after inhaling three different kinds of cigarette was studied through the animal passive smoking pattern. The samples were prepared by nitric acid solution digestion and determination of seven kinds of heavy metals including Hg, Se, Sn, Pb, Cd, Ni and Cr was performed by inductively coupled plasma-atomic emission spectrometry （ICP-AES）. The ICP-AES method was established with good precision and accuracy, relative standard deviation （n=6） was between 2.9% and 5.9%, and the recovery was in the range of 95.0%-104.2%. Concentration of six heavy metals increases in some extent in blood and urine after period of smoking and the increasing of heavy metals in blood and urine all shows time dependence. Significantly higher heavy metal levels are observed in the blood and urine of the cigarette inhaling rabbits in the exposed group. The concentration of six kinds of heavy metals in the blood of the rabbit increases after 16 weeks exposing to cigarette smoking. Three times of rig, ten times of Se and trace amount ofPb, Cd, Ni and Cr are detected in the blood after 16 weeks of smoking. For urine samples, about three times of Hg, two times of Se, five times of Pb and trace amount of Cd are detected after 16 weeks of inhalation of cigarette. Comparatively, higher concentration of heavy metals are detected after inhaling of Nise cigarette.展开更多
A method was developed for the simultaneous determination of seven trace impurities (Cd, Mn, Pb, Zn, Cu, Fe and Ni) in high purity cobalt oxide by ICP AES. The matrix effect was eliminated by preci pitation with 1 nit...A method was developed for the simultaneous determination of seven trace impurities (Cd, Mn, Pb, Zn, Cu, Fe and Ni) in high purity cobalt oxide by ICP AES. The matrix effect was eliminated by preci pitation with 1 nitroso 2 naphthol. The matrix effect of cobalt on the absorptions of trace impurities, the effects of reaction time, pH value, dosage of precipitant on the formation of cobalt 1 nitroso 2 naphthol complex, the effects of hydrochloric acid on the stability of this complex and masking of elements were studied. Recoveries of the impurities in spiked sample are from 90% to 110% with a precision of 1.1% 5.0% RSD. The detection limits of the seven elements are in the range of 0.01 0.24μg/g. The method can be applied to the analysis of high purity cobalt metal, cobalt oxide and other cobalt compounds.展开更多
基金Project(21075138) supported by the National Natural Science Foundation of ChinaProject(cstc2011jjA0780) supported by Natural Science Foundation of Chongqing City,ChinaProject(KJ121311) supported by Educational Commission of Chongqing City of China
文摘The contents ofMg, Al, Si, Ti, Cr, Mn, Fe, Co, Cu, Ga, As, Se, Cd, Sb, Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS）. The sample was dissolved in HNO3 and HCI by microwave digestion. Most of the spectral interferences could be avoided by measuring in the high resolution mode. The matrix effects because of the presence of excess HC1 and nickel were evaluated. Correction for matrix effects was made using Sc, Rh and T1 as internal standards. The optimum conditions for the determination were tested and discussed. The detection limits range from 0.012 to 1.76 ~tg/g depending on the type of elements. The applicability of the proposed method is also validated by the analysis of high purity nickel reference material （NIST SRM 671）. The relative standard deviation （RSD） is less than 3.3%. Results for determination of trace elements in high purity nickel were presented.
基金Project (04JJ40016) supported by the Natural Science Foundation of Hunan Province, China
文摘The contents of Cr, Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method. The sample digestions were performed in closed microwave vessels with HNO3, HClO4 and FIE The optimum conditions for the determination were obtained. The applicability of the proposed method was validated by the analysis of coal fly ash reference material （NIST SRM 1633a）. The results show that most of the spectral interferences can be avoided by measuring in the high resolution mode （maximum mass resolution R=9 000）. The detection limit is from 0.05 to 0.21 μg/g, and the precision is fine with relative standard deviation less than 4.3%.
基金Project(21075138)supported by the National Natural Science Foundation of ChinaProject(cstc2013jcyjA10088)supported by Chongqing Natural Science Foundation,ChinaProject(KJ121311)supported by Scientific and Technological Research Program of Chongqing Municipal Education Commission,China
文摘An analytical method, using sector field inductively coupled plasma mass spectrometry （SF-ICP-MS） for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in electrolytic manganese metal, was described. At the beginning, the samples were decomposed by HNO3 and H2504, and then analyzed by SF-ICP-MS. Most of the spectral interferences could be avoided by measuring in different mass resolution modes. The matrix effects due to the excess of sulfuric acid and Mn were evaluated. Correction of matrix effects was conducted by using the internal standard elements. The optimum condition for the determination was investigated and discussed. The detection limit is in the range of 0.001-0.169 gg/L. The current method is applied to the determination of trace impurities in electrolytic manganese metal. And experiments show that good results can be obtained much faster, more accurately and conveniently by current method.
基金Project(21271187)supported by the National Natural Science Foundation of ChinaProject(cstc2013jcyj A10088)supported by the Chongqing Natural Science Foundation,China+1 种基金Projects(2013FJ3093,2013SK3268)supported by the Science and Technology Project of Hunan Province,ChinaProject(KJZH14217)supported by Achievement Transfer Education in Chongqing,China
文摘An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system(ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching,and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of0.9-37.5 ng/L, the relative standard deviation of each element is within 1.1%-4.8%, and the recovery of each element is 90%-108%.
文摘OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain,which causes hypoxia or ischemia in some areas.This work aimed to quantify the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro,analyze its effect on the types and abundance of intestinal flora,and study its mechanism on inflammation and apoptosis pathways as a treatment for cerebral ischemia.METHODS Microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS)were used to determine the minerals and heavy metals in 10 batches of Qishiwei Zhenzhu pill in vitro.With the use of the middle cerebral artery obstruction(MCAO)model,ICP-MS was applied to determine the content of minerals and heavy metals in hepatic portal vein blood,abdominal aortic blood,brain,liver,kidney,hair,urine and feces at different time periods.On this model,the ileum,cecum,and colon tissues were tested for intestinal pathology,and 16S rRNA was used for sequencing.Species taxonomy,αdiversity,and species microbial composition and structure analysis were also performed.Polymerase chain reaction and Western blotting were employed to determine the mRNA and protein expression of p38 MAPK,caspase-3,IL^(-1)βand TNF-αin the ischemic brain tissues of rats.RESULTS The average content of heavy metals in the 10 batches of Qishiwei Zhenzhu pill samples is in the descending order Hg>Cu>Pb.Significant differences in the metal elements are found among Qishiwei Zhenzhu pill from different manufacturers but not among the different batches of the same manufacturer.An extremely low content of heavy metals are absorbed into the blood or accumulated in the brain,liver,kidney,and other tissues.Stool is the main excretion route of minerals and heavy metals from Qishiwei Zhenzhu pill.This medicine helps repair the intestinal mucosa in MCAO rats.At the phylum level,it can regulate the abundance of Firmicutes and Proteobacteria in the intestinal flora of rats with cerebral ischemia.At the genus level,it can adjust the abundance of Escherichia Shigella.At the species level,it can adjust the abundance of Lactobacillus yoelii and Lactobacillus reuteri.Cluster classification results show that Qishiwei Zhenzhu pill can improve the intestinal flora of rats with cerebral ischemia,reduce the mRNA and protein expression of caspase-3 and IL^(-1)βin rat brain tissues,and have a tendency to decrease the mRNA expression of p38 MAPK and TNF-α.CONCLUSION Quantifying the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro will help improve their quality standards.Minerals and heavy metals are mainly excreted in feces,accumulate in extremely low levels in various tissues,and do not damage the intestinal mucosa.The effective material basis of Qishiwei Zhenzhu pill in treating cerebral ischemia may be related to their Li,Cr,and Cd elements.These pills can improve the environment of intestinal flora,and their mechanism of treatment for cerebral ischemia may be related to the down-regulation of IL^(-1)βinflammatory factor and inhibition of cell apoptosis.
文摘In this paper,the determination of six heavy metal ions (arsenic,lead,cadmium,chromium,mercury and nickel) in the Chinese Herb by inductively coupled plasma-mass spectrometry (ICP-MS) was studied.The samples were digested by nitric acid and hydrogen peroxide in a microwave oven.The Sc,Y,In,Bi were added as internal standards to eliminate the matrix interferences.The results show that most of the relative standard deviations of these trace elements were below 3.5%,the standard recoveries of these elements were in the range of 91%-107%,and the detection limits were in the range of 0.001-0.006 μg·L-1. This method is accurate,rapid,convenience,and can be applied to the determination of arsenic,lead,cadmium,chromium,mercury and nickel in Chinese Herb with good results.
文摘Inductively coupled plasma mass spectrometry(ICP-MS) was used to determine the concentration of Pb in atmospheric particulate samples,and the enrichment factor was calculated.The causes of the results were also discussed.
文摘Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pressure and working temperature. The etching process of Si3N4 is studied by inductively coupled plasma (ICP) with a gas mixture of SF6 and O2. The influence of the technique parameters, such as ICP power, DC bias, gas composition, total flow rate, on the etching selectivity of Si3N4/EPG533 which is used as a mask layer and the etching rate of Si3N4 is studied, in order to get a better etching selectivity of Si3N4/EPG533 with a faster etching rate of Si3N4. The optimized process parameters of etching Si3N4 by ICP are obtained after a series of experiments and analysis. Under the conditions of total ICP power of 250 W, DC bias of 50W, total flow rate of 40 sccm and O2 composition of 30%, the etching selectivity of 2.05 can be reached when Si3N4 etching rate is 336 nm/min.
基金Project(11JJ5053) supported by the Provincial Natural Science Foundation of Hunan Province,China
文摘Concentration of heavy metals in blood and urine of rabbit after inhaling three different kinds of cigarette was studied through the animal passive smoking pattern. The samples were prepared by nitric acid solution digestion and determination of seven kinds of heavy metals including Hg, Se, Sn, Pb, Cd, Ni and Cr was performed by inductively coupled plasma-atomic emission spectrometry （ICP-AES）. The ICP-AES method was established with good precision and accuracy, relative standard deviation （n=6） was between 2.9% and 5.9%, and the recovery was in the range of 95.0%-104.2%. Concentration of six heavy metals increases in some extent in blood and urine after period of smoking and the increasing of heavy metals in blood and urine all shows time dependence. Significantly higher heavy metal levels are observed in the blood and urine of the cigarette inhaling rabbits in the exposed group. The concentration of six kinds of heavy metals in the blood of the rabbit increases after 16 weeks exposing to cigarette smoking. Three times of rig, ten times of Se and trace amount ofPb, Cd, Ni and Cr are detected in the blood after 16 weeks of smoking. For urine samples, about three times of Hg, two times of Se, five times of Pb and trace amount of Cd are detected after 16 weeks of inhalation of cigarette. Comparatively, higher concentration of heavy metals are detected after inhaling of Nise cigarette.
文摘A method was developed for the simultaneous determination of seven trace impurities (Cd, Mn, Pb, Zn, Cu, Fe and Ni) in high purity cobalt oxide by ICP AES. The matrix effect was eliminated by preci pitation with 1 nitroso 2 naphthol. The matrix effect of cobalt on the absorptions of trace impurities, the effects of reaction time, pH value, dosage of precipitant on the formation of cobalt 1 nitroso 2 naphthol complex, the effects of hydrochloric acid on the stability of this complex and masking of elements were studied. Recoveries of the impurities in spiked sample are from 90% to 110% with a precision of 1.1% 5.0% RSD. The detection limits of the seven elements are in the range of 0.01 0.24μg/g. The method can be applied to the analysis of high purity cobalt metal, cobalt oxide and other cobalt compounds.
