An analytical method for the determination of 26 impurity elements （such as Li, Be, Na, Mg, Al, Si, P, S, K, Ca, Sc, Ti, V, Cr, Co, Ni, Ga, Ge, Y, Nb, Mo, Ag, Cd, Sb, W and Pb） in MnZn ferrite powder by direct curre...An analytical method for the determination of 26 impurity elements （such as Li, Be, Na, Mg, Al, Si, P, S, K, Ca, Sc, Ti, V, Cr, Co, Ni, Ga, Ge, Y, Nb, Mo, Ag, Cd, Sb, W and Pb） in MnZn ferrite powder by direct current glow discharge mass spectrometry （GD-MS） was established. MnZn ferrite powder was mixed with copper powder, used as a conductor, and pressed. The effects of MnZn ferrite powder preparation conditions and glow discharge parameters for the sensitivity and stability of signal analysis were investigated. By determining the choice of isotope and the application of the mass resolutions of 4000 （MR, medium resolution） and 10000 （HR, high resolution）, mass spectral interference was eliminated. The contents of impurity elements in MnZn ferrite powder was calculated by subtraction after normalizing the total signal of Mn, Zn, Fe, O and Cu. The results showed that the detection limit of 26 kinds of impurity elements was between 0.002 and 0.57 μg/g, and the relative standard deviation （RSD） was between 3.33% and 32.35%. The accuracy of this method was verified by the ICP-MS. The method was simple and practical, which is applied to the determination of impurity elements in MnZn ferrite powder.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
Based on comprehensive analysis of the crystal structure, chemical and phase composition of natural arsenopyrite of the "Panimba" deposit (Krasnoyarsk region), an analytical expression for calculating the im...Based on comprehensive analysis of the crystal structure, chemical and phase composition of natural arsenopyrite of the "Panimba" deposit (Krasnoyarsk region), an analytical expression for calculating the impurity density in structure of minerals type of marcasite are received.展开更多
The content analysis of radioactive waste and radiation dose evaluation is considered as one of the important factors in the reactor facility design.This kind of buildings consists of the concrete for the most part an...The content analysis of radioactive waste and radiation dose evaluation is considered as one of the important factors in the reactor facility design.This kind of buildings consists of the concrete for the most part and uses it as the structure and shield of the building.Generally,the concrete has impurities such as cobalt,europium,nickel,and cesium with specific content depending on the production method or manufacturing company.Dominant radioactive nuclides generated from the fundamental components of concrete are considered that it is less contributed to the radiation dose because they are beta decay nuclides in general.Thus,impurities of irradiated concrete in the reactor facilities,are considered occasionally an important evaluation factor for induced activity.In this study,the influence on the activation of impurities in concrete was evaluated from the radiation dose and induced activity calculations.The calculation was evaluated at the bio-shield which is one of the areas with the highest neutron irradiation among the concrete structure in the reactor facility.The results show that radioactive nuclides with gamma decay were produced in these impurities.Moreover,the radiation dose of concrete with impurities was higher than concrete without impurities.The increased radiation dose was quantified through the content of impurities.展开更多
The structure of bupirimate was identified by using MS and NMR.The structures of 10 impurities were identified by using GC-MS.The method provides a powerful tool for structure analysis special in complex samples.
Inductively coupled plasma mass spectrometry (ICP-MS) was used to detect trace metal impurities in reagents such as H2O2, HNO3and H2SO4. The limit of detection to metal elements can be down to 2-20 ng/L in H2O2 and HN...Inductively coupled plasma mass spectrometry (ICP-MS) was used to detect trace metal impurities in reagents such as H2O2, HNO3and H2SO4. The limit of detection to metal elements can be down to 2-20 ng/L in H2O2 and HNO3 and 0.1-1.0 ng/L in H2SO4.展开更多
The structure of coenzyme Q10 sample was identified by MS,IR and NMR.And the impurities were identified by HPLC-ESI MS.The unknown impurities were coenzyme Q10’s structure isomeride,Q9,Q11
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
Macitentan (MAC) is a pulmonary arterial hypertension (PAH) drug marketed as a tablet and often has stability issues in the final dosage form. Quantitative determination of MAC and its associated impurities in tablet ...Macitentan (MAC) is a pulmonary arterial hypertension (PAH) drug marketed as a tablet and often has stability issues in the final dosage form. Quantitative determination of MAC and its associated impurities in tablet dosage form has not been previously reported. This study quantified impurities present in Macitentan tablets using a binary solvent-based gradient elution method using reversed phase-high performance liquid chromatography.The developed method w as validated per International Conference on Harmonization (ICH) guidelines and the drug product w as subjected to forced degradation studies to evaluate stability. The developed method efficiently separated the drug and impurities (48 min) w ithout interference from solvents,excipients,or other impurities. The developed method met all guidelines in all characteristics w ith recoveries ranging from 85%-115%,linearity w ith r 2≥0. 996 6,and substantial robustness. The stability-indicating nature of the method w as evaluated using stressed conditions (hydrolysis:1 N HCl at 80℃/15 min; 1 N NaOH at 25℃/45 min; humidity stress (90%relative humidity) at 25℃for 24 h,oxidation:at 6%(v/v) H2O2,80℃/15 min,thermolysis:at105℃/16 h and photolysis:UV light at 200 Wh/m2; Fluorescent light at 1. 2 million luxh). Forced degradation experiments show ed that the developed method w as effective for impurity profiling. All stressed samples w ere assayed and mass balance w as> 96%. Forced degradation results indicated that MAC tablets w ere sensitive to hydrolysis (acid and alkali) and thermal conditions. The developed method is suitable for both assay and impurity determination,w hich is applicable to the pharmaceutical industry.展开更多
The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carri...The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carried out by LC-MSn using electrospray ionization source and an ion trap mass analyzer. The formation of the impurities was discussed. Also the fragmentation pathways of these compounds were studied.展开更多
Fenthion is an organothiophosphate insecticide,which is a subset of the organophosphates.The analysis of impurities in the pesticide plays an important role in quality control,making a strong impact on the quality of ...Fenthion is an organothiophosphate insecticide,which is a subset of the organophosphates.The analysis of impurities in the pesticide plays an important role in quality control,making a strong impact on the quality of preparation,crops,non-target organisms,human health and the ecological environment.In this article,fenthion and 7 impurities were separated by GC and HPLC,and identified by using electron impact mass spectrometry(EI MS) and electrospray ionization mass spectrometry(ESI MS) methods.The fragmentation reactions of fenthion were further investigated in order to speculate the fragmentation structures of展开更多
Zinc extraction from crude zinc oxide(CZO)is beneficial to the full utilization of secondary resources and environmental protection.In this paper,a systematic investigation was carried out to study the leaching behavi...Zinc extraction from crude zinc oxide(CZO)is beneficial to the full utilization of secondary resources and environmental protection.In this paper,a systematic investigation was carried out to study the leaching behavior of CZO by using ammonia-ammonium carbonate solution.It was found that the maximum leaching rate of zinc from CZO dust was 95.7%under the conditions of[Zn]T:[NH 3]T:[CO_(3)^(2−)]=1:7.00:1.75,liquid to solid ratio 5:1,leaching temperature 30℃ and leaching time 60 min.Compared with pure zinc oxide(PZO)leaching,the CZO leaching required longer time and more leaching agents,which is caused by the Cd^(2+),Pb^(2+) and other metal cationic impurities in CZO.The metal cationic impurities dissolved in the leaching solution and combined with ammonium to form complexes,consuming leaching agents and affecting zinc leaching.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
In this study,Al-65V alloy has been produced by electrode heating for 3−15 min.The impurities content,microstructure and the vanadium content of the alloy in the slag are investigated.The results indicate that differe...In this study,Al-65V alloy has been produced by electrode heating for 3−15 min.The impurities content,microstructure and the vanadium content of the alloy in the slag are investigated.The results indicate that different heating time shows obviously impacts not only on the impurities and microstructure of AlV alloy,but also on the vanadium recovery rate of slag.The impurities contents of C,O and N are 0.085%,0.022%and 0.036%,respectively,which meet the commercial standard when the electric heating time is controlled to 10 min,and the content of vanadium in slag is 0.18%.展开更多
基金Project(21275162)supported by the National Natural Science Foundation of ChinaProject(KJZH14217)supported by the Achievement Transfer Program of Institutions of Higher Education in Chongqing,ChinaProject(KJ1601224)supported by the Scientific and Technological Research Program of Chongqing Municipal Education Commission,China
文摘An analytical method for the determination of 26 impurity elements （such as Li, Be, Na, Mg, Al, Si, P, S, K, Ca, Sc, Ti, V, Cr, Co, Ni, Ga, Ge, Y, Nb, Mo, Ag, Cd, Sb, W and Pb） in MnZn ferrite powder by direct current glow discharge mass spectrometry （GD-MS） was established. MnZn ferrite powder was mixed with copper powder, used as a conductor, and pressed. The effects of MnZn ferrite powder preparation conditions and glow discharge parameters for the sensitivity and stability of signal analysis were investigated. By determining the choice of isotope and the application of the mass resolutions of 4000 （MR, medium resolution） and 10000 （HR, high resolution）, mass spectral interference was eliminated. The contents of impurity elements in MnZn ferrite powder was calculated by subtraction after normalizing the total signal of Mn, Zn, Fe, O and Cu. The results showed that the detection limit of 26 kinds of impurity elements was between 0.002 and 0.57 μg/g, and the relative standard deviation （RSD） was between 3.33% and 32.35%. The accuracy of this method was verified by the ICP-MS. The method was simple and practical, which is applied to the determination of impurity elements in MnZn ferrite powder.
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Based on comprehensive analysis of the crystal structure, chemical and phase composition of natural arsenopyrite of the "Panimba" deposit (Krasnoyarsk region), an analytical expression for calculating the impurity density in structure of minerals type of marcasite are received.
基金This work was supported by the R&D program throughout the National Fusion Research Institute(NFRI)funded by the Ministry of Science of the Republic of Korea(Project No.:201800000002652),and Innovative Technology Center for Radiation Safety(ITRS).
文摘The content analysis of radioactive waste and radiation dose evaluation is considered as one of the important factors in the reactor facility design.This kind of buildings consists of the concrete for the most part and uses it as the structure and shield of the building.Generally,the concrete has impurities such as cobalt,europium,nickel,and cesium with specific content depending on the production method or manufacturing company.Dominant radioactive nuclides generated from the fundamental components of concrete are considered that it is less contributed to the radiation dose because they are beta decay nuclides in general.Thus,impurities of irradiated concrete in the reactor facilities,are considered occasionally an important evaluation factor for induced activity.In this study,the influence on the activation of impurities in concrete was evaluated from the radiation dose and induced activity calculations.The calculation was evaluated at the bio-shield which is one of the areas with the highest neutron irradiation among the concrete structure in the reactor facility.The results show that radioactive nuclides with gamma decay were produced in these impurities.Moreover,the radiation dose of concrete with impurities was higher than concrete without impurities.The increased radiation dose was quantified through the content of impurities.
文摘The structure of bupirimate was identified by using MS and NMR.The structures of 10 impurities were identified by using GC-MS.The method provides a powerful tool for structure analysis special in complex samples.
文摘Inductively coupled plasma mass spectrometry (ICP-MS) was used to detect trace metal impurities in reagents such as H2O2, HNO3and H2SO4. The limit of detection to metal elements can be down to 2-20 ng/L in H2O2 and HNO3 and 0.1-1.0 ng/L in H2SO4.
文摘The structure of coenzyme Q10 sample was identified by MS,IR and NMR.And the impurities were identified by HPLC-ESI MS.The unknown impurities were coenzyme Q10’s structure isomeride,Q9,Q11
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.
基金the management of Sinotherapeutics Inc. for supporting this study
文摘Macitentan (MAC) is a pulmonary arterial hypertension (PAH) drug marketed as a tablet and often has stability issues in the final dosage form. Quantitative determination of MAC and its associated impurities in tablet dosage form has not been previously reported. This study quantified impurities present in Macitentan tablets using a binary solvent-based gradient elution method using reversed phase-high performance liquid chromatography.The developed method w as validated per International Conference on Harmonization (ICH) guidelines and the drug product w as subjected to forced degradation studies to evaluate stability. The developed method efficiently separated the drug and impurities (48 min) w ithout interference from solvents,excipients,or other impurities. The developed method met all guidelines in all characteristics w ith recoveries ranging from 85%-115%,linearity w ith r 2≥0. 996 6,and substantial robustness. The stability-indicating nature of the method w as evaluated using stressed conditions (hydrolysis:1 N HCl at 80℃/15 min; 1 N NaOH at 25℃/45 min; humidity stress (90%relative humidity) at 25℃for 24 h,oxidation:at 6%(v/v) H2O2,80℃/15 min,thermolysis:at105℃/16 h and photolysis:UV light at 200 Wh/m2; Fluorescent light at 1. 2 million luxh). Forced degradation experiments show ed that the developed method w as effective for impurity profiling. All stressed samples w ere assayed and mass balance w as> 96%. Forced degradation results indicated that MAC tablets w ere sensitive to hydrolysis (acid and alkali) and thermal conditions. The developed method is suitable for both assay and impurity determination,w hich is applicable to the pharmaceutical industry.
文摘The impurities in ethyl-2-[[2′-cyanobiphenyl-4-yl] methyl] amino]-3-nitrobenzoate,an intermediate for synthesis of candesartan cilexiti,were detected by LC-MSn. The structural assignment of these impurities was carried out by LC-MSn using electrospray ionization source and an ion trap mass analyzer. The formation of the impurities was discussed. Also the fragmentation pathways of these compounds were studied.
文摘Fenthion is an organothiophosphate insecticide,which is a subset of the organophosphates.The analysis of impurities in the pesticide plays an important role in quality control,making a strong impact on the quality of preparation,crops,non-target organisms,human health and the ecological environment.In this article,fenthion and 7 impurities were separated by GC and HPLC,and identified by using electron impact mass spectrometry(EI MS) and electrospray ionization mass spectrometry(ESI MS) methods.The fragmentation reactions of fenthion were further investigated in order to speculate the fragmentation structures of
基金Project(2020YFC1909805)supported by the National Key Research and Development Program of ChinaProjects(51504293,51574284)supported by the National Natural Science Foundation of China+2 种基金Project(2018-GX-A7)supported by Qinghai Provincial Major Scientific and Technological Special Project of ChinaProject(2020SK2125)supported by the Key Research and Development Program of Hunan Province,ChinaProject(CSUZC202129)supported by Open Sharing Fund for the Large-scale Instruments and Equipments of Central South University,China。
文摘Zinc extraction from crude zinc oxide(CZO)is beneficial to the full utilization of secondary resources and environmental protection.In this paper,a systematic investigation was carried out to study the leaching behavior of CZO by using ammonia-ammonium carbonate solution.It was found that the maximum leaching rate of zinc from CZO dust was 95.7%under the conditions of[Zn]T:[NH 3]T:[CO_(3)^(2−)]=1:7.00:1.75,liquid to solid ratio 5:1,leaching temperature 30℃ and leaching time 60 min.Compared with pure zinc oxide(PZO)leaching,the CZO leaching required longer time and more leaching agents,which is caused by the Cd^(2+),Pb^(2+) and other metal cationic impurities in CZO.The metal cationic impurities dissolved in the leaching solution and combined with ammonium to form complexes,consuming leaching agents and affecting zinc leaching.
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(51734006)supported by the National Natural Science Foundation of ChinaProject(2014HA003)supported by the Cultivating Plan Program for the Leader in Science and Technology of Yunnan Province of China+1 种基金Project(2017HB009)supported by the Science and Technological Talent Cultivation Plan of Yunnan Province,ChinaProject(2017HA006)supported by the Program for the Academician Free Exploration Fund of Yunnan Province,China
文摘In this study,Al-65V alloy has been produced by electrode heating for 3−15 min.The impurities content,microstructure and the vanadium content of the alloy in the slag are investigated.The results indicate that different heating time shows obviously impacts not only on the impurities and microstructure of AlV alloy,but also on the vanadium recovery rate of slag.The impurities contents of C,O and N are 0.085%,0.022%and 0.036%,respectively,which meet the commercial standard when the electric heating time is controlled to 10 min,and the content of vanadium in slag is 0.18%.
