The Reference Listed drug(RLD)plays a critical role in the development and research of generic medicinal products,serving as the comparator product used in the marketing authorization application of new generic medici...The Reference Listed drug(RLD)plays a critical role in the development and research of generic medicinal products,serving as the comparator product used in the marketing authorization application of new generic medicinal product and re-evaluation of generic medicinal product.In China,RLDs are sourced from various origins,but their quality and market availability can be constrained by multiple factors,including emergent issues such as nitrosamine impurities.Five classes of medicinal products have been reported to be at risk for containing nitrosamine impurities:sartan-based medicines,metformin-containing products,ranitidine medicines,rifampicin medicines,and Champix.This paper explores the control strategies implemented by drug regulatory agencies in the United States and the European Union to manage nitrosamine impurities and assesses their impact on the market availability and quality of RLDs in China.The aim is to offer valuable insights for generic drug manufacturers and regulatory bodies both domestically and internationally.展开更多
The cleanliness of seed cotton plays a critical role in the pre-treatment of cotton textiles,and the removal of impurity during the harvesting process directly determines the quality and market value of cotton textile...The cleanliness of seed cotton plays a critical role in the pre-treatment of cotton textiles,and the removal of impurity during the harvesting process directly determines the quality and market value of cotton textiles.By fusing band combination optimization with deep learning,this study aims to achieve more efficient and accurate detection of film impurities in seed cotton on the production line.By applying hyperspectral imaging and a one-dimensional deep learning algorithm,we detect and classify impurities in seed cotton after harvest.The main categories detected include pure cotton,conveyor belt,film covering seed cotton,and film adhered to the conveyor belt.The proposed method achieves an impurity detection rate of 99.698%.To further ensure the feasibility and practical application potential of this strategy,we compare our results against existing mainstream methods.In addition,the model shows excellent recognition performance on pseudo-color images of real samples.With a processing time of 11.764μs per pixel from experimental data,it shows a much improved speed requirement while maintaining the accuracy of real production lines.This strategy provides an accurate and efficient method for removing impurities during cotton processing.展开更多
Magnesium(Mg),as one of the most abundant elements in earth's crust,is the lightest structural metal with extensive applications across various industries.However,the performance of Mg-based products is highly dep...Magnesium(Mg),as one of the most abundant elements in earth's crust,is the lightest structural metal with extensive applications across various industries.However,the performance of Mg-based products is highly dependent on their impurity levels,and the lack of high-purity Mg,along with efficient purification method,has posed significant challenge to its widespread industrial adoption.This study investigates the impurity behavior in Mg ingots during the vacuum gasification purification process.Through the analysis of binary phase diagrams,iron(Fe)-based foam material was selected for the filtration and purification of Mg vapor in a vacuum tube furnace.A novel approach combining vacuum gasification,vapor purification,and directional condensation is proposed.The effect of filter pore sizes and filtration temperatures on the efficacy of impurity removal was evaluated.Experimental results demonstrate that Fe-based foam with a pore size of 60 ppi,at a filtration temperature of 773 K,effectively removes impurities such as calcium(Ca),potassium(K),sodium(Na),manganese(Mn),silicon(Si),aluminum(Al),and various oxides,sulfides,and chlorides from the vapor phase.Consequently,high-purity Mg with a purity level exceeding 5N3 was obtained in the condensation zone.展开更多
The effects of the structure and concentration of impurities on the alkylation of naphthalene with 1-octene catalyzed by chloroaluminate ionic liquid(IL)were investigated.The presence of impurities containing oxygen a...The effects of the structure and concentration of impurities on the alkylation of naphthalene with 1-octene catalyzed by chloroaluminate ionic liquid(IL)were investigated.The presence of impurities containing oxygen and nitrogen led to a decrease in the catalytic performance of chloroaluminate IL.As the water concentration increased to 65 mg·g^(-1),the total selectivity of multi-octylnaphthalene gradually decreased to 42.33%,and the average friction coefficient of the multi-octylnaphthalene base oil gradually increased to 0.201.When the concentration of impurities increased to a critical value,the chloroaluminate IL began to deactivate,leading to a decrease in naphthalene conversion.The critical concentrations for ethanolamine,water,methanol,ether,and diisopentyl sulfide were 33 mg·g^(-1),65 mg·g^(-1),67mg·g^(-1),87 mg·g^(-1),and 123 mg·g^(-1),respectively.Impurities with higher basicity resulted in an earlier onset of chloroaluminate IL deactivation.The changes of Lewis and Brønsted acids in chloroaluminate IL under the influence of impurities were investigated using in situ IR and 27Al NMR spectroscopy.2,6-dimethylpyridine as an indicator could detect the changes of Brønsted acid in chloroaluminate IL better,but the changes of Lewis acid were not obvious because of the overlap between the characteristic peaks.2,6-dichloropyridine as an indicator could exclusively detect the changes of Lewis acid in chloroaluminate IL.With the increase inwater concentration,the Lewis acid in chloroaluminate IL was continuously consumed and converted into Brønsted acid,and the Lewis acid gradually decreased,while the Brønsted acid showed a change of increasing first and then decreasing.展开更多
[Objectives]To establish a HPLC-MS method for the determination of polymer impurities in cefathiamidine and its preparations.[Methods]Kromasil 100-5 C_(18) column(4.6 mm ×250 mm,5μm)was used for analysis;mobile ...[Objectives]To establish a HPLC-MS method for the determination of polymer impurities in cefathiamidine and its preparations.[Methods]Kromasil 100-5 C_(18) column(4.6 mm ×250 mm,5μm)was used for analysis;mobile phase ammonium acetate solution(pH 6.30)-acetonitrile,gradient elution;volumetric flow rate 1.0 mL/min;column temperature 40℃;multi-reaction monitoring mode was used for analysis,and positive ion scanning was chosen as the electrospray ion source.[Results]The resolution between impurities and main peaks under this method was greater than 1.5,and 8 known impurities and 2 polymer impurities could be completely separated and distinguish-ed.It was inferred that the molecular ion peak[M+H]^(+):m/z727.1874,m/z 785.1937 was the possible polymer impurity of this product.[Conclusions]A method for the analysis of polymer impurities in cefathiamidine and its preparations was formed,which could achieve the purpose of simultaneous analysis of small molecule impurities and polymer impurities,and could better control the content of single impurities in the polymer,providing a reliable inspection basis for strict control of cefathiamidine quality.展开更多
Potential mutagenic impurities in Active Pharmaceutical Ingredient, Meropenem Trihydrate were assessed and a novel analytical method for their quantification was developed and validated. This Liquid Chromatographic me...Potential mutagenic impurities in Active Pharmaceutical Ingredient, Meropenem Trihydrate were assessed and a novel analytical method for their quantification was developed and validated. This Liquid Chromatographic method using High Resolution Mass Spectrometer (LC-HRMS) technique is proved to be suitable for simultaneous quantification of all ten identified impurities with required specificity, sensitivity, resolution, precision, accuracy, and other method characteristics as per ICH Guidelines. The acceptable limit of less than 2.9 μg/g was considered for evaluations, based on drug substance dosage and duration of treatment. The method stands most sensitive with a Limit of Detection of 0.35 μg/g, considering the challenge full acceptance criteria as per current regulatory standards.展开更多
To clarify the precipitation of silica hydrate from the real desilication solutions of aluminosilicate solid wastes by adding seeds and improve integrated waste utilization,the seeded precipitation was studied using s...To clarify the precipitation of silica hydrate from the real desilication solutions of aluminosilicate solid wastes by adding seeds and improve integrated waste utilization,the seeded precipitation was studied using synthesized sodium silicate solution containing different inorganic salt impurities.The results show that sodium chloride,sodium sulfate,sodium carbonate,or calcium chloride can change the siloxy group structure.The number of high-polymeric siloxy groups decreases with increasing sodium chloride or sodium sulfate concentration,which is detrimental to seeded precipitation.Calcium chloride favors the polymerization of silicate ions,and even the chain groups precipitate with the precipitation of high-polymeric sheet and cage-like siloxy groups.The introduced sodium cations in sodium carbonate render a more open network structure of high-polymeric siloxy groups,although the carbonate ions favor the polymerization of siloxy groups.No matter how the four impurities affect the siloxy group structure,the precipitates are always amorphous opal-A silica hydrate.展开更多
Gas blowing is a valid method to remove the impurities from metallurgical grade silicon(MG-Si) melt.The thermodynamic behavior of impurities Fe,Al,Ca,Ti,Cu,C,B and P in MG-Si was studied in the process of O2 blowing...Gas blowing is a valid method to remove the impurities from metallurgical grade silicon(MG-Si) melt.The thermodynamic behavior of impurities Fe,Al,Ca,Ti,Cu,C,B and P in MG-Si was studied in the process of O2 blowing.The removal efficiencies of impurities in MG-Si were investigated using O2 blowing in ladle.It is found that the removal efficiencies are higher than 90% for Ca and Al and nearly 50% for B and Ti.The morphology of inclusions was analyzed and the phases Al3Ni,NiSi2 and Al3Ni were confirmed in MG-Si by X-ray diffraction.It was found that SiB4 exists in Si?B binary system.The chemical composition of inclusions in MG-Si before and after refining was analyzed by SEM-EDS.It is found that the amount of white inclusion reduces for the removal of most Al and Ca in the forms of molten slag inclusion and the contents of Fe,Ni and Mn in inclusion increase for their inertia in silicon melt with O2 blowing.展开更多
An HPLC method for routine quality control of biapenem was established.A Dikma Diamonsil C_(18) column(250mm×4.6 mm,5μm) was used with diode array detection and single wavelength detection at 220 nm.The mobile p...An HPLC method for routine quality control of biapenem was established.A Dikma Diamonsil C_(18) column(250mm×4.6 mm,5μm) was used with diode array detection and single wavelength detection at 220 nm.The mobile phase was consisted of acetonitrile-0.1%triethylamine water(1:99,v/v).The liner range for biapenem quantification was 0.05-10.0 mg/mL(r^2= 0.999). The LOD and LOQ of impurity were 4.8 ng(S/N = 3) and 18.5 ng(S/N = 10),respectively.Intra-day RSD of main impurity and total impurity were 1.84%and 3.37%(n = 3);inter-day RSD of main impurity and total impurity were 4.84%and 7.58% (n = 9).The test solution was stable when stored at 4℃for 6 h.The impurity peaks of biapenem can be identified by chromatographic spectral correlation analysis using high-performance liquid chromatography-diode array detection data from the quality control method by calculating correlation coefficients without reference standards.Two hydrolysis degradation products with relative retention times(RRTs) of 0.528 and 0.743,two dimers with RRTs of 1.062 and 2.817 were identified in the quality control chromatogram.It provides a new way to identify impurity peaks by the routine HPLC-UV method.展开更多
The model of dislocations was used to construct the model of grain boundary (GB) with pure rare earths, and rare earth elements and impurities. The influence of the interaction between rare earth elements and impuriti...The model of dislocations was used to construct the model of grain boundary (GB) with pure rare earths, and rare earth elements and impurities. The influence of the interaction between rare earth elements and impurities on the cohesive properties of 5.3° low angle GB of Fe was investigated by the recursion method. The calculated results of environment sensitive embeding energy( E ESE ) show that the preferential segregation of rare earth elements towards GBs exists. Calculations of bond order integrals (BOI) show that rare earth elements increase the cohesive strength of low angle GB, and impurities such as S, P weaken the intergranular cohesion of the GB. So rare earth element of proper quantity added in steel not only cleanses other harmful impurities off the GBs, but also enhances the intergranular cohesion. This elucidates the action mechanism of rare earth elements in steel from electronic level and offers theoretical evidence for applications of rare earth elements in steels.展开更多
Effect of impurities in recycling water on Pb-Ag anode passivation in zinc electrowinning process was investigated by linear scan voltammetry.Results show that passivation process would be affected in the presence of ...Effect of impurities in recycling water on Pb-Ag anode passivation in zinc electrowinning process was investigated by linear scan voltammetry.Results show that passivation process would be affected in the presence of Cl^-and F-in recycling water.It was highly advantageous to take H2SO4 concentration as 180g/L,Mn^2+ concentration as 3-5 g/L and F-less than 42mg/L.However,passivation process would not be affected when Cl^-concentration was less than 13mg/L without any other ions,or when mass ratio of Mn^2+ to Cl^-existing in electrolyte was 8,where Cl^-concentration could reach up to 625mg/L.展开更多
The role of trivalent antimony was investigated in removing As, Sb, and Bi impurities from a copper electrolyte. Puri- fication experiments were carried out by adding a various concentrations of Sb(III) ions in a sy...The role of trivalent antimony was investigated in removing As, Sb, and Bi impurities from a copper electrolyte. Puri- fication experiments were carried out by adding a various concentrations of Sb(III) ions in a synthetic electrolyte containing 185 g/L sulfuric acid, 45 g/L Cu2+, 10 g/L As, and 0.5 g/L Bi under stirring at 65℃ for 2 h. The electrolyte was filtered, and the structure, morphology and composition of the precipitate were analyzed by means of chemical analysis, scanning electron mi- croscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and IR spectroscopy. The precipitate is composed of irregular lumps which are agglomerated by fine dendritic and floccus particles, and it mainly consists of As, Sb, Bi, and O elements. Characteristic bands in the IR spectra of the precipitate are As-OX (X=As, Sb, Bi), Sb-OY (Y=Sb, Bi), O-As-O1 As-OH, Sb-OH, and O-H. The precipitate is a mixture of microcrystalline SbAsQ, (Sb,As)203, and amorphous phases. As, Sb, and Bi impurities are effectively removed from the copper electrolyte by Sb(III) ions attributing to these pre- cipitates.展开更多
The binding energy and the photon energy dependence of the photoionization cross-section are calculated for a hydrogenic impurity in GaAs/Ga 1-xAl xAs quantum well wires.The correlation between confined and non-co...The binding energy and the photon energy dependence of the photoionization cross-section are calculated for a hydrogenic impurity in GaAs/Ga 1-xAl xAs quantum well wires.The correlation between confined and non-confined direction of the wire in the variational wave function is taken into account.The results show that the photoionization cross-sections are affected by the width of the wire and that their magnitudes are larger than those in infinite potential quantum well wires.In comparison with previous's results,the variational wave function improves the binding energy and decreases the value of photoionization cross-sections of the hydrogenic impurities,which makes the results more reasonable.展开更多
A An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, ...A An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.展开更多
The purification of metallurgical-grade silicon (MG-Si) has been investigated during electron beam melting (EBM) process. The results show that the phosphorus, calcium and aluminum contents decrease significantly ...The purification of metallurgical-grade silicon (MG-Si) has been investigated during electron beam melting (EBM) process. The results show that the phosphorus, calcium and aluminum contents decrease significantly after melting, and magnesium is partially removed. However, no significant change in content for boron and iron has been found. Langmuir's equation and Henry law were used to derive the removal effi-ciency for each impurity element. The free surface temperature was estimated by the Hertz-Knudsen-Langmuir equation and silicon's vapor pressure equation. Good agreement was found between measured and calculated impurities' removal efficiency for phosphorus, calcium and aluminum, magnesium, boron and iron. The deviation between the two results was also analyzed in depth.展开更多
The effect of grinding on the spodumene flotation was investigated. The flotation response of spodumene ground by different mills was different, due to the variation of metal ions on spodumene surfaces caused by grind...The effect of grinding on the spodumene flotation was investigated. The flotation response of spodumene ground by different mills was different, due to the variation of metal ions on spodumene surfaces caused by grinding environments and/or impurities. The samples were subjected to acid pickling treatment to remove most of the metal ions from the surfaces, and then all samples showed the same poor flotation response, which confirmed the significance of surface metal ions. Metal ion impurities may come from both grinding environments and lattice substitutions in spodumene. Density functional theory (DFT) calculation revealed that Fe and Ca could exist as lattice substitutions on the spodumene surface while Mg substitution is unlikely to occur. Furthermore, Fe is considered to be active site for the absorption of sodium oleate on the spodumene surface. Morphology analysis showed differences in particle size and shape for samples ground by different mills, resulting in different amounts of exposed surfaces. The particle size, cleavage characteristics caused by grinding environments, and metal ion impurities originated from grinding and isomorphous substitutions, play significant roles in the chemisorption of collector on the spodumene surface.展开更多
An effective parameter in the miscible-CO_2 enhanced oil recovery procedure is the minimum miscibility pressure(MMP)defined as the lowest pressure that the oil in place and the injected gas into reservoir achieve misc...An effective parameter in the miscible-CO_2 enhanced oil recovery procedure is the minimum miscibility pressure(MMP)defined as the lowest pressure that the oil in place and the injected gas into reservoir achieve miscibility at a given temperature. Flue gases released from power plants can provide an available source of CO_2,which would otherwise be emitted to the atmosphere, for injection into a reservoir. However, the costs related to gas extraction from flue gases is potentially high. Hence, greater understanding the role of impurities in miscibility characteristics between CO_2 and reservoir fluids helps to establish which impurities are tolerable and which are not. In this study, we simulate the effects of the impurities nitrogen(N_2), methane(C_1), ethane(C_2) and propane(C_3) on CO_2 MMP. The simulation results reveal that,as an impurity, nitrogen increases CO_2–oil MMP more so than methane. On the other hand, increasing the propane(C_3)content can lead to a significant decrease in CO_2 MMP, whereas varying the concentrations of ethane(C_2) does not have a significant effect on the minimum miscibility pressure of reservoir crude oil and CO_2 gas. The novel relationships established are particularly valuable in circumstances where MMP experimental data are not available.展开更多
The influence of impurity content on the microstructure and mechanical properties of ZK60 magnesium alloys was investigated by optical microscopy,scanning electron microscopy and tensile test.ZK60 alloys were prepared...The influence of impurity content on the microstructure and mechanical properties of ZK60 magnesium alloys was investigated by optical microscopy,scanning electron microscopy and tensile test.ZK60 alloys were prepared by changing holding time of alloy melt during semi-continuous casting in order to control the content of impurity elements.The alloy with lower purity content is found to have less second precipitates and larger grain size in the as-cast state.However,in the as-extruded state,reducing impurities brings about a decrease in grain size and an increase in yield strength from 244 MPa to 268 MPa,while the elongations in the as-extruded alloys with different contents of impurities are almost the same.After T5 treatment,impurity content is found to have more obvious effect on the yield strength of ZK60 alloy.The yield strength of ZK60-45 alloys with low impurity content is increased up to 295 MPa after T5 treatment.展开更多
In this paper, a two-dimensional axisymmetric fluid model was established to investigate the influence of nitrogen impurity content on the discharge pattern and the relevant discharge characteristics in an atmosphere ...In this paper, a two-dimensional axisymmetric fluid model was established to investigate the influence of nitrogen impurity content on the discharge pattern and the relevant discharge characteristics in an atmosphere pressure helium dielectric barrier discharge(DBD). The results indicated that when the nitrogen content was increased from 1 to 100 ppm, the discharge pattern evolved from a concentric-ring pattern into a uniform pattern, and then returned to the concentricring pattern. In this process, the discharge mode at the current peak moment transformed from glow mode into Townsend mode, and then returned to glow mode. Further analyses revealed that with the increase of impurity level, the rate of Penning ionization at the pre-ionization stage increased at first and decreased afterwards, resulting in a similar evolution pattern of seed electron level. This evolution trend was believed to be resulted from the competition between the N2 partial pressure and the consumption rate of metastable species. Moreover, the discharge uniformity was found positively correlated with the spatial uniformity of seed electron density as well as the seed electron level. The reason for this correlation was explained by the reduction of radial electric field strength and the promotion of seed electron uniformity as pre-ionization level increases. The results obtained in this work may help better understand the pattern formation mechanism of atmospheric helium DBD under the variation of N2 impurity level, thereby providing a possible means of regulating the discharge performance in practical application scenarios.展开更多
基金Subject construction funding project of Institute for Chemical Drug Control(Grant No.2024HYZX42)in National Institutes for Food and Drug Control,Beijing,China。
文摘The Reference Listed drug(RLD)plays a critical role in the development and research of generic medicinal products,serving as the comparator product used in the marketing authorization application of new generic medicinal product and re-evaluation of generic medicinal product.In China,RLDs are sourced from various origins,but their quality and market availability can be constrained by multiple factors,including emergent issues such as nitrosamine impurities.Five classes of medicinal products have been reported to be at risk for containing nitrosamine impurities:sartan-based medicines,metformin-containing products,ranitidine medicines,rifampicin medicines,and Champix.This paper explores the control strategies implemented by drug regulatory agencies in the United States and the European Union to manage nitrosamine impurities and assesses their impact on the market availability and quality of RLDs in China.The aim is to offer valuable insights for generic drug manufacturers and regulatory bodies both domestically and internationally.
基金supported in part by the Six Talent Peaks Project in Jiangsu Province under Grant 013040315in part by the China Textile Industry Federation Science and Technology Guidance Project under Grant 2017107+1 种基金in part by the National Natural Science Foundation of China under Grant 31570714in part by the China Scholarship Council under Grant 202108320290。
文摘The cleanliness of seed cotton plays a critical role in the pre-treatment of cotton textiles,and the removal of impurity during the harvesting process directly determines the quality and market value of cotton textiles.By fusing band combination optimization with deep learning,this study aims to achieve more efficient and accurate detection of film impurities in seed cotton on the production line.By applying hyperspectral imaging and a one-dimensional deep learning algorithm,we detect and classify impurities in seed cotton after harvest.The main categories detected include pure cotton,conveyor belt,film covering seed cotton,and film adhered to the conveyor belt.The proposed method achieves an impurity detection rate of 99.698%.To further ensure the feasibility and practical application potential of this strategy,we compare our results against existing mainstream methods.In addition,the model shows excellent recognition performance on pseudo-color images of real samples.With a processing time of 11.764μs per pixel from experimental data,it shows a much improved speed requirement while maintaining the accuracy of real production lines.This strategy provides an accurate and efficient method for removing impurities during cotton processing.
基金supported by the Yunnan Province Nonferrous Metal Vacuum Metallurgy Top Team[No.202305AS350012]。
文摘Magnesium(Mg),as one of the most abundant elements in earth's crust,is the lightest structural metal with extensive applications across various industries.However,the performance of Mg-based products is highly dependent on their impurity levels,and the lack of high-purity Mg,along with efficient purification method,has posed significant challenge to its widespread industrial adoption.This study investigates the impurity behavior in Mg ingots during the vacuum gasification purification process.Through the analysis of binary phase diagrams,iron(Fe)-based foam material was selected for the filtration and purification of Mg vapor in a vacuum tube furnace.A novel approach combining vacuum gasification,vapor purification,and directional condensation is proposed.The effect of filter pore sizes and filtration temperatures on the efficacy of impurity removal was evaluated.Experimental results demonstrate that Fe-based foam with a pore size of 60 ppi,at a filtration temperature of 773 K,effectively removes impurities such as calcium(Ca),potassium(K),sodium(Na),manganese(Mn),silicon(Si),aluminum(Al),and various oxides,sulfides,and chlorides from the vapor phase.Consequently,high-purity Mg with a purity level exceeding 5N3 was obtained in the condensation zone.
基金financial support of the Scientific Research Funds of Huaqiao University (605-50Y17073)
文摘The effects of the structure and concentration of impurities on the alkylation of naphthalene with 1-octene catalyzed by chloroaluminate ionic liquid(IL)were investigated.The presence of impurities containing oxygen and nitrogen led to a decrease in the catalytic performance of chloroaluminate IL.As the water concentration increased to 65 mg·g^(-1),the total selectivity of multi-octylnaphthalene gradually decreased to 42.33%,and the average friction coefficient of the multi-octylnaphthalene base oil gradually increased to 0.201.When the concentration of impurities increased to a critical value,the chloroaluminate IL began to deactivate,leading to a decrease in naphthalene conversion.The critical concentrations for ethanolamine,water,methanol,ether,and diisopentyl sulfide were 33 mg·g^(-1),65 mg·g^(-1),67mg·g^(-1),87 mg·g^(-1),and 123 mg·g^(-1),respectively.Impurities with higher basicity resulted in an earlier onset of chloroaluminate IL deactivation.The changes of Lewis and Brønsted acids in chloroaluminate IL under the influence of impurities were investigated using in situ IR and 27Al NMR spectroscopy.2,6-dimethylpyridine as an indicator could detect the changes of Brønsted acid in chloroaluminate IL better,but the changes of Lewis acid were not obvious because of the overlap between the characteristic peaks.2,6-dichloropyridine as an indicator could exclusively detect the changes of Lewis acid in chloroaluminate IL.With the increase inwater concentration,the Lewis acid in chloroaluminate IL was continuously consumed and converted into Brønsted acid,and the Lewis acid gradually decreased,while the Brønsted acid showed a change of increasing first and then decreasing.
基金Supported by2023 Central Funds for Guiding Local Science and Technology Development(ZY20230102)Guilin City Scientific Research and Technology Development Plan Project(20220104-4).
文摘[Objectives]To establish a HPLC-MS method for the determination of polymer impurities in cefathiamidine and its preparations.[Methods]Kromasil 100-5 C_(18) column(4.6 mm ×250 mm,5μm)was used for analysis;mobile phase ammonium acetate solution(pH 6.30)-acetonitrile,gradient elution;volumetric flow rate 1.0 mL/min;column temperature 40℃;multi-reaction monitoring mode was used for analysis,and positive ion scanning was chosen as the electrospray ion source.[Results]The resolution between impurities and main peaks under this method was greater than 1.5,and 8 known impurities and 2 polymer impurities could be completely separated and distinguish-ed.It was inferred that the molecular ion peak[M+H]^(+):m/z727.1874,m/z 785.1937 was the possible polymer impurity of this product.[Conclusions]A method for the analysis of polymer impurities in cefathiamidine and its preparations was formed,which could achieve the purpose of simultaneous analysis of small molecule impurities and polymer impurities,and could better control the content of single impurities in the polymer,providing a reliable inspection basis for strict control of cefathiamidine quality.
文摘Potential mutagenic impurities in Active Pharmaceutical Ingredient, Meropenem Trihydrate were assessed and a novel analytical method for their quantification was developed and validated. This Liquid Chromatographic method using High Resolution Mass Spectrometer (LC-HRMS) technique is proved to be suitable for simultaneous quantification of all ten identified impurities with required specificity, sensitivity, resolution, precision, accuracy, and other method characteristics as per ICH Guidelines. The acceptable limit of less than 2.9 μg/g was considered for evaluations, based on drug substance dosage and duration of treatment. The method stands most sensitive with a Limit of Detection of 0.35 μg/g, considering the challenge full acceptance criteria as per current regulatory standards.
基金financial support from the National Natural Science Foundation of China(No.52074364)。
文摘To clarify the precipitation of silica hydrate from the real desilication solutions of aluminosilicate solid wastes by adding seeds and improve integrated waste utilization,the seeded precipitation was studied using synthesized sodium silicate solution containing different inorganic salt impurities.The results show that sodium chloride,sodium sulfate,sodium carbonate,or calcium chloride can change the siloxy group structure.The number of high-polymeric siloxy groups decreases with increasing sodium chloride or sodium sulfate concentration,which is detrimental to seeded precipitation.Calcium chloride favors the polymerization of silicate ions,and even the chain groups precipitate with the precipitation of high-polymeric sheet and cage-like siloxy groups.The introduced sodium cations in sodium carbonate render a more open network structure of high-polymeric siloxy groups,although the carbonate ions favor the polymerization of siloxy groups.No matter how the four impurities affect the siloxy group structure,the precipitates are always amorphous opal-A silica hydrate.
基金Projects(51104080,u1137601) supported by the National Natural Science Foundation of ChinaProject(2009CD027) supported by the Natural Science Foundation of Yunnan Province,ChinaProject(14118557) supported by the Personnel Training Foundation of Kunming University of Science and Technology,China
文摘Gas blowing is a valid method to remove the impurities from metallurgical grade silicon(MG-Si) melt.The thermodynamic behavior of impurities Fe,Al,Ca,Ti,Cu,C,B and P in MG-Si was studied in the process of O2 blowing.The removal efficiencies of impurities in MG-Si were investigated using O2 blowing in ladle.It is found that the removal efficiencies are higher than 90% for Ca and Al and nearly 50% for B and Ti.The morphology of inclusions was analyzed and the phases Al3Ni,NiSi2 and Al3Ni were confirmed in MG-Si by X-ray diffraction.It was found that SiB4 exists in Si?B binary system.The chemical composition of inclusions in MG-Si before and after refining was analyzed by SEM-EDS.It is found that the amount of white inclusion reduces for the removal of most Al and Ca in the forms of molten slag inclusion and the contents of Fe,Ni and Mn in inclusion increase for their inertia in silicon melt with O2 blowing.
基金National Key New Drug R&D Program Foundation of China(Grant No.2009ZX09313-027).
文摘An HPLC method for routine quality control of biapenem was established.A Dikma Diamonsil C_(18) column(250mm×4.6 mm,5μm) was used with diode array detection and single wavelength detection at 220 nm.The mobile phase was consisted of acetonitrile-0.1%triethylamine water(1:99,v/v).The liner range for biapenem quantification was 0.05-10.0 mg/mL(r^2= 0.999). The LOD and LOQ of impurity were 4.8 ng(S/N = 3) and 18.5 ng(S/N = 10),respectively.Intra-day RSD of main impurity and total impurity were 1.84%and 3.37%(n = 3);inter-day RSD of main impurity and total impurity were 4.84%and 7.58% (n = 9).The test solution was stable when stored at 4℃for 6 h.The impurity peaks of biapenem can be identified by chromatographic spectral correlation analysis using high-performance liquid chromatography-diode array detection data from the quality control method by calculating correlation coefficients without reference standards.Two hydrolysis degradation products with relative retention times(RRTs) of 0.528 and 0.743,two dimers with RRTs of 1.062 and 2.817 were identified in the quality control chromatogram.It provides a new way to identify impurity peaks by the routine HPLC-UV method.
文摘The model of dislocations was used to construct the model of grain boundary (GB) with pure rare earths, and rare earth elements and impurities. The influence of the interaction between rare earth elements and impurities on the cohesive properties of 5.3° low angle GB of Fe was investigated by the recursion method. The calculated results of environment sensitive embeding energy( E ESE ) show that the preferential segregation of rare earth elements towards GBs exists. Calculations of bond order integrals (BOI) show that rare earth elements increase the cohesive strength of low angle GB, and impurities such as S, P weaken the intergranular cohesion of the GB. So rare earth element of proper quantity added in steel not only cleanses other harmful impurities off the GBs, but also enhances the intergranular cohesion. This elucidates the action mechanism of rare earth elements in steel from electronic level and offers theoretical evidence for applications of rare earth elements in steels.
基金Project(50925417) supported by China National Funds for Distinguished Young ScientistsProject(50830301) supported by the National Natural Science Foundation of China+2 种基金 Project(08JJ3020) supported by the Natural Science Foundation of Hunan Province,ChinaProject(2008SK2007) supported Key Program of Science and Technology of Hunan Province,ChinaPorject(2009ZX07212-001-01) supported by Key Project for Water Pollution Control and Management Technology of China
文摘Effect of impurities in recycling water on Pb-Ag anode passivation in zinc electrowinning process was investigated by linear scan voltammetry.Results show that passivation process would be affected in the presence of Cl^-and F-in recycling water.It was highly advantageous to take H2SO4 concentration as 180g/L,Mn^2+ concentration as 3-5 g/L and F-less than 42mg/L.However,passivation process would not be affected when Cl^-concentration was less than 13mg/L without any other ions,or when mass ratio of Mn^2+ to Cl^-existing in electrolyte was 8,where Cl^-concentration could reach up to 625mg/L.
基金support by the National Natural Scientific Foundation of China(No. 50904023)the Natural Science Research Project of the Education Department of Henan Province (No.2010B450001)+1 种基金the Innovation Scientists and Technicians Troop Construction Projects of Henan Province(No. 104100510005)the Basic and Frontier Technologies Research Projects of Henan Province, China(No. 092300410064)
文摘The role of trivalent antimony was investigated in removing As, Sb, and Bi impurities from a copper electrolyte. Puri- fication experiments were carried out by adding a various concentrations of Sb(III) ions in a synthetic electrolyte containing 185 g/L sulfuric acid, 45 g/L Cu2+, 10 g/L As, and 0.5 g/L Bi under stirring at 65℃ for 2 h. The electrolyte was filtered, and the structure, morphology and composition of the precipitate were analyzed by means of chemical analysis, scanning electron mi- croscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and IR spectroscopy. The precipitate is composed of irregular lumps which are agglomerated by fine dendritic and floccus particles, and it mainly consists of As, Sb, Bi, and O elements. Characteristic bands in the IR spectra of the precipitate are As-OX (X=As, Sb, Bi), Sb-OY (Y=Sb, Bi), O-As-O1 As-OH, Sb-OH, and O-H. The precipitate is a mixture of microcrystalline SbAsQ, (Sb,As)203, and amorphous phases. As, Sb, and Bi impurities are effectively removed from the copper electrolyte by Sb(III) ions attributing to these pre- cipitates.
文摘The binding energy and the photon energy dependence of the photoionization cross-section are calculated for a hydrogenic impurity in GaAs/Ga 1-xAl xAs quantum well wires.The correlation between confined and non-confined direction of the wire in the variational wave function is taken into account.The results show that the photoionization cross-sections are affected by the width of the wire and that their magnitudes are larger than those in infinite potential quantum well wires.In comparison with previous's results,the variational wave function improves the binding energy and decreases the value of photoionization cross-sections of the hydrogenic impurities,which makes the results more reasonable.
基金the Natural Science Foundation of Hunan Province, China (No. 05JJ40017).
文摘A An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.
文摘The purification of metallurgical-grade silicon (MG-Si) has been investigated during electron beam melting (EBM) process. The results show that the phosphorus, calcium and aluminum contents decrease significantly after melting, and magnesium is partially removed. However, no significant change in content for boron and iron has been found. Langmuir's equation and Henry law were used to derive the removal effi-ciency for each impurity element. The free surface temperature was estimated by the Hertz-Knudsen-Langmuir equation and silicon's vapor pressure equation. Good agreement was found between measured and calculated impurities' removal efficiency for phosphorus, calcium and aluminum, magnesium, boron and iron. The deviation between the two results was also analyzed in depth.
基金Project(51674290)supported by the National Natural Science Foundation of ChinaProject(201606370130)supported by the China Scholarship CouncilProject(2016zzts107)supported by the Fundamental Research Funds for the Central Universities of Central South University,China
文摘The effect of grinding on the spodumene flotation was investigated. The flotation response of spodumene ground by different mills was different, due to the variation of metal ions on spodumene surfaces caused by grinding environments and/or impurities. The samples were subjected to acid pickling treatment to remove most of the metal ions from the surfaces, and then all samples showed the same poor flotation response, which confirmed the significance of surface metal ions. Metal ion impurities may come from both grinding environments and lattice substitutions in spodumene. Density functional theory (DFT) calculation revealed that Fe and Ca could exist as lattice substitutions on the spodumene surface while Mg substitution is unlikely to occur. Furthermore, Fe is considered to be active site for the absorption of sodium oleate on the spodumene surface. Morphology analysis showed differences in particle size and shape for samples ground by different mills, resulting in different amounts of exposed surfaces. The particle size, cleavage characteristics caused by grinding environments, and metal ion impurities originated from grinding and isomorphous substitutions, play significant roles in the chemisorption of collector on the spodumene surface.
文摘An effective parameter in the miscible-CO_2 enhanced oil recovery procedure is the minimum miscibility pressure(MMP)defined as the lowest pressure that the oil in place and the injected gas into reservoir achieve miscibility at a given temperature. Flue gases released from power plants can provide an available source of CO_2,which would otherwise be emitted to the atmosphere, for injection into a reservoir. However, the costs related to gas extraction from flue gases is potentially high. Hence, greater understanding the role of impurities in miscibility characteristics between CO_2 and reservoir fluids helps to establish which impurities are tolerable and which are not. In this study, we simulate the effects of the impurities nitrogen(N_2), methane(C_1), ethane(C_2) and propane(C_3) on CO_2 MMP. The simulation results reveal that,as an impurity, nitrogen increases CO_2–oil MMP more so than methane. On the other hand, increasing the propane(C_3)content can lead to a significant decrease in CO_2 MMP, whereas varying the concentrations of ethane(C_2) does not have a significant effect on the minimum miscibility pressure of reservoir crude oil and CO_2 gas. The novel relationships established are particularly valuable in circumstances where MMP experimental data are not available.
基金Project(50725413)supported by the National Natural Science Foundation of ChinaProject(2007CB613704)supported by the National Basic Research Program of ChinaProject(20090191120013)supported by the PhD Program Foundation of Ministry of Education of China
文摘The influence of impurity content on the microstructure and mechanical properties of ZK60 magnesium alloys was investigated by optical microscopy,scanning electron microscopy and tensile test.ZK60 alloys were prepared by changing holding time of alloy melt during semi-continuous casting in order to control the content of impurity elements.The alloy with lower purity content is found to have less second precipitates and larger grain size in the as-cast state.However,in the as-extruded state,reducing impurities brings about a decrease in grain size and an increase in yield strength from 244 MPa to 268 MPa,while the elongations in the as-extruded alloys with different contents of impurities are almost the same.After T5 treatment,impurity content is found to have more obvious effect on the yield strength of ZK60 alloy.The yield strength of ZK60-45 alloys with low impurity content is increased up to 295 MPa after T5 treatment.
基金supported by National Natural Science Foundation of China (Grant No. 51877086)
文摘In this paper, a two-dimensional axisymmetric fluid model was established to investigate the influence of nitrogen impurity content on the discharge pattern and the relevant discharge characteristics in an atmosphere pressure helium dielectric barrier discharge(DBD). The results indicated that when the nitrogen content was increased from 1 to 100 ppm, the discharge pattern evolved from a concentric-ring pattern into a uniform pattern, and then returned to the concentricring pattern. In this process, the discharge mode at the current peak moment transformed from glow mode into Townsend mode, and then returned to glow mode. Further analyses revealed that with the increase of impurity level, the rate of Penning ionization at the pre-ionization stage increased at first and decreased afterwards, resulting in a similar evolution pattern of seed electron level. This evolution trend was believed to be resulted from the competition between the N2 partial pressure and the consumption rate of metastable species. Moreover, the discharge uniformity was found positively correlated with the spatial uniformity of seed electron density as well as the seed electron level. The reason for this correlation was explained by the reduction of radial electric field strength and the promotion of seed electron uniformity as pre-ionization level increases. The results obtained in this work may help better understand the pattern formation mechanism of atmospheric helium DBD under the variation of N2 impurity level, thereby providing a possible means of regulating the discharge performance in practical application scenarios.