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
Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications ...Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications such as solriamfetol,which is used to treat excessive daytime sleepiness.Although the highperformance liquid chromatography analysis of commercial solriamfetol has revealed the presence of several impurities,their synthesis,structure elucidation,and chromatographic determination have not been reported yet.To bridge this gap,we herein identified,synthesized,and isolated eight processrelated solriamfetol impurities,characterized them using spectroscopic and chromatographic techniques,and proposed plausible mechanisms of their formation.Moreover,we developed and validated a prompt impurity analysis method based on ultrahigh-performance liquid chromatography with UV detection,revealing that its selectivity,linearity,accuracy,precision,and quantitation limit meet the acceptance criteria of method validation stipulated by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use.Thus,the developed method was concluded to be suitable for the routine analysis of solriamfetol substances.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
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
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
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
Light-absorbing impurities on glaciers are important factors that influence glacial surface albedo and accelerate glacier melt. In this study, the quantity of light-absorbing impurities on Keqikaer Glacier in western ...Light-absorbing impurities on glaciers are important factors that influence glacial surface albedo and accelerate glacier melt. In this study, the quantity of light-absorbing impurities on Keqikaer Glacier in western Tien Shan, Central Asia, was measured. We found that the average concentrations of black carbon was 2,180 ng/g, with a range from 250 ng/g to more than 10,000 ng/g. The average concentrations of organic carbon and mineral dust were 1,738 ng/g and 194 μg/g, respectively. Based on simulations performed with the Snow Ice Aerosol Radiative model simulations, black carbon and dust are responsible for approximately 64% and 9%, respectively, of the albedo reduction, and are associated with instantaneous radiative forcing of 323.18 W/m2(ranging from 142.16 to 619.25 W/m2) and 24.05 W/m2(ranging from 0.15 to69.77 W/m2), respectively. For different scenarios, the albedo and radiative forcing effect of black carbon is considerably greater than that of dust. The estimated radiative forcing at Keqikaer Glacier is higher than most similar values estimated by previous studies on the Tibetan Plateau, perhaps as a result of black carbon enrichment by melt scavenging. Light-absorbing impurities deposited on Keqikaer Glacier appear to mainly originate from central Asia, Siberia, western China(including the Taklimakan Desert) and parts of South Asia in summer, and from the Middle East and Central Asia in winter.A footprint analysis indicates that a large fraction(>60%) of the black carbon contributions on Keqikaer Glacier comes from anthropogenic sources. These results provide a scientific basis for regional mitigation efforts to reduce black carbon.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
In this paper, we report the results of quality control based in pbysicochemical characteriza- tion and impurities determination of three samples of fluconazole drug substances marketed in Morocco. These samples were ...In this paper, we report the results of quality control based in pbysicochemical characteriza- tion and impurities determination of three samples of fluconazole drug substances marketed in Morocco. These samples were supplied by different pharmaceuticals companies. The sample A, as the discovered product, was supplied by Pfizer, while samples B and C (generics), were manufactured by two different Indian industries. Solid-state characterization of the three samples was realized with different physicochemical methods as: X-ray powder diffraction, Fourier-transformation infrared spectroscopy, differential scanning calorimetry. High performance liquid chromatography was used to quantify the impurities in the different samples. The results from the physicochemical methods cited above, showed difference in polymorph structure of the three drug substances. Sample A consisted in pure polymorph II1, sample B consisted in pure polymorph I1, sample C consisted in a mixture of fluconazole Form Ili, form II and the monohydrate. This result was confirmed by differential scanning calorimetry. Also it was demonstrated that solvents used during the re-crystallization step were among the origins of these differences in the structure form. On the other hand, the result of the stability study under humidity and temperature showed that fluconazole polymorphic transformation could be owed to the no compliance with the conditions of storage. The HPLC analysis of these compounds showed the presence of specific展开更多
An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, ...An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, 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 HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.展开更多
A methodology(HPLC)proposed in this paper for simultaneously quantitative determination of ilaprazole and its related impurities in commercial tablets was developed and validated.The chromatographic separation was car...A methodology(HPLC)proposed in this paper for simultaneously quantitative determination of ilaprazole and its related impurities in commercial tablets was developed and validated.The chromatographic separation was carried out by gradient elution using an Agilent C8 column(4.6 mm×250 mm,5 mm)which was maintained at 25℃.The mobile phase composed of solvent A(methanol)and solvent B(solution consisting 0.02 mmol/l monopotassium phosphate and 0.025 mmol/l sodium hydroxide)was at a flow rate of 1.0 ml/min.The samples were detected and quantified at 237 nm using an ultraviolet absorbance detector.Calibration curves of all analytes from 0.5 to 3.5 mg/ml were good linearity(r≥0.9990)and recovery was greater than 99.5% for each analyte.The lower limit of detection(LLOD)and quantification(LOQ)of this analytical method were 10 ng/ml and 25 ng/ml for all impurities,respectively.The stress studies indicated that the degradation products could not interfere with the detection of ilaprazole and its related impurities and the assay can thus be considered stability-indicating.The method precisions were in the range of 0.41-1.21 while the instrument precisions were in the range of 0.38-0.95 in terms of peak area RSD% for all impurities,respectively.This method is considered stabilityindicating and is applicable for accurate and simultaneous measuring of the ilaprazole and its related impurities in commercial enteric-coated tablets.展开更多
The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry ( HR-ICP-MS ) was investigated. To overcome some poteutially problematic spectral iuter...The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry ( HR-ICP-MS ) was investigated. To overcome some poteutially problematic spectral iuterference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02μg/ g to 6 μg/ g depending on the elements. The experimental resalts for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.展开更多
A novel inductively coupled plasma mass spectrometry method for direct determination of trace rare earth impurities in high purity europium oxide (Eu_2O_3) was developed. The spectral interference,matrix effect,instru...A novel inductively coupled plasma mass spectrometry method for direct determination of trace rare earth impurities in high purity europium oxide (Eu_2O_3) was developed. The spectral interference,matrix effect,instrument parameters fluctuation were investigated and the optimized experimental conditions were established. Under the selected conditions,the detection limits of the method are 3~7 ng·L (-1),the RSD is varied between 2.1%~8.4%,and the percentage recovery is ranged from 90% to 113% for the analytes. The solid detection limit for gross amount of 13 rare earth impurities is 0.19 μg·g (-1) when the matrix (Eu) concentration of 0.1 mg·ml (-1) was chosen. Compared with the reported methods in the literature,this method has several attractive features: simple,small sample amount required,no internal standard and matrix matching requirements.展开更多
A preliminary experiment triggering a plasma current quench by laser ablation of high-Z impurities has been performed in the HL-1M tokamak. The injection of impurities with higher electric charges into tokamak plasmas...A preliminary experiment triggering a plasma current quench by laser ablation of high-Z impurities has been performed in the HL-1M tokamak. The injection of impurities with higher electric charges into tokamak plasmas can increase the radiation cooling of the plasma. Resistive, highly radiating plasma formed prior to the thermal quench can dissipate both the thermal and magnetic energies, which is possibly a simple and potential approach to reducing significantly the plasma thermal energy and magnetic energy before a disruption thereby a safe plasma termination is obtained.展开更多
Covalent organic nanospheres(CONs)were explored as a fiber coating for solid-phase microextraction of genotoxic impurities(GTIs)from active ingredients(AIs).CONs were synthesized by an easy solutionphase procedure at...Covalent organic nanospheres(CONs)were explored as a fiber coating for solid-phase microextraction of genotoxic impurities(GTIs)from active ingredients(AIs).CONs were synthesized by an easy solutionphase procedure at 25℃.The obtained nanospheres exhibited a high specific surface area,good thermostability,high acid and alkali resistance,and favorable crystallinity and porosity.Two types of GTIs,alkyl halides(1-iodooctane,1-chlorobenzene,1-bromododecane,1,2-dichlorobenzene,1-bromooctane,1-chlorohexane,and 1,8-dibromooctane)and sulfonate esters(methyl p-toluenesulfonate and ethyl ptoluenesulfonate),were chosen as target molecules for assessing the performance of the coating.The prepared coating achieved high enhancement factors(5097-9799)for the selected GTIs.The strong affinity between CONs and GTIs was tentatively attributed to π-π and hydrophobicity interactions,large surface area of the CONs,and size-matching of the materials.Combined with gas chromatography-mass spectrometry(GC-MS),the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range(0.2-200 ng/g)with a low detection limit(0.04-2.0 ng/g),satisfactory recovery(80.03%-109.5%),and high repeatability(6.20%-14.8%)and reproducibility(6.20%-14.1%).Therefore,the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.展开更多
Highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of five potential genotoxic impurities in ranolazine active pharmaceutical ingred...Highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of five potential genotoxic impurities in ranolazine active pharmaceutical ingredient. Chromatographic separation achieved using Poroshell C18 PFP 150 × 3.0 mm 2.7 μ column and 0.1% formic acid in water as Mobile phase A and 0.1% formic acid in methanol as mobile phase B using gradient elution and a flow rate of 0.4 ml/min with a run time of 18 minutes. Mass spectrometric conditions were optimized using electrospray ionization in positive mode. Method shows excellent linearity from 0.05 - 5.0 ppm of the ranolazine test concentration for all the five impurities. The correlation coefficient was observed greater than 0.99. Satisfactory recoveries were observed for all the five impurities within the range of 102.9% - 112.3%. Method has been validated as per ICH recommended guidelines with a LOQ of 0.15 ppm achieved. The developed method was able to quantify all the five impurities at a concentration level of 1 ng/ml (0.5 ppm with respect to 2 mg/ml ranolazine).展开更多
Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studi...Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi- peridin-3-ol (Ben-2), which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.展开更多
The removal of metallic impurities from off-grade copper concentrate was investigated in alkaline solution with H2O2. The analysis results of XRD and SEM-EDS revealed the oxidative mechanisms of all sulfides. The infl...The removal of metallic impurities from off-grade copper concentrate was investigated in alkaline solution with H2O2. The analysis results of XRD and SEM-EDS revealed the oxidative mechanisms of all sulfides. The influence of various parameters of alkaline leaching were investigated including concentrations of sodium hydroxide and hydrogen peroxide, liquid to solid ratio, leaching time and temperature. The results showed that the removal rate of Mo, As and Zn were increased with increasing leaching time and H2O2 concentration, and that the removal rate of Mo, As and Zn were firstly increased and then slightly decreased with increasing liquid to solid ratio, temperature and NaOH concentration, respectively. More than 95% Mo, 94% As, and 94 % Zn are removed from the off-grade concentrate under the optimum conditions, while only 1.7% Cu is dissolved. These optimum conditions were sodium hydroxide 1.5 mol/L, hydrogen peroxide 1.0 mol/L, temperature 50°C, liquid to solid ratio 5/1 mL/g and leaching time 5 h.展开更多
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This research was funded by the Deanship of Scientific Research at the German-Jordanian University and the Deanship of Scientific Research at Zarqa University.The graphical abstract was created with BioRender software.
文摘Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications such as solriamfetol,which is used to treat excessive daytime sleepiness.Although the highperformance liquid chromatography analysis of commercial solriamfetol has revealed the presence of several impurities,their synthesis,structure elucidation,and chromatographic determination have not been reported yet.To bridge this gap,we herein identified,synthesized,and isolated eight processrelated solriamfetol impurities,characterized them using spectroscopic and chromatographic techniques,and proposed plausible mechanisms of their formation.Moreover,we developed and validated a prompt impurity analysis method based on ultrahigh-performance liquid chromatography with UV detection,revealing that its selectivity,linearity,accuracy,precision,and quantitation limit meet the acceptance criteria of method validation stipulated by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use.Thus,the developed method was concluded to be suitable for the routine analysis of solriamfetol substances.
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.
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.
基金supported by the National Natural Science Foundation of China (41630754, 41671067, and 41501063)the Chinese Academy of Sciences (KJZD-EW-G03-04), the State Key Laboratory of Cryosphere Science (SKLCS-ZZ-2015)the Foundation for Excellent Youth Scholars of Northwest Institute of Eco-Environment and Resources, CAS
文摘Light-absorbing impurities on glaciers are important factors that influence glacial surface albedo and accelerate glacier melt. In this study, the quantity of light-absorbing impurities on Keqikaer Glacier in western Tien Shan, Central Asia, was measured. We found that the average concentrations of black carbon was 2,180 ng/g, with a range from 250 ng/g to more than 10,000 ng/g. The average concentrations of organic carbon and mineral dust were 1,738 ng/g and 194 μg/g, respectively. Based on simulations performed with the Snow Ice Aerosol Radiative model simulations, black carbon and dust are responsible for approximately 64% and 9%, respectively, of the albedo reduction, and are associated with instantaneous radiative forcing of 323.18 W/m2(ranging from 142.16 to 619.25 W/m2) and 24.05 W/m2(ranging from 0.15 to69.77 W/m2), respectively. For different scenarios, the albedo and radiative forcing effect of black carbon is considerably greater than that of dust. The estimated radiative forcing at Keqikaer Glacier is higher than most similar values estimated by previous studies on the Tibetan Plateau, perhaps as a result of black carbon enrichment by melt scavenging. Light-absorbing impurities deposited on Keqikaer Glacier appear to mainly originate from central Asia, Siberia, western China(including the Taklimakan Desert) and parts of South Asia in summer, and from the Middle East and Central Asia in winter.A footprint analysis indicates that a large fraction(>60%) of the black carbon contributions on Keqikaer Glacier comes from anthropogenic sources. These results provide a scientific basis for regional mitigation efforts to reduce black carbon.
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.
文摘In this paper, we report the results of quality control based in pbysicochemical characteriza- tion and impurities determination of three samples of fluconazole drug substances marketed in Morocco. These samples were supplied by different pharmaceuticals companies. The sample A, as the discovered product, was supplied by Pfizer, while samples B and C (generics), were manufactured by two different Indian industries. Solid-state characterization of the three samples was realized with different physicochemical methods as: X-ray powder diffraction, Fourier-transformation infrared spectroscopy, differential scanning calorimetry. High performance liquid chromatography was used to quantify the impurities in the different samples. The results from the physicochemical methods cited above, showed difference in polymorph structure of the three drug substances. Sample A consisted in pure polymorph II1, sample B consisted in pure polymorph I1, sample C consisted in a mixture of fluconazole Form Ili, form II and the monohydrate. This result was confirmed by differential scanning calorimetry. Also it was demonstrated that solvents used during the re-crystallization step were among the origins of these differences in the structure form. On the other hand, the result of the stability study under humidity and temperature showed that fluconazole polymorphic transformation could be owed to the no compliance with the conditions of storage. The HPLC analysis of these compounds showed the presence of specific
基金supported by the Natural Science Foundation of Hunan Province(No.05JJ40017)Education Department of Hunan Province(No.05B064).
文摘An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, 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 HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.
文摘A methodology(HPLC)proposed in this paper for simultaneously quantitative determination of ilaprazole and its related impurities in commercial tablets was developed and validated.The chromatographic separation was carried out by gradient elution using an Agilent C8 column(4.6 mm×250 mm,5 mm)which was maintained at 25℃.The mobile phase composed of solvent A(methanol)and solvent B(solution consisting 0.02 mmol/l monopotassium phosphate and 0.025 mmol/l sodium hydroxide)was at a flow rate of 1.0 ml/min.The samples were detected and quantified at 237 nm using an ultraviolet absorbance detector.Calibration curves of all analytes from 0.5 to 3.5 mg/ml were good linearity(r≥0.9990)and recovery was greater than 99.5% for each analyte.The lower limit of detection(LLOD)and quantification(LOQ)of this analytical method were 10 ng/ml and 25 ng/ml for all impurities,respectively.The stress studies indicated that the degradation products could not interfere with the detection of ilaprazole and its related impurities and the assay can thus be considered stability-indicating.The method precisions were in the range of 0.41-1.21 while the instrument precisions were in the range of 0.38-0.95 in terms of peak area RSD% for all impurities,respectively.This method is considered stabilityindicating and is applicable for accurate and simultaneous measuring of the ilaprazole and its related impurities in commercial enteric-coated tablets.
文摘The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry ( HR-ICP-MS ) was investigated. To overcome some poteutially problematic spectral iuterference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02μg/ g to 6 μg/ g depending on the elements. The experimental resalts for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.
文摘A novel inductively coupled plasma mass spectrometry method for direct determination of trace rare earth impurities in high purity europium oxide (Eu_2O_3) was developed. The spectral interference,matrix effect,instrument parameters fluctuation were investigated and the optimized experimental conditions were established. Under the selected conditions,the detection limits of the method are 3~7 ng·L (-1),the RSD is varied between 2.1%~8.4%,and the percentage recovery is ranged from 90% to 113% for the analytes. The solid detection limit for gross amount of 13 rare earth impurities is 0.19 μg·g (-1) when the matrix (Eu) concentration of 0.1 mg·ml (-1) was chosen. Compared with the reported methods in the literature,this method has several attractive features: simple,small sample amount required,no internal standard and matrix matching requirements.
基金Project supported by IAEA International Science Foundation (Grant No IS 105123).
文摘A preliminary experiment triggering a plasma current quench by laser ablation of high-Z impurities has been performed in the HL-1M tokamak. The injection of impurities with higher electric charges into tokamak plasmas can increase the radiation cooling of the plasma. Resistive, highly radiating plasma formed prior to the thermal quench can dissipate both the thermal and magnetic energies, which is possibly a simple and potential approach to reducing significantly the plasma thermal energy and magnetic energy before a disruption thereby a safe plasma termination is obtained.
基金supported by the Key Research and Development Program of Shandong Province(Grant No.:2019GSF111001)the National Natural Science Foundation of China(Grant No.:21906096)+2 种基金the Youth Science Funds of the Shandong Academy of Sciences(Grant No.:2019QN009)the Youth Ph.D.Cooperation Funds of Qilu University of Technology(Shandong Academy of Sciences,Grant No.:2018BSHZ0029)the Program for Taishan Scholars of Shandong Province(Grant No.:tsqn202103099).
文摘Covalent organic nanospheres(CONs)were explored as a fiber coating for solid-phase microextraction of genotoxic impurities(GTIs)from active ingredients(AIs).CONs were synthesized by an easy solutionphase procedure at 25℃.The obtained nanospheres exhibited a high specific surface area,good thermostability,high acid and alkali resistance,and favorable crystallinity and porosity.Two types of GTIs,alkyl halides(1-iodooctane,1-chlorobenzene,1-bromododecane,1,2-dichlorobenzene,1-bromooctane,1-chlorohexane,and 1,8-dibromooctane)and sulfonate esters(methyl p-toluenesulfonate and ethyl ptoluenesulfonate),were chosen as target molecules for assessing the performance of the coating.The prepared coating achieved high enhancement factors(5097-9799)for the selected GTIs.The strong affinity between CONs and GTIs was tentatively attributed to π-π and hydrophobicity interactions,large surface area of the CONs,and size-matching of the materials.Combined with gas chromatography-mass spectrometry(GC-MS),the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range(0.2-200 ng/g)with a low detection limit(0.04-2.0 ng/g),satisfactory recovery(80.03%-109.5%),and high repeatability(6.20%-14.8%)and reproducibility(6.20%-14.1%).Therefore,the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.
文摘Highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of five potential genotoxic impurities in ranolazine active pharmaceutical ingredient. Chromatographic separation achieved using Poroshell C18 PFP 150 × 3.0 mm 2.7 μ column and 0.1% formic acid in water as Mobile phase A and 0.1% formic acid in methanol as mobile phase B using gradient elution and a flow rate of 0.4 ml/min with a run time of 18 minutes. Mass spectrometric conditions were optimized using electrospray ionization in positive mode. Method shows excellent linearity from 0.05 - 5.0 ppm of the ranolazine test concentration for all the five impurities. The correlation coefficient was observed greater than 0.99. Satisfactory recoveries were observed for all the five impurities within the range of 102.9% - 112.3%. Method has been validated as per ICH recommended guidelines with a LOQ of 0.15 ppm achieved. The developed method was able to quantify all the five impurities at a concentration level of 1 ng/ml (0.5 ppm with respect to 2 mg/ml ranolazine).
基金the management of Deva Holding A.S., Istanbul, Turkey, for supporting this workthe Scientific and Technological Research Council of Turkey (TUBITAK-TEYDEB Project no: 3110426) for the financial support
文摘Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi- peridin-3-ol (Ben-2), which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.
文摘The removal of metallic impurities from off-grade copper concentrate was investigated in alkaline solution with H2O2. The analysis results of XRD and SEM-EDS revealed the oxidative mechanisms of all sulfides. The influence of various parameters of alkaline leaching were investigated including concentrations of sodium hydroxide and hydrogen peroxide, liquid to solid ratio, leaching time and temperature. The results showed that the removal rate of Mo, As and Zn were increased with increasing leaching time and H2O2 concentration, and that the removal rate of Mo, As and Zn were firstly increased and then slightly decreased with increasing liquid to solid ratio, temperature and NaOH concentration, respectively. More than 95% Mo, 94% As, and 94 % Zn are removed from the off-grade concentrate under the optimum conditions, while only 1.7% Cu is dissolved. These optimum conditions were sodium hydroxide 1.5 mol/L, hydrogen peroxide 1.0 mol/L, temperature 50°C, liquid to solid ratio 5/1 mL/g and leaching time 5 h.