有机锡化合物已广泛应用于食品包装材料及其生产过程中,对人体健康存在着潜在的危害。特别是食用植物油因甘油三酯(脂肪)含量较高,约占植物油的95%以上,给分析检测带来较大的基体干扰。本文采用低温冷冻提取结合固相萃取技术,建立了高...有机锡化合物已广泛应用于食品包装材料及其生产过程中,对人体健康存在着潜在的危害。特别是食用植物油因甘油三酯(脂肪)含量较高,约占植物油的95%以上,给分析检测带来较大的基体干扰。本文采用低温冷冻提取结合固相萃取技术,建立了高效液相色谱-串联质谱法同时测定食用植物油样品中二丁基二氯化锡、二苯基二氯化锡、三丁基氯化锡、三苯基氯化锡同时分析的方法。实验对比了甲醇、乙腈、乙醇三种有机萃取溶剂分别在低温冷冻提取和常规液液振荡提取条件下的提取效率,并考察了PSA、中性氧化铝、弗罗里硅土及活性炭四种净化材料对食用油提取液的净化效果。确定了食用油中有机锡化合物的最佳提取净化方案为:以10 m L甲醇为提取溶剂在低温冷冻条件下充分提取两次,并通过50 mg活性炭净化提取液。为评价该方法的准确性,对食用油样品进行三个不同水平的添加回收实验,各有机锡化合物的平均回收率在74.2%~99.5%之间,接近或优于现行国标及相关研究(70%~120%),可应用于菜籽油、花生油、芝麻油、大豆油、玉米油及调和油等不同基质的食用植物油中有机锡化合物的同时测定。展开更多
Li[Li0.2Ni0.13Coo.13Mn0.54]O2 cathode materials were synthesized by carbonate-based co-precipitation method, and then, its surface was coated by thin layers of FePO4. The prepared samples were characterized by X-ray d...Li[Li0.2Ni0.13Coo.13Mn0.54]O2 cathode materials were synthesized by carbonate-based co-precipitation method, and then, its surface was coated by thin layers of FePO4. The prepared samples were characterized by X-ray diffraction （XRD）, field emission scanning electron micro- scope （FESEM）, energy-dispersive spectroscopy （EDS）, and transmission electron microscopy （TEM）. The XRD and TEM results suggest that both the pristine and the coated materials have a hexagonal layered structure, and the FePO4 coating layer does not make any major change in the crystal structure. The FePO4-coated sample exhibits both improved initial discharge capacity and columbic efficiency compared to the pristine one. More significantly, the FePO4 coating layer has a much positive influence on the cycling perfor- mance. The FePO4-coated sample exhibits capacity reten- tion of 82 % after 100 cycles at 0.5℃ between 2.0 and 4.8 V, while only 28 % for the pristine one at the same charge-discharge condition. The electrochemical impe- dance spectroscopy （EIS） results indicate that this improved cycling performance could be ascribed to the presence of FePO4 on the surface of Li[Li0.2Ni0.13Co0.13Mno.54102 par- ticle, which helps to protect the cathode from chemical attacks by HF and thus suppresses the large increase in charge transfer resistance.展开更多
为了更加高效准确地评价沥青质分散剂,首次利用测定掺稀后黏度变化的实验方法取代现有沉淀评价方法,结合对现有市售分散剂的评价结果,分析了原有方法的缺点与不足。利用新方法探索了不同基团、链长、结构对分散剂分散性能的影响。结果表...为了更加高效准确地评价沥青质分散剂,首次利用测定掺稀后黏度变化的实验方法取代现有沉淀评价方法,结合对现有市售分散剂的评价结果,分析了原有方法的缺点与不足。利用新方法探索了不同基团、链长、结构对分散剂分散性能的影响。结果表明,在用沉淀法测定时,强极性的烷基苯磺酸和长链离子液体分散剂出现增稠现象。针对塔河某掺稀井最为合适的沥青质分散剂应是具有C18烷基链长、含有2~4个极性头基团的多胺类非离子型表面活性剂。在此基础上,以油酸和二乙烯三胺合成了新型的长链烷基酰胺二胺型沥青质分散剂。通过掺稀黏度法测得,新合成的分散剂与沥青混合液在30、60℃下的平均黏度为890和277 m Pa·s,比常用的Span80多元醇类分散剂分别提高27%和46%。展开更多
Amorphous solid dispersions(ASDs)are popular for enhancing the solubility and bioavailability of poorly water-soluble drugs.Various approaches have been employed to produce ASDs and novel techniques are emerging.This ...Amorphous solid dispersions(ASDs)are popular for enhancing the solubility and bioavailability of poorly water-soluble drugs.Various approaches have been employed to produce ASDs and novel techniques are emerging.This review provides an updated overview of manufacturing techniques for preparing ASDs.As physical stability is a critical quality attribute for ASD,the impact of formulation,equipment,and process variables,together with the downstream processing on physical stability of ASDs have been discussed.Selection strategies are proposed to identify suitable manufacturing methods,which may aid in the development of ASDs with satisfactory physical stability.展开更多
As the efficiency of dispersants with different origins is questionable for each typical oil sample, the present study provides a reproducible and reliable method for screening asphaltene dispersants for a typical asp...As the efficiency of dispersants with different origins is questionable for each typical oil sample, the present study provides a reproducible and reliable method for screening asphaltene dispersants for a typical asphal- tenic crude oil. Four different asphaltene dispersants （polyisobutylene succinimide, polyisobutylene succinic ester, nonylphenol-formaldehyde resin modified by polyamines, and rapeseed oil amide） were prepared and their performance on two oils from an Iranian field under laboratory and reservoir conditions was studied. A thorough analysis including ash content and SARA tests was performed on the solid asphaltene particles to characterize the nature of deposits. Then a highly efficient carrier fluid, which is crucial when injecting dispersant into the wells, was selected from a variety of chemicals by comparing their solubility. In the next step, using an optical microscope, a viscometer, and a Turbiscan, the screening of dispersants under laboratory conditions was done on a mixture of dead oil and dispersant to evaluate the onset of asphaltene precipitation and its stability when titrating by a precipitant. Finally, two different mixtures of the efficient dispersants, live oil, and carrier fluid were used with the solid detection system （SDS） and the filtration method to examine their effects on the onset pressure of asphaltene precipitation and the asphaltene content of the crude oil under reservoir conditions. The results show that the combination of experimental methods used in this work could be consistently applied to screening asphaltene dispersants. Among the four different dispersants applied here, the dispersant based on nonylphenol-formaldehyde resin modified by polyamines showed the best performance on the available live oils. This chemical modified the onset pressure of asphaltene precipitation of light oil from 4300 psi to about 3600 psi and decreased the precipitated asphaltene of heavy oil by about 30 %.展开更多
The influence of the precipitating reagents and dispersants on the formation of nano-aluminum hydroxide from sodium aluminate solution by chemical precipitation was investigated. The influence of the dispersed seeds o...The influence of the precipitating reagents and dispersants on the formation of nano-aluminum hydroxide from sodium aluminate solution by chemical precipitation was investigated. The influence of the dispersed seeds on the decomposi-tion process was investigated too. The alkaline aluminate solutions were used as original solutions with a concentration of Al2O3 having 14.78 g/dm3, αk—1.6 and127 g/dm3, αk—1.6. For the precipitation processes there were used follow-ing precipitating reagents—solutions HCl, NaHCO3 and NH4HCO3 with a concentration of 80 g/dm3, dispersants—PEG 6000, (NaPO3)6 and Tween 20. For the decomposition process the dispersed seeds and factories seeds were used. Structural studies of the aluminum hydroxide particles were carried out by means of the electron-probe microanalysis and scanning electron microscopy, and phase composition of products was determined by means of X-ray diffraction analysis. Ammonium bicarbonate and Tween 20 were determined as the optimal precipitating reagent and dispersant, correspondingly, resulting in dispersed aluminum hydroxide, which is used as a seed in the decomposition process. It was established that this product in form of dispersed seed considerably reduces the duration of the decomposition process;the maximal decomposition of solution (73.9%) was observed after injection of dispersеd aluminum hydroxide into solution. The final aluminum hydroxide having 90% of particles less than 100 nanometers was obtained within 7 hours of steady decreasing temperature from 70°C to 48°C.展开更多
文摘有机锡化合物已广泛应用于食品包装材料及其生产过程中,对人体健康存在着潜在的危害。特别是食用植物油因甘油三酯(脂肪)含量较高,约占植物油的95%以上,给分析检测带来较大的基体干扰。本文采用低温冷冻提取结合固相萃取技术,建立了高效液相色谱-串联质谱法同时测定食用植物油样品中二丁基二氯化锡、二苯基二氯化锡、三丁基氯化锡、三苯基氯化锡同时分析的方法。实验对比了甲醇、乙腈、乙醇三种有机萃取溶剂分别在低温冷冻提取和常规液液振荡提取条件下的提取效率,并考察了PSA、中性氧化铝、弗罗里硅土及活性炭四种净化材料对食用油提取液的净化效果。确定了食用油中有机锡化合物的最佳提取净化方案为:以10 m L甲醇为提取溶剂在低温冷冻条件下充分提取两次,并通过50 mg活性炭净化提取液。为评价该方法的准确性,对食用油样品进行三个不同水平的添加回收实验,各有机锡化合物的平均回收率在74.2%~99.5%之间,接近或优于现行国标及相关研究(70%~120%),可应用于菜籽油、花生油、芝麻油、大豆油、玉米油及调和油等不同基质的食用植物油中有机锡化合物的同时测定。
基金financially supported by the National Nature Science Foundation of China (No.51302017)the National High Technology Research and Development Program of China (No.2012AA110102)the fund from the Science and Technology Commission of Beijing (No.2121100006712002)
文摘Li[Li0.2Ni0.13Coo.13Mn0.54]O2 cathode materials were synthesized by carbonate-based co-precipitation method, and then, its surface was coated by thin layers of FePO4. The prepared samples were characterized by X-ray diffraction （XRD）, field emission scanning electron micro- scope （FESEM）, energy-dispersive spectroscopy （EDS）, and transmission electron microscopy （TEM）. The XRD and TEM results suggest that both the pristine and the coated materials have a hexagonal layered structure, and the FePO4 coating layer does not make any major change in the crystal structure. The FePO4-coated sample exhibits both improved initial discharge capacity and columbic efficiency compared to the pristine one. More significantly, the FePO4 coating layer has a much positive influence on the cycling perfor- mance. The FePO4-coated sample exhibits capacity reten- tion of 82 % after 100 cycles at 0.5℃ between 2.0 and 4.8 V, while only 28 % for the pristine one at the same charge-discharge condition. The electrochemical impe- dance spectroscopy （EIS） results indicate that this improved cycling performance could be ascribed to the presence of FePO4 on the surface of Li[Li0.2Ni0.13Co0.13Mno.54102 par- ticle, which helps to protect the cathode from chemical attacks by HF and thus suppresses the large increase in charge transfer resistance.
文摘为了更加高效准确地评价沥青质分散剂,首次利用测定掺稀后黏度变化的实验方法取代现有沉淀评价方法,结合对现有市售分散剂的评价结果,分析了原有方法的缺点与不足。利用新方法探索了不同基团、链长、结构对分散剂分散性能的影响。结果表明,在用沉淀法测定时,强极性的烷基苯磺酸和长链离子液体分散剂出现增稠现象。针对塔河某掺稀井最为合适的沥青质分散剂应是具有C18烷基链长、含有2~4个极性头基团的多胺类非离子型表面活性剂。在此基础上,以油酸和二乙烯三胺合成了新型的长链烷基酰胺二胺型沥青质分散剂。通过掺稀黏度法测得,新合成的分散剂与沥青混合液在30、60℃下的平均黏度为890和277 m Pa·s,比常用的Span80多元醇类分散剂分别提高27%和46%。
基金supported,in whole or in part,by the Bill&Melinda Gates Foundation[No.OPP1159809,USA]supported by the National Institute of Allergy and Infectious Diseases of the National Institutes of Health under Award(No.R01AI132681,USA)
文摘Amorphous solid dispersions(ASDs)are popular for enhancing the solubility and bioavailability of poorly water-soluble drugs.Various approaches have been employed to produce ASDs and novel techniques are emerging.This review provides an updated overview of manufacturing techniques for preparing ASDs.As physical stability is a critical quality attribute for ASD,the impact of formulation,equipment,and process variables,together with the downstream processing on physical stability of ASDs have been discussed.Selection strategies are proposed to identify suitable manufacturing methods,which may aid in the development of ASDs with satisfactory physical stability.
文摘As the efficiency of dispersants with different origins is questionable for each typical oil sample, the present study provides a reproducible and reliable method for screening asphaltene dispersants for a typical asphal- tenic crude oil. Four different asphaltene dispersants （polyisobutylene succinimide, polyisobutylene succinic ester, nonylphenol-formaldehyde resin modified by polyamines, and rapeseed oil amide） were prepared and their performance on two oils from an Iranian field under laboratory and reservoir conditions was studied. A thorough analysis including ash content and SARA tests was performed on the solid asphaltene particles to characterize the nature of deposits. Then a highly efficient carrier fluid, which is crucial when injecting dispersant into the wells, was selected from a variety of chemicals by comparing their solubility. In the next step, using an optical microscope, a viscometer, and a Turbiscan, the screening of dispersants under laboratory conditions was done on a mixture of dead oil and dispersant to evaluate the onset of asphaltene precipitation and its stability when titrating by a precipitant. Finally, two different mixtures of the efficient dispersants, live oil, and carrier fluid were used with the solid detection system （SDS） and the filtration method to examine their effects on the onset pressure of asphaltene precipitation and the asphaltene content of the crude oil under reservoir conditions. The results show that the combination of experimental methods used in this work could be consistently applied to screening asphaltene dispersants. Among the four different dispersants applied here, the dispersant based on nonylphenol-formaldehyde resin modified by polyamines showed the best performance on the available live oils. This chemical modified the onset pressure of asphaltene precipitation of light oil from 4300 psi to about 3600 psi and decreased the precipitated asphaltene of heavy oil by about 30 %.
文摘The influence of the precipitating reagents and dispersants on the formation of nano-aluminum hydroxide from sodium aluminate solution by chemical precipitation was investigated. The influence of the dispersed seeds on the decomposi-tion process was investigated too. The alkaline aluminate solutions were used as original solutions with a concentration of Al2O3 having 14.78 g/dm3, αk—1.6 and127 g/dm3, αk—1.6. For the precipitation processes there were used follow-ing precipitating reagents—solutions HCl, NaHCO3 and NH4HCO3 with a concentration of 80 g/dm3, dispersants—PEG 6000, (NaPO3)6 and Tween 20. For the decomposition process the dispersed seeds and factories seeds were used. Structural studies of the aluminum hydroxide particles were carried out by means of the electron-probe microanalysis and scanning electron microscopy, and phase composition of products was determined by means of X-ray diffraction analysis. Ammonium bicarbonate and Tween 20 were determined as the optimal precipitating reagent and dispersant, correspondingly, resulting in dispersed aluminum hydroxide, which is used as a seed in the decomposition process. It was established that this product in form of dispersed seed considerably reduces the duration of the decomposition process;the maximal decomposition of solution (73.9%) was observed after injection of dispersеd aluminum hydroxide into solution. The final aluminum hydroxide having 90% of particles less than 100 nanometers was obtained within 7 hours of steady decreasing temperature from 70°C to 48°C.
