为了实现致密岩心的孔隙量化表征,采用核磁共振(nuclear magnetic resonance,NMR)技术,利用T2弛豫时间和孔隙半径(r)的正比关系可测致密岩心的孔隙度、渗透率和孔径分布,利用核磁共振T2截止值可区分孔隙中的自由流体和束缚流体。从核磁...为了实现致密岩心的孔隙量化表征,采用核磁共振(nuclear magnetic resonance,NMR)技术,利用T2弛豫时间和孔隙半径(r)的正比关系可测致密岩心的孔隙度、渗透率和孔径分布,利用核磁共振T2截止值可区分孔隙中的自由流体和束缚流体。从核磁共振表征岩心孔隙的原理出发,分析了核磁共振T2谱与岩心孔隙度、渗透率、孔径分布、孔隙内可动流体的关系。根据上述原理,通过实例验证了核磁共振技术在致密岩心孔隙度和渗透率量化表征中的准确性和适用性。实验岩心的T2截止值和孔径分布测试表明:1号岩心T2截止值为21.85 ms,2号岩心的T2截止值为40.11 ms;1号岩心小孔隙分量大,2号岩心孔隙分布较均匀。截止值的计算结果表明地区经验法得出的T2截止值不完全适用于该区域的致密岩心,有必要建立区域性的截止值变化范围图版。展开更多
A series of triple hierarchical micro-mesomacroporous N-doped carbon shells with hollow cores have been successfully prepared via etching N-doped hollow carbon spheres with CO_2 at high temperatures.The surface areas,...A series of triple hierarchical micro-mesomacroporous N-doped carbon shells with hollow cores have been successfully prepared via etching N-doped hollow carbon spheres with CO_2 at high temperatures.The surface areas, total pore volumes and microporepercentages of the CO_2-activated samples evidently increase with increasing activation temperature from 800 to950 °C, while the N contents show a contrary trend from7.6 to 3.8 at%. The pyridinic and graphitic nitrogen groups are dominant among various N-containing groups in the samples. The 950 °C-activated sample(CANHCS-950) has the largest surface area(2072 m^2 g^(-1)), pore volume(1.96 cm^3 g^(-1)), hierarchical micro-mesopore distributions(1.2, 2.6 and 6.2 nm), hollow macropore cores(*91 nm)and highest relative content of pyridinic and graphitic N groups. This triple micro-meso-macropore system could synergistically enhance the activity because macropores could store up the reactant, mesopores could reduce the transport resistance of the reactants to the active sites, and micropores could be in favor of the accumulation of ions.Therefore, the CANHCS-950 with optimized structure shows the optimal and comparable oxygen reduction reaction(ORR) activity but superior methanol tolerance and long-term durability to commercial Pt/C with a 4 e--dominant transfer pathway in alkaline media. These excellent properties in combination with good stability and recyclability make CANHCSs among the most promising metal-free ORR electrocatalysts reported so far in practical applications.展开更多
As part of the method development, the injection volume as a critical quality attribute in fast fused-core chromatography was evaluated. Spilanthol, a pharmaceutically interesting N- alkylamide currently under investi...As part of the method development, the injection volume as a critical quality attribute in fast fused-core chromatography was evaluated. Spilanthol, a pharmaceutically interesting N- alkylamide currently under investigation in our laboratory, was chosen as the model compound. Spilanthol was dissolved in both PBS and MeOH/H20 （70/30, v/v） and subsequently analyzed using a fused-core system hereby selecting five chromatographic characteristics （retention time, area, height, theoretical plates and symmetry factor） as responses. We demonstrated that the injection volume significantly influenced both the qualitative and quantitative performance of fused-core chromatography, a phenomenon which is confounded with the nature of the used sample solvent. From 2 ~tL up to 100 laL injection volume with PBS as solvent, the symmetry factor decreased favorably by 20%. Moreover, the theoretical plates and the quantitative parameters （area and height） increased up to 30%. On the contrary, in this injection volume range, the theoretical plates for the methanol-based samples decreased by more than 60%, while the symmetry factor increased and the height decreased, both by 30%. The injection volume is thus a critical and often overlooked parameter in fused-core method description and validation.展开更多
文摘为了实现致密岩心的孔隙量化表征,采用核磁共振(nuclear magnetic resonance,NMR)技术,利用T2弛豫时间和孔隙半径(r)的正比关系可测致密岩心的孔隙度、渗透率和孔径分布,利用核磁共振T2截止值可区分孔隙中的自由流体和束缚流体。从核磁共振表征岩心孔隙的原理出发,分析了核磁共振T2谱与岩心孔隙度、渗透率、孔径分布、孔隙内可动流体的关系。根据上述原理,通过实例验证了核磁共振技术在致密岩心孔隙度和渗透率量化表征中的准确性和适用性。实验岩心的T2截止值和孔径分布测试表明:1号岩心T2截止值为21.85 ms,2号岩心的T2截止值为40.11 ms;1号岩心小孔隙分量大,2号岩心孔隙分布较均匀。截止值的计算结果表明地区经验法得出的T2截止值不完全适用于该区域的致密岩心,有必要建立区域性的截止值变化范围图版。
基金the financial support from the National Key Research and Development Program of China(2016YFB0700204)NSFC(51502327,51602332)+1 种基金Science and Technology Commission of Shanghai Municipality(15520720400,15YF1413800,14DZ2261203 and 16DZ2260603)Key Project for Young Researcher of State Key Laboratory of High Performance Ceramics and Superfine Microstructure and One Hundred Talent Plan of Chinese Academy of Sciences
文摘A series of triple hierarchical micro-mesomacroporous N-doped carbon shells with hollow cores have been successfully prepared via etching N-doped hollow carbon spheres with CO_2 at high temperatures.The surface areas, total pore volumes and microporepercentages of the CO_2-activated samples evidently increase with increasing activation temperature from 800 to950 °C, while the N contents show a contrary trend from7.6 to 3.8 at%. The pyridinic and graphitic nitrogen groups are dominant among various N-containing groups in the samples. The 950 °C-activated sample(CANHCS-950) has the largest surface area(2072 m^2 g^(-1)), pore volume(1.96 cm^3 g^(-1)), hierarchical micro-mesopore distributions(1.2, 2.6 and 6.2 nm), hollow macropore cores(*91 nm)and highest relative content of pyridinic and graphitic N groups. This triple micro-meso-macropore system could synergistically enhance the activity because macropores could store up the reactant, mesopores could reduce the transport resistance of the reactants to the active sites, and micropores could be in favor of the accumulation of ions.Therefore, the CANHCS-950 with optimized structure shows the optimal and comparable oxygen reduction reaction(ORR) activity but superior methanol tolerance and long-term durability to commercial Pt/C with a 4 e--dominant transfer pathway in alkaline media. These excellent properties in combination with good stability and recyclability make CANHCSs among the most promising metal-free ORR electrocatalysts reported so far in practical applications.
基金funded by the "Institute for the Promotion of Innovation through Science and Technology in Flanders (IWT-Vlaanderen)’’ to Jente Boonen(No.091257) and to Matthias D’Hondt(No.101529)
文摘As part of the method development, the injection volume as a critical quality attribute in fast fused-core chromatography was evaluated. Spilanthol, a pharmaceutically interesting N- alkylamide currently under investigation in our laboratory, was chosen as the model compound. Spilanthol was dissolved in both PBS and MeOH/H20 （70/30, v/v） and subsequently analyzed using a fused-core system hereby selecting five chromatographic characteristics （retention time, area, height, theoretical plates and symmetry factor） as responses. We demonstrated that the injection volume significantly influenced both the qualitative and quantitative performance of fused-core chromatography, a phenomenon which is confounded with the nature of the used sample solvent. From 2 ~tL up to 100 laL injection volume with PBS as solvent, the symmetry factor decreased favorably by 20%. Moreover, the theoretical plates and the quantitative parameters （area and height） increased up to 30%. On the contrary, in this injection volume range, the theoretical plates for the methanol-based samples decreased by more than 60%, while the symmetry factor increased and the height decreased, both by 30%. The injection volume is thus a critical and often overlooked parameter in fused-core method description and validation.
