Synthesis of large pore-diameter SBA-15 mesostructured spherical silica and its application in ultra-high-performance liquid chromatography

A modified synthesis approach for spherical large pore-diameter SBA-15 mesoporous silica (SLP-SBA-15) with particle size range of 0.5–1 μm was being reported. It was worth mentioning that in this improved methodology, the use of cetyltrimethylammonium bromide (CTAB) as co-template significantly reduced the self-assembly time from 24 h to 45 min. Moreover, under reflux condition, the reaction time could be further shortened by reducing the aging time from 48 h to 6 h. The resultant SLP-SBA-15 was thereafter successfully functionalized and packed into an ultra-high-performance liquid chromatography (UHPLC) column for the separation of aromatic compounds. A variety of characterizations demonstrated that the silica products exhibited a well-ordered 2d hexagonal mesostructure with well-formed spherical morphology. pore-diameter can be enlarged up to 8.2 nm without affecting the structural order. The SLP-SBA-15 samples showed excellent thermal and hydrothermal stabilities. The octadecyltriethoxysilane functionalized SLP-SBA-15 (SLP-C18-SBA-15) was demonstrated to be an effective stationary phase in UHPLC application because the column exhibited significantly reduced column pressure (2800 psi) at a flow rate of 0.4 ml/min. Accordingly, it would afford greater flexibility for tuning of the flow rate to meet the fast separation requirement.     

Structural and electrical properties of tantalum nitride thin films fabricated by using reactive radio-frequency magnetron sputtering

TaN thin film is an attractive interlayer as well as a diffusion barrier layer in [FeN/TaN]_n multilayers for the application as potential write-head materials in high-density magnetic recording. We synthesized two series of TaN films on glass and Si substrates by using reactive radio-frequency sputtering under 5-mtorr Ar/N₂ processing pressure with varied N₂ partial pressure, and carried out systematic characterization analyses of the films. We observed clear changes of phases in the films from metallic bcc Ta to a mixture of bcc Ta(N) and hexagonal Ta₂N, then sequentially to fcc TaN and a mixture of TaN with N-rich phases when the N₂ partial pressure increased from 0.0% to 30%. The changes were associated with changes in the grain shapes as well as in the preferred crystalline orientation of the films from bcc Ta [100] to [110], then to random and finally to fcc TaN [111], correspondingly. They were also associated with a change in film resistivity from metallic to semiconductor-like behavior in the range of 77–295 K. The films showed a typical polycrystalline textured structure with small, crystallized domains and irregular grain shapes. Clear preferred (111) stacks parallel to the substrate surface with embedded amorphous regions were observed in the film. TaN film with [111]-preferred orientation and a resistivity of 6.0 mΩ cm was obtained at 25% N₂ partial pressure, which may be suitable for the interlayer in [FeN/TaN]_n multilayers. Received: 6 December 1999 / Accepted: 24 July 2000 / Published online: 9 November 2000     

N-Bridged Acyclic Trimeric Poly-Cyclodiphosphazanes: Highly Tuneable Cyclodiphosphazane Building Blocks

We have synthesized a completely new family of acyclic trimeric cyclodiphosphazane compounds comprising NH, NⁱPr, N^tBu and NPh bridging groups. In addition, the first NH-bridged acyclic dimeric cyclophosphazane has been produced. The trimeric species display highly tuneable characteristics so that the distance between the terminal N(H)R moieties can be readily modulated by the steric bulk present in the bridging groups (ranging from ≈6 to ≈10 Å). Moreover, these species exhibit pronounced topological changes when a weak non-bonding NH⋅⋅⋅π aryl interaction is introduced. Finally, the NH-bridged chloride binding affinities have been calculated and benchmarked along with the existing experimental data available for monomeric cyclodiphosphazanes. Our results underscore these species as promising hydrogen bond donors for supramolecular host–guest applications.     

多晶Sr2Fe1－xAlxMoO6的晶粒内低场磁电阻效应

用传统的固相反应法合成了Fe位掺杂Al的双钙钛矿型氧化物Sr2Fe1-xAlxMoO6 (x=00，005，010，015，03)多晶材料. x射线衍射和扫描电子显微分析显示，在Fe位掺杂Al既没有引入杂相，也没有明显改变Sr2FeMoO6多晶材料的晶粒尺寸和晶界状态. 非磁性Al离子的掺杂使晶粒内部磁有序区细化成更小的区域，同时使反铁磁区内的磁耦合作用变弱. 这一方面提高了亚铁磁区磁化方向的磁场灵敏度；另一方面也降低了反铁磁区对自旋相关电子的散射；两方面的共同作用使Sr2FeMoO6的低场磁电阻效应明显增强，但这种尺寸效应也使材料的磁电阻在高温下下降得更快. 关键词： 低场磁电阻 掺杂 自旋极化电子     

Determination of cytokinins in coconut (Cocos nucifera L.) water using capillary zone electrophoresis-tandem mass spectrometry

The applicability of CZE in combination with MS and MS/MS methods for the simultaneous separation and determination of 12 cytokinins was investigated for the first time. Cytokinins were first completely separated by CZE within less than 20 min using a volatile buffer and then detected directly by MS or MS/MS. Satisfactory separation of the 12 cytokinin standards was achieved using a 25 mM ammonium formate/formic acid buffer (pH 3.4) and 3% ACN v/v with a separation voltage of 25 kV. On the basis of the resolution of the neighboring peaks, the various parameters for CZE-MS optimization, such as buffer pH value, concentration of buffer and organic modifier, applied voltage and sheath liquid, were evaluated systematically. MS/MS with multiple reaction monitoring detection was carried out to obtain sufficient selectivity and sensitivity. The combination of on-line sample stacking and CZE-MS/MS achieved a detection limit in the range of 0.05-0.18 microM for the 12 cytokinins at an S/N of 3. The optimized CZE-MS/MS method was simple, rapid, low cost, robust and highly selective. Furthermore, the developed method was successfully applied to screen for endogenous cytokinins in purified coconut water extract sample. Nine cytokinins were detected and quantified in coconut water after SPE.     

High-performance flow-focusing geometry for spontaneous generation of monodispersed droplets

A high-performance flow-focusing geometry for spontaneous generation of monodispersed droplets is demonstrated. In this geometry, a two-phase flow is forced through a circular orifice integrated inside a silicon-based microchannel. The orifice with its cusp-like edge exerts a ring of maximized stress around the flow and ensures controlled breakup of droplets for a wide range of flow rates, forming highly periodic and reproducible dispersions. The droplet generation can be remarkably rapid, exceeding 10(4) s(-1) for water-in-oil droplets and reaching 10(3) s(-1) for oil-in-water droplets, being largely controlled by flow rate of the continuous phase. The droplet diameter and generation frequency are compared against a quasi-equilibrium model based on the critical Capillary number. The droplets are obtained despite the low Capillary number, below the critical value identified by the ratio of viscosities between the two phases and simple shear-flow.     

Low-cost Imaging of Fluorescent DNA in Agarose Gel Electrophoresis using Raspberry Pi cameras

Low-cost analytical solutions built around microcomputers like the Raspberry Pi help to facilitate laboratory investigations in resource limited venues. Here, three camera modules (V1.3 with and without filter, as well as NoIR) that work with this microcomputer were assessed for their suitability in imaging fluorescent DNA following agarose gel electrophoresis. Evaluation of their utility was based on signal-to-noise (SNR) and noise variance metrics that were developed. Experiments conducted with samples were subjected to Polymerase Chain Reaction (PCR), and the amplified products were separated using gel electrophoresis and stained with Midori green. Image analysis revealed the NoIR camera performed the best with SNR and noise variance values of 21.7 and 0.222 respectively. In experiments conducted using UV LED lighting to simulate ethidium bromide (EtBr) excitation, the NoIR and V1.3 with filter removed cameras showed comparable SNR values.