Analysis of saturated free fatty acids from pollen by HPLC with fluorescence detection

A sensitive method for the determination of free fatty acids using 2‐(2‐(anthracen‐10‐yl)‐1H‐naphtho[2,3‐d]imidazol‐1‐yl) ethyl‐p‐toluenesulfonate (ANITS) as tagging reagent with fluorescence detection has been developed. ANITS could easily and quickly label fatty acids in the presence of the K₂CO₃ catalyst at 90 °C for 40 min in N,N‐dimethylformamide solvent. From the extracts of rape bee pollen samples, 20 free fatty acids were sensitively determined. Fatty acid derivatives were separated on a reversed‐phase Eclipse XDB‐C₈ column by HPLC in conjunction with gradient elution. The corresponding derivatives were identified by post‐column APCI/MS in positive‐ion detection mode. ANITS‐fatty acid derivatives gave an intense molecular ion peak at m/z [M+H]⁺; with MS/MS analysis, the collision‐induced dissociation spectra of m/z [M+H]⁺ produced the specific fragment ions at m/z [M–345]⁺ and m/z 345.0 (here, m/z 345 is the core structural moiety of the ANITS molecule). The fluorescence excitation and emission wavelengths of the derivatives were λ_ex = 250 nm and λ_em = 512 nm, respectively. Linear correlation coefficients for all fatty acid derivatives are >0.9999. Detection limits, at a signal‐to‐noise ratio of 3 : 1, are 24.76–98.79 fmol for the labeled fatty acids.     

用于测定钢液低氧含量的双层固体电解质研究

采用“毛坯浆料法”在ＺｒＯ２（９％摩尔含量ＭｇＯ）管状固体电解质基体表面制备了厚度为１－４μｍ的ＺｒＯ２（１０％摩尔含量Ｙ２Ｏ３）固体电解质涂层，并分别对此在本实验室和美国ＬｅｅｄｓａｎｄＮｏｒｔｈｒｕｐ公司进行了钢液低氧含量测试，结果表明：涂层没有破坏基体的抗热震性：氧浓差电池电动势的重现性偏差由原来的±２ｍＶ；电动势的绝对值提高１０ｍＶ左右；而比日本Ｔｏｒａｙ公司的同类产品提高３５ｍＶ，这说明     

辅酶Q10的合成方法

辅酶Q10(CoQ10)是一种用途十分广泛的生化药物,但国内未见关于CoQ10合成的研究报道.本文介绍国外关于CoQ10的合成方法,重点介绍从烟草中提取的天然茄呢醇为原料的合成法,并予评述.     

基于线性CCD的寻线智能车设计

本设计以第八届"飞思卡尔"杯全国大学生智能车竞赛为背景,提出了一种根据线性CCD采集图像引导直立小车循迹行驶的方案。本文介绍了这一方案的基本思想,所依据的物理原理,并重点介绍在双速度控制算法下对转向及障碍问题的优化处理,并根据方案实际制作了小车。实践证明该方案是可行的,并且效果较好。     

Fabrication and Microstructure Characterization of Ti3SiC2 Synthesized from Ti/Si/2TiC Powders Using the Pulse Discharge Sintering (PDS) Technique

Ti/Si/2TiC powders were prepared using a mixture method (M) and a mechanical alloying (MA) method to fabricate Ti₃SiC₂ at 1200°–1400°C using a pulse discharge sintering (PDS) technique. The results showed that the Ti₃SiC₂ samples with <5 wt% TiC could be rapidly synthesized from the M powders; however, the TiC content was always >18 wt% in the MA samples. Further sintering of the M powder showed that the purity of Ti₃SiC₂ could be improved to >97 wt% at 1250°–1300°C, which is ∼200°–300°C lower than that of sintered Ti/Si/C and Ti/SiC/C powders using the hot isostatic pressing (HIPing) technique. The microstructure of Ti₃SiC₂ also could be controlled using three types of powders, i.e., fine, coarse, or duplex-grained, within the sintering temperature range. In comparison with Ti/Si/C and Ti/SiC/C mixture powders, it has been suggested that high-purity Ti₃SiC₂ could be rapidly synthesized by sintering the Ti/Si/TiC powder mixture at relatively lower temperature using the PDS technique.     

Conformational disorder in the Brill transition of uniaxially-oriented nylon 10/10 sample investigated through the temperature-dependent measurement of X-ray fiber diagram

X-ray fiber diagram of uniaxially-oriented nylon 10/10 sample has been measured at the various temperatures. The 11th layer line originating from the methylene zigzag sequences became diffuse above the Brill transition region (140-170 °C), while the layer reflections corresponding mainly to the original repeating period of the parent nylon chains were kept almost unchanged. This observation makes us confirm that in the Brill transition region, the conformational disordering occurs in the methylene sequential parts with keeping the repeating period of the whole skeletal chain by still forming the intermolecular hydrogen bonds between the amide groups of the neighboring chains. This conclusion is consistent with the already-reported infrared spectral data. The characteristic X-ray diffraction patterns observed at the various temperatures were reproduced well by a computer simulation technique utilizing the previously-reported molecular dynamics calculation results.     

Cemented backfill technology based on phosphorous gypsum

Physical-chemical properties of phosphorous gypsum, proportion and cemented mechanism of slurry with gypsum as aggregate were studied to remove the harms of gypsum pile, combining with difficult problems of excessive mined-out gobs, enormous ore body under roadway and low recovery ratio of Yongshaba Mine, Kaiyang Phosphor Mine Group, Guizhou Province, China. An appropriate backfill system and craftwork were designed, using shattering milling method to crush gypsum, double-axles mixing and strong activation mixing way to mix slurry, cemented slurry and mullock backfill alternately process. The results show that gypsum is fit for backfilling afterwards by adding fly ash, though it is not an ideal aggregate for fine granule and coagulate retardation. The suggested dosage (the mass ratio of cement to fly ash to gypsum) is 1:1:6–1:1:8 with mass fraction of solid materials 60%–63%. Slurry is transported in suspend state with non-plastic strength, and then in concretion state after backfilling. The application to mine shows the technology is feasible, and gypsum utilization ratio is up to 100%. Transportation and backfill effect is very good for paste-like slurry and drenching cemented slurry into mullock, and the compressive strength and recovery ratio are 2.0 MPa and 82.6%, respectively, with the maximum subsidence of surface only 1.307 mm. Furthermore, the investment of system is about 7×10⁶ yuan (RMB), only 1/10 of that of traditional paste backfill system. Foundation item: Project (2006BAB02A03) supported by the National Key Technology Research and Development Program; Project (08MX16) supported by Mittal Scientific and Technological Innovation Projects of Central South University during 2008     

粗晶硬质合金强度和致密度影响因素的研究

针对粗晶WC-Co硬质合金的成分和工艺优化要求,运用正交实验设计,考察了含碳量、烧结工艺、钴含量、镍含量、球磨球料比和球磨时间对试样抗弯强度和体积收缩率的影响。研究表明,烧结制度是影响抗弯强度的最主要因素;其次是碳含量与烧结工艺的交互作用、Co含量与球磨时间的交互作用。烧结工艺是影响体积收缩率的最主要因素。     

基于单片机虚拟串口驱动LCD1602的电路仿真

基于Multisim10仿真软件,设计单片机的虚拟串口驱动LCD1602液晶电路。实现了虚拟串口扩展并行输出的功能。该设计适用单片机UART串口被占用时,以最少的单片机I/O口驱动LCD1602,满足显示电路中复杂信息的需求。与传统的设计手段相比,在Multisim10平台支撑下,设计电路更方便快捷,并可通过仿真结果直接观测和验证设计电路是否达到要求,具有省时、低耗、高效的优越性。     

用1，10－二氮杂菲分光光度法测定沉淀法白炭黑中的铁含量

提出并研究了使用１，１０－二氮杂菲分光光度法测定沉淀法白炭黑中铁含量的分析方法。其具体步骤为：首先用氢氟酸处理试样，使沉淀法白炭黑（二氧化硅）转化成四氟化硅气体逸出。而后在ｐＨ为４～５条件下，用盐酸羟胺处理剂将残留液中的三价铁离子还原成二价铁离子，加入１，１０－二氮杂菲显色剂（与二价铁离子反应可生成橙红色络合物），再用分光光度法测定其中的铁含量。实验表明，本方法原理可靠，分析步骤简便，抗铜、锰离子干扰性强，精密度与准确度较高。