高效液相色谱法测定卷柏中的穗花杉双黄酮

用反相高效液相色谱法测定卷柏提取物中的穗花杉双黄酮。结果表明：穗花杉双黄酮在质量浓度为41.2mg／L～206mg／L时，峰面积Y与其质量浓度X的线性关系良好，回归方程为Y=547．028X 15．4895(r=0.9999)，最低检测限为2．0μg/L；穗花杉双黄酮的平均回收率为99．42％(n=3)，相对标准偏差RSD为0．79％；连续进样、日内进样和日间进样所得检测结果的RSD分别为0．12％、0．11％和0．11％。     

Use of mesoporous SBA-15 for nanostructuring titania for photocatalytic applications

SBA15–TiO₂ samples prepared by introducing titanium with a grafting method and having TiO₂ loadings below 15 wt.% have been characterized by XRF, XRD, IR, porosimetry, SEM, HRTEM, and UV–Visible diffuse reflectance. Differently from the samples reported in the literature characterized by a high TiO₂ loading, no evidences have been found for the presence of titania particles inside or outside the mesopores of SBA-15. Three different titanium species were instead evidenced to be present. The first two derive from the reaction of titanium with silanol groups in the corona area of inner SBA-15 walls leading to the formation of either TiO₄ tetrahedral sites (by reaction by hydroxyl nests of surface defect sites) and/or pseudo-octahedral surface sites anchored by two (or more) Si or Ti ions through bridging oxygens. The third species derives from the reaction of titanium in the regions with high sylanol density, e.g. in the micropores located in the corona of SBA-15 channels, leading to the formation of TiO₂-like nanoareas (probably Si-doped) with dimensions of around 1–2 nm maximum. The potential interest of these materials as photocatalysts, for the presence of a TiO₂-like nanoareas highly accessible by reactants, is discussed.     

A polyamide-silica composite prepared by the sol-gel process

Summary A new kind of organic-inorganic hybrid composite was prepared by means of the sol-gel process. The polymer employed was a mixed-isomer aromatic polyamide having good solubility and thermal stability. The silica constituting the inorganic phase was produced by the hydrolysis and condensation of tetramethoxysilane. The bonding between the phases involved aminophenyl-trimethoxysilane, in which the amino group can react with the phthaloyl chloride end-capped polymer, and the methoxysilane groups undergo hydrolysis. The composition of these composites was varied by changing the linear polymer chain length and relative amount of tetramethoxysilane. The gelation time was found to range from a few minutes to several days. Thermogravimetric analyses showed that decomposition starts at approximately 450 °C. Thin films cast from materials having a relatively high silica content were opaque and rigid, but those with low silica content were flexible and transparent.     

Gas hold-up in non-newtonian solutions in a bubble column with internals

Bubble characteristics and gas hold-up were studied in a two phase (air-aqueous CMC solution) bubble column provided with helical coils and straight tubes as internals. The effects of superficial gas velocity, rheological properties, and volume fraction covered by the internals, on gas hold-up were studied. Hold-up values determined directly and by simultaneous pressure drop measurements matched well. Enhancement of gas hold-up values up to 55 per cent was achieved in systems using internals. The gas hold-up results were also compared with the values obtained from correlations reported in the literature.     

反相高效液相色谱法测定meso-四苯基卟啉钴的纯度

采用反相高效液相色谱法测定合成meso-四苯基卟啉钴的纯度;以甲醇乙腈二氯甲烷(体积比为55∶35∶10)为流动相,ShimpackCLCODS柱(150mm×6.0mmi.d,5μm)为分离柱,流速为1.5mL/min,检测波长420nm;meso四苯基卟啉钴的测定在1.0～10μg/mL时线性关系良好(相关系数r=0.9993),加标回收率为97.03%～101.42%,重复进样的相对标准偏差RSD为0.64%～2.92%(n=5)。方法的准确度高,精密度好,实际应用效果好。     

Separation and identification of phenolic acids and related compounds by gas chromatography and fourier transform infrared spectroscopy

Phenolic acids and related compounds were separated by gas chromatography using three separate columns. One of these columns was coupled to a Fourier transform infrared spectrometer. The trimethylsilyl derivatives could be separated and identified by comparing the relative retention times of the three different columns. However, where there was overlap, the accompanying infrared data clearly distinguished between the questionable derivatives, thus enabling characterization of all derivatives.The use of trade, firm, or corporation names in this article is for the information and convenience of the reader. Such use does not constitute an official endorsement or approval by the U.S. Department of Agriculture or the Forest Service of any product or service to the exclusion of others that may be suitable.     

熔融石英耐火材料

阐述了熔融石英耐火材料的主要性能与应用领域。     

溴虫腈土壤和甘蓝微量残留量的气相色谱法测定

采用气相色谱法定量分析溴虫腈土壤和甘蓝微量残留量。样品经丙酮提取 ,液 液分配及氧化铝柱层析法净化后 ,以GC ECD测定 ,DB 170 1毛细管柱 ,氮气为载气 ,柱温 2 6 0℃ ,汽化室温度 2 5 0℃ ,检测器温度 2 80℃ ,外标法定量。该方法快速、准确 ,在 0 0 1～ 2 0 0mg/L范围内线性相关系数r2 =0 9999,平均回收率 90 0 %～ 10 3 6 7% ,变异系数 4 4 8%～ 5 89% ,最小检测量 2× 10 12 g ,最低检出浓度 3 3× 10 4mg/kg。     

All-glass system for preparative gas chromatography using capillary columns

A zero dead-volume all-glass-lined stainless-steel effluent splitter with a modified thermal gradient collector was designed for preparative gas chromatography using glass capillary columns. This system gives efficient collection of extremely pure samples of the 1-ng to 10-g range for spectral analysis and biological testing.Approved as TA 15656 by the director of the Texas Agricultural Experiment Station in cooperation with ARS, USDA. Supported by the Texas Department of Agriculture interagency agreement IAC-0487 (78-79).