高效液相色谱法测定皮革中的双酚A、双酚F和双酚S

建立了一种测定皮革中双酚A、双酚F和双酚S含量的分析方法。皮革样品经甲醇超声提取、旋转蒸发仪浓缩后,在277 nm波长条件下,使用高效液相色谱仪进行分析,经二极管阵列器检测,甲醇-水溶液洗脱后,外标法进行定量。结果显示,双酚A、双酚F和双酚S在1 mg·L^(-1)~30 mg·L^(-1)的范围内线性相关系数均大于0.9995,检出限均小于0.64 mg·kg^(-1),高、中、低三个水平加标回收率范围为85.8%~97.1%,相对标准偏差为0.11%~2.22%,满足检测要求。

S^(*)-收敛和局部强紧空间

定向空间是定向完备偏序集的拓扑推广,局部强紧空间可以刻画为拟连续的定向空间.本文给出了关于局部强紧空间的一个拓扑版的Scott收敛定理.通过引入S^(*)-收敛的概念并定义有限逼近空间,本文得到以下主要结果:(i)定向空间X是局部强紧的当且仅当S_(X)^(*)-收敛是可拓扑化的;(ii)对任意T0空间X,S_(X)^(*)-收敛是可拓扑化的当且仅当X是有限逼近空间;(iii)若定向空间X上的Lawson拓扑是紧的,则X是赋予Scott拓扑的定向完备偏序集.

Study of Quality Standards of Xiao’er Qingre Enema Preparation in Hospitals

Objective:To establish the quality standards for the preparation of Xiao’er Qingre enema in hospitals.Method:Thin-layer chromatography(TLC)was used to identify Radix Isatidis and Glycyrrhizae in the prescription.The content of(R,S)-Goitrin was determined by high-performance liquid chromatography(HPLC).Results:In TLC identification,there was no interference between the negative controls of Radix Isatidis and glycyrrhizae,and the spots were well-separated.The HPLC results of(R,S)-Goitrin showed a good linear relationship between the peak area and concentration within the range of 0.476-95.2μg·mL-1(r=0.9999).Conclusion:The TLC and HPLC methods established in this experiment are simple,reproducible,and specific,making them suitable for the quality control Xiao’er Qingre enema preparation in hospitals.

Factors Controlling Precipitation of Barite and Witherite and Genesis of the Ankang-Xunyang Barium Deposits,Shaanxi,China

The barium deposits in Ankang and Xunyang counties,Shaanxi Province,China,occur in the northernmost part of the world-class barium metallogenic belt in south Qinling.The deposits are hosted by the Lower Silurian carbonaceous siliceous rocks,with a unique combination of barite and witherite.The homogenization temperatures of fluid inclusions in the barite are mainly concentrated between 135 and 155 ℃,whereas those from the witherite have two peaks of 165-175 ℃,and 215-225℃,respectively.Laser Raman analysis of fluid inclusions indicates that the vapor phase of fluid inclusions in barite is dominated by H_2O,although some contains N_2,H_2S,and CH_4.The compositions of the vapor and liquid phases of fluid inclusions in witherite can be divided into two end-members,one dominated by H_2O without other volatiles,and the other containing CH_4,C_2H_6,C_3H_8,C_2H_4,and C_6H_6 in addition to H_2O.CO_2,H_2S,and some CH_4 are interpreted as products of chemical reactions during mineralization.Organic gases（CH_4,C_2H_6,C_3H_8,C_2H_4,and C_6H_6） in the fluids were critical in the formation of barium sulfate versus carbonate.The δ^（34）S values of barite range from 38.26‰ to54.23‰（CDT）,the δ^（34）S values of sulfides coexisting with barium minerals vary from 22.44‰ to25.11‰（CDT）,and those in the wall rock from 11.60‰ to 19.06‰（CDT）.We propose that the SO_4^（2-）generally experienced bacterial sulfate reduction in seawater before mineralization,and some SO_4^（2-）also experienced thermochemical sulfate reduction in hydrothermal system during mineralization.The δ^（13）C values of witherite range from-27.30‰ to-11.80‰（PDB）,suggesting that carbon was sourced from organic substances（like CH_4,C_2H_4,and C_2H_6）.The formation of witherite was possibly associated with thermochemical sulfate reduction,which caused the consumption of the organic gases and SO_4^（2-） in the hydrothermal solutions,consequently inhibiting barite formation.The important conditions for forming witherite include high fluid temperatures,high Ba^（2＋） concentrations,CO_2 in the fluids,low HS^- concentrations,and the subsequent rapid diffusion of H_2S during thermochemical sulfate reduction of the fluids.

Crustal structure and accurate hypocenter determination along the Longmenshan fault zone

A P and S wave velocity model is obtained for the crust in the region along the Longmenshan fault zone, Sichuan Province, China, by using data from a refraction profiling survey carried out in this region and those from local earthquakes. 202 local earthquakes along the fault zone are based on this velocity model, location errors being estimated to be about 1.5 km. The present relocations fairly improved the accuracy of hypocenter locations for earthquakes in this area, which is recognized from small scatter of data in the arrival time distance diagram compared with that for the original locations in the Earthquake Catalogue of Sichuan Seismic Network. The obtained hypocenter distribution shows that shallow earthquakes, confined to the upper crust in the depth range from 3 km to 22 km, are actively occurring along the main fault of the Longmenshan fault zone. The velocity model and the location method are presently used quite effective for precisely locating local earthquakes such as those in Sichuan Province. Installation of these with the real time processing system developed by Tohoku University in the Sichuan Telemetered Seismic Network would help to improve the location accuracy of events beneath the network.

Determination of Palladium II in 5% Pd/BaSO₄by ICP-MS with Microwave Digestion, and UV-VIS Spectrophotometer

Determination palladiums have been reported 5% (w/w) Pd/BaSO4 known as Rosenmund Catalyst. The determination of palladium II known as Rosenmund Catalyst is always an expensive procedure usually involving procedures such as flame atomic absorption spectrophotometry, emission spectrometry, and many spectrophotometric methods. In this study, palladium II in 5% Pd/BaSO4, was synthesized and employed to develop an extractive UV-Visible Spectrophotometric, and an inductively coupled plasma mass spectrometry ICP/MS methods for the determination of palladium II. Specification for Pd is 4.85% to 5.10%;the result was 4.97% for the UV-Visible spectrophotometer and 4.90% for the ICP/MS. Both results meet the requirements.

A novel binary effective medium model to describe the prepeak stressstrain relationship of combined bodies of rock-like material and rock

Combined bodies of rock-like material and rock are widely encountered in geotechnical engineering,such as tunnels and mines.The existing theoretical models describing the stress-strain relationship of a combined body lack a binary feature.Based on effective medium theory,this paper presents the governing equation of the“elastic modulus”for combined and single bodies under triaxial compressive tests.A binary effective medium model is then established.Based on the compressive experiment of concretegranite combined bodies,the feasibility of determining the stress threshold based on crack axial strain is discussed,and the model is verified.The model is further extended to coal-rock combined bodies of more diverse types,and the variation laws of the compressive mechanical parameters are then discussed.The results show that the fitting accuracy of the model with the experimental curves of the concretegranite combined bodies and various types of coal-rock combined bodies are over 95%.The crack axial strain method can replace the crack volumetric strain method,which clarifies the physical meanings of the model parameters.The variation laws of matrix parameters and crack parameters are discussed in depth and are expected to be more widely used in geotechnical engineering.

Determination of Elastic-plastic Poisson's Ratio in Elastic-Plastic FEM

ＤｅｔｅｒｍｉｎａｔｉｏｎｏｆＥｌａｓｔｉｃ－ｐｌａｓｔｉｃＰｏｉｓｓｏｎ＇ｓＲａｔｉｏｉｎＥｌａｓｔｉｃ－ＰｌａｓｔｉｃＦＥＭＸＵＷｅｉｌｉ，ＸＩＮＧＺｈｏｎｇｗｅｎ，ＬＩＣｈｕｎｆｅｎｇ，ＹＡＮＧＹｕｙｉｎｇ（徐伟力）（邢忠文）（李春峰）（杨玉英...

The Tongliao MS5.3 Earthquake and Its Foreshock Determination

Taking the 2013 Tongliao MS5. 3 earthquake as a research subject, on the basis of statistical analysis of earthquake sequence using the HypoDD location method and focal mechanism solutions,the paper analyzes and discusses the relationship between the ML4. 4 and MS5. 3 earthquakes. The results show that the Tongliao MS5. 3 earthquake occurred under the background of medium-small earthquakes long-term quiescence and short-term enhancement in the epicentral area. The results of accurate seismic location shows that the Tongliao MS5. 3 earthquake sequence is distributed in the NW direction,extending 10 km,and the ML≥3. 0 aftershocks are concentrated south of the mainshock. The distance between the MS5. 3 mainshock and the ML4. 4 foreshock is about 1. 8 km,with a focal depth of 7. 208 km and 7. 089 km,respectively,their focal location is very close,and may have occurred on the same fault plane. The results of focal mechanism shows that the Tongliao MS5. 3 earthquake is of the strike-slip type,the focal mechanism of aftershocks are disordered,and with time lapse,the type is changed from strike-slip to thrust and normal faulting. The bigger foreshocks had similar focal mechanism and were all normal fault types,which exhibits to some extent,an obvious crustal medium anisotropy in the epicentral area before macroscopic rupturing,as represented by alignment fractures,with stress action enhanced,this"consistency"of seismic precursor regime would gestate the mainshock. According to the characteristics of temporal-spatial distribution of earthquake sequence and similarity of focal mechanism,we judge that the Tongliao MS5. 3 earthquake sequence is a foreshock-mainshock-aftershock type.

Simultaneous determination of ten components in Dianxiankang Capsules by HPLC QAMS

Objective:To establish an high performance liquid chromatography-quantitative analysis of multi components by single marker(HPLC-QAMS)method for simultaneous determination of gastrodin,parishin E,parishin B,parishin,tenuifolin,onjisaponin B,methylophiopogonanone A,methylophiopogonanone B,β-asarone andαasarone in Dianxiankang Capsules.Methods:Waters Symmetry C_(18)column was used with acetonitrile-0.05%phosphoric acid solution as mobile phase for gradient elution.Multiwavelength switching detection.The contents of gastrodin,parishin E,parishin B,parishin,onjisaponin B,methylophiopogonanone A,methylophiopogonanone B,β-asarone andα-asarone were calculated by relative correction factor.At the same time,the contents of 10 components in 12 batches of Dianxiankang Capsules were determined by external standard method(ESM).Results:An HPLC-QAMS method was established tenuifolin as the internal reference substance was established.The relative correction factors of gastrodin,parishin E,parishin B,parishin,onjisaponin B,methylophiopogonanone A,methylophiopogonanone B,β-asarone andα-asarone were 0.8238,0.7239,1.0229,1.1881,0.7272,1.3108,0.9314,0.6549 and 1.0572,respectively.The relative correction factors had good repeatability and no significant difference with ESM(P>0.05).Conclusion:HPLC-QAMS can be used for simultaneous determination of multi-index components in Dianxiankang Capsules.

Experimental Determination of the Landé g-Factors for 5s^2 ^1S and 5s5p ^3P States of the ^87Sr Atom

We present an experimental determination on the Lande g-factors for the 5 s^2 ^1 S0 and 5 s5 p ^3P0 states in ultra-cold atomic systems, which is important for evaluating the Zeeman shift of the clock transition in the ^87Sr optical lattice clock. The Zeeman shift of the 5 s5 p ^3 P0-5 s^2 ^1 S0 forbidden transition is measured with the π-polarized and σ^±-polarized interrogations at different magnetic field strengths. Moreover, in the g-factor measurement with the σ^±-transition spectra, it is unnecessary to calibrate the external magnetic field. By this means, the ground state 5 s^2 ^1 S0 g-factor for the ^87Sr atom is-1.306（52） ×10^-4, which is the first experimental determination to the best of our knowledge, and the result matches very well with the theoretical estimation. The differential g-factorδg between the 5 s5 p^3 P0 state and the 5 s^2 ^1 S0 state of the ^87Sr atoms is measured in the experiment as well,which are-7.67（36） ×10^-5 with π-transition spectra and-7.72（43） X 10^-5 with σ^±-transition spectra, in good agreement with the previous report [Phys. Rev. A 76（2007） 022510]. This work can also be used for determining the differential g-factor of the clock states for the optical clocks based on other atoms.

The Use of Yanai’s Generalized Coefficient of Determination to Reduce the Number of Variables in DEA Models

This paper proposes a new method to reduce the dimensionality of input and output spaces in DEA models. The method is based on Yanai’s Generalized Coefficient of Determination and on the concept of pseudo-rank of a matrix. In addition, the paper suggests a rule to determine the cardinality of the subset of selected variables in a way to gain the maximal discretionary power and to suffer a minimal informational loss.

Ceramic Nanocrystalline Superconductor Gadolinium Barium Copper Oxide (GdBaCuO) at Different Treating Temperatures

With the discovery of high-TC superconducting materials like Yttrium Barium Cupric Oxide, Bismuth Strontium Calcium Copper Oxide and Thallium Calcium Barium Copper Oxide, tremendous interest has developed over the past two years in understanding these materials as well as utilizing them in a variety of applications. The thin films of these materials are expected to play an important role in the area of microelectronics, especially for interconnects in integrated circuits, Josephson junctions, magnetic field sensors and optical detectors. Here, the authors designed a new nanocrystalline ceramic type II high-TC superconductor, Gadolinium Barium Copper Oxide (GdBaCuO/GBCO). The GBCO perovskite phase structure was prepared by the conventional solid state thermochemical reaction technique involving mixing, milling, calcination and sintering. In GBCO system, the method for controlling microstructure and superconducting state is related to oxygen content consideration because small changes in oxygen concentration can often?lead to huge change in Tc. In order to show the viability of the proposed method, super-conducting powder was prepared in special furnace. The sample was analyzed by X-Ray Diffraction (XRD), an indispensible non-destructive tool for structural materials characterization and quality control which makes use of the Debye-Scherrer method. The comparison of XRD results with JCPDS files confirmed the orthorhombic structure of the sample. Micro-structural features are studied using Scanning Electron Microscopy (SEM) which revealed that its particle size is in the nanometer range. It also confirmed the calculated value of particle size from Debye Scherrer’s formula. EDX plot shows the presence of all the constituents. X-ray instrumental peak broadening analysis was used to evaluate the size and lattice strain by the Williamson-Hall Plot method.

氯化钡沉淀+ICP-OES法测定工业硫酸中砷含量

研究了利用氯化钡饱和溶液除去硫酸溶液中的硫酸根,再用电感耦合等离子体发射光谱仪测定工业硫酸中砷含量的方法。探讨了砷元素常用分析谱线的干扰情况及酸度效应对砷含量测定结果的影响,通过试验验证了方法的可靠性。试验结果表明,向制备的硫酸溶液中加入饱和氯化钡溶液沉淀除去硫酸根,有利于消除硫酸基体对ICP-OES测定结果的影响,砷的加标回收率为99.6%~101.5%,平行测定的相对标准偏差小于5%,与原子荧光光度法、砷斑法的测定结果无明显差异。

紫外分光光度法测定双酚S(英文)

建立了测定双酚S的紫外分光光度法。在pH值为6.0的磷酸盐缓冲溶液中,双酚S浓度在4.8×10-7~4.0×10-5mol.L-1范围内与其吸光度值呈显著线性相关,相关系数为0.9999,相对标准偏差为0.12%,检测限为4.0×10-7mol.L-1。该方法快速、灵敏,可用于常见样品中双酚S的测定。

蛋白质-铬天青S体系的弹性光散射及其初步分析应用

在pH3.5左右的柠檬酸-NaOH介质中,蛋白质与铬天青S可以通过以静电引力为主的分子间作用力结合生成大分子离子缔合物,产生最大散射波长约为370nm的弹性光散射信号.基于这一现象可以测定低至0.02μg·mL^(-1)的血清白蛋白,工作曲线在0～1.0μg·mL^(-1)范围内呈线性关系.这一新方法的灵敏度比Coomassie亮蓝法高50倍.用普通的荧光分光光度计测量了这一体系的散射光谱,研究了pH,离子强度和试剂浓度等实验条件对散射光强的影响,考察了阳离子、阴离子和非离子表面活性剂以及氨基酸和常见金属离子对反应体系的作用.将这一方法用于测定尿中徽量蛋白,结果满意.

Al／BaTiO_3／Si结构的湿敏特性

用氩离子束镀膜法制备ＢａＴｉＯ_３／Ｓｉ系统，并在４００－９００℃的温度下用氮气保护进行退火，然后制成Ａｌ／ＢａＴｉＯ３／Ｓｉ的ＭＩＳ结构。用俄歇电子能谱分析ＢａＴｉＯ３膜的化学组分．研究电容－相对湿度和电流－相对湿度特性，以及固定电荷密度对湿敏特性的影响．结果表明，当相对湿度从１２％变化到９２％时，电容量增加４８％到５０％；在３Ｖ偏压下，电流量增加４２０％到４４０％；随着固定电荷密度的减小，吸附响应时间增加，电流变化率减小．

高效液相色谱法测定板山岗颗粒中(R,S)-告依春含量

目的建立测定板山岗颗粒中(R,S)-告依春含量的高效液相色谱(HPLC)法。方法色谱柱为Kromasil 100-5 C18柱(250 mm×4. 6 mm,5μm),流动相为甲醇-水(12∶88,V/V),流速为1. 0 m L/min,检测波长为244 nm,柱温为30℃,进样量为10μL。结果(R,S)-告依春进样量在0. 04~0. 32μg范围内与峰面积积分值线性关系良好;精密度、稳定性、重复性试验的RSD值均小于2%;平均加样回收率为97. 96%,RSD为1. 63%(n=9)。结论该方法操作简便、准确,精密度、稳定性、重复性均良好,可用于板山岗颗粒中(R,S)-告依春含量的测定。

丽春红S褪色分光光度法测定溴酸根离子的研究

在盐酸介质中,依据溴酸根离子氧化丽春红S褪色的原理提出了测定溴酸根离子的新方法,研究了测定的最佳条件。测定的最大吸收波长λmax为510 nm,溴酸根离子在0.5-5.0μg/mL范围内符合比尔定律,线性回归方程为A510=0.318 5ρ-0.040 6,相关系数为0.994 94,表观摩尔吸光系数为4.08×10^4L/（mol.cm）。该法可用于化学试剂中的微量溴酸根测定,结果满意。

Al(Ⅲ)-CAS-OP-PVA体系分光光度法测定沸石分子筛中的铝

研究了在聚乙二醇辛基苯基醚（乳化剂ＯＰ）及聚乙烯醇（ＰＶＡ）存在下铝（Ⅲ）与铬天青Ｓ（ＣＡＳ）的显色反应。在ｐＨ５．３的ＨＡｃ－ＮａＡｃ缓冲介质中，题示体系最大吸收波长λｍａｘ＝６１２ｎｍ，对比度Δλ＝１０２ｎｍ，表观摩尔吸光系数ε６１２ｎｍ＝２．８４×１０４Ｌ·ｍｏｌ－１·ｃｍ－１。铝（Ⅲ）浓度在０－０．６０μｇ／ｍＬ范围内遵守比耳定律。本法已成功地用于沸石分子筛中铝含量的测定，结果良好。该法具有稳定性高、准确度好的特点。