Spectro M8型直读光谱仪分析生铁中硅、锰和磷

用 HB 30 0 0型磨样机制取样品 ,Spectro M8型直读光谱仪分析生铁中硅、锰和磷 ,方法可行 ,数据准确 ,取得了理想效果。

Investigation of the interaction between indigotin and two serum albumins by spectroscopic approaches

The binding characteristics of indigotin with human serum albumin （HSA） and bovine serum albumin （BSA） have been investigated by various spectroscopic techniques. Spectroscopic analysis revealed that the quenching mechanism between indigotin and HSA/BSA belonged to the static quenching. The displacement experiments suggested that indigotin primarily bound to tryptophan residues on proteins within site I. The thermodynamic parameters indicated that the binding of indigoti^HSA/BSA mainly depended on the hydrophobic interaction. The binding distance of indigotin to HSA/BSA was evaluated. The results by synchronous fluorescence, three- dimensional fluorescence, Fourier Transform Infrared spectroscopy （FT-IR） and circular dichroism （CD） spectra showed that the conformation of proteins altered in the presence of indigotin.

Two-Dimensional Terahertz Time-Domain Spectroscopy and Its Applications

In this work, we review the developing progress of two-dimensional terahertz time-domain spectroscopy（THz-TDS） and its diverse applications, including analyzing the polarization of THz radiation from a laser-induced plasma source and studying the corresponding physical mechanism, and characterizing the optical properties of crystals, etc.

A rapid and sensitive liquid chromatography-tandem mass spectrometric assay for duloxetine in human plasma:Its pharmacokinetic application

This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.

Spectrophotometric Methods for Simultaneous Determination of Amlodipine Besylate and Atenolol in Their Tablet Dosage Form

Three simple,specific,accurate and precise spectrophotometric methods are developed for simultaneous determination of amlodipine besylate(AM)and atenolol(AT)in tablets.The first method is dual wavelength spectrophotometry(DW).The second method is ratio subtraction(RS)which depends on subtraction of the plateau values from the ratio spectrum,coupled to first derivative of ratio spectra(1 DD).The third method applies bivariate calibration method using 210and 225nm as an optimum pair of wavelength for amlodipine and atenolol.The calibration curves are linear over the concentration range of 4~40μg·mL-1 for both drugs.The specificity of the developed methods is investigated by analyzing laboratory prepared mixtures of the two drugs and their combined dosage form.The two methods are validated as per ICH guidelines and can be applied for routine quality control testing.

Reagent-free determination of amikacin content in amikacin sulfate injections by FTIR derivative spectroscopy in a continuous flow system

The quantitative estimation of amikacin （AMK） in AMK sulfate injection samples is reported using FTIR-derivative spectrometric method in a continuous flow system. Fourier transform of mid-IR spectra were recorded without any sample pretreatment. A good linear calibration （r40.999, %RSDo 2.0） in the range of 7.7-77.0 mg/mL was found. The results showed a good correlation with the manufacturer＇s and overall they all fell within acceptable limits of most pharmacopoeial monographs on AMK sulfate.

ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY DURING CORROSION PROCESS OF 8090 Al-Li ALLOY IN EXCO SOLUTION

The corrosion behavior and electrochemical impedance spectroscopy (EIS) features of 8090 Al-Li alloys in EXCO solution were investigated, and the EIS was simulated using an equivalent circuit. At the beginning of immersion in EXCO solution, the EIS is comprised by a depressed capacitive arc at high-mediate frequency and an inductive arc at low frequency, and the inductive component decreases and disappears with im- mersion time. Once exfoliation or severe pitting corrosion is produced, two capacitive arcs appear in the EIS. These two capacitive arcs are originated from the two parts of the corroded alloy surface, the original flat alloy surface and the new inter-face exposed to the aggressive EXCO solution due to the exfoliation or pitting corrosion. Some corrosion development features of 8090 Al-Li alloys in EXCO solution can be obtained through simulated EIS information.

Studies of Mixed-valence Compounds(Ⅰ)──In-Situ FTIR and UV-Visible-Near-IR Spectroelectrochemical Studies of Mixed-valence Isopolyanion Mo_6O_(19)^(3-) in Aprotic Media

The mixed-valence isopolyanion Mo6O193- was investigated by means of cyclic voltammographic, in-situ FTIR and UV-Visible-Near-IR spectro-electrochemicalmethods in aprotic media. The experimental results indicate that the Mo6O193-was formed whereafter Mo6O193- was reduced, (E0' = - 0. 690 V, n = 1 ). The characteristic absorptions of Mo6O193- are 500 nm, 900 nm and 1100 nm in UV-VisibleNear-IR spectrum and 940 cm-1 in IR spectrum.

A Reflectance Thin-layer Spectro-electrochemical Method

IntroduCtion Speetroeleetroehemieal measurement 15 simultaneously to determine theeleetroehemieal and speetral

Analysis of Urea in Petfood Matrices: Comparison of Spectro-Colorimetric, Enzymatic and Liquid Chromatography Electrospray Ionization High Resolution Mass Spectrometry Methods

Adulteration may consist in non authorized source of nitrogen addition to increase the protein content of some raw materials. Urea which is authorized for feed is a non nutritional source of nitrogen in food and pet food. Adulteration of food or pet food raw material by urea is thus monitored by manufacturer and governmental authorities with official methods which are either enzymatic (Association of Official Agricultural Chemists, AOAC) or spectro-colorimetric (European Community, EC). Each method gives results which are not comparable and spectro-colorimetric methods may result in false-positive urea detection. Liquid chromatographic (LC/UV-DAD) analysis of extracts from spectro-colorimetric method indicates that presence of free amino-acid may interfere with colorimetric detection of urea in the EC method with pet food samples. Liquid chromatography electrospray ionization high resolution mass spectrometry (LC/ESI-HRMS) has allowed to quantify low content (<0.01%) of urea in pet food water extracts for samples which resulted in significant urea detection with colorimetric method and in content below the detection threshold with enzymatic method. This study demonstrates the EC colorimetric method is not applicable to pet food and also food samples which have a complex composition with significant levels of free amino acids. On the other hand we clearly evidenced by means of the LC/ESI-HRMS results that the AOC Enzymatic method is applicable to urea quantification in pet food samples and gives reliable results.

SPECTRO M8光谱仪一例计算机故障的排除

本文介绍了一例SPECTRO M8计算机故障及其排除措施。

Review： Tip-based vibrational spectroscopy for nanoscale analysis of emerging energy materials

Vibrational spectroscopy is one of the key instrumentations that provide non-invasive investigation of structural and chemical composition for both organic and inorganic materials. However, diffraction of light funda- mentally limits the spatial resolution of far-field vibrational spectroscopy to roughly half the wavelength. In this article, we thoroughly review the integration of atomic force microscopy （AFM） with vibrational spectroscopy to enable the nanoscale characterization of emerging energy materials, which has not been possible with far-field optical techniques. The discussed methods utilize the AFM tip as a nanoscopic tool to extract spatially resolved electronic or molecular vibrational resonance spectra of a sample illuminated by a visible or infrared （IR） light source. The absorption of light by electrons or individual functional groups within molecules leads to changes in the sample＇s thermal response, optical scattering, and atomic force interactions, all of which can be readily probed by an AFM tip. For example, photothermal induced resonance （PTIR） spectroscopy methods measure a sample＇s local thermal expansion or temperature rise. Therefore, they use the AFM tip as a thermal detector to directly relate absorbed IR light to the thermal response of a sample. Optical scattering methods based on scanning near-field optical microscopy （SNOM） correlate the spectrum of scattered near-field light with molecular vibrational modes. More recently, photo-induced force microscopy （PiFM） has been developed to measure the change of the optical force gradient due to the light absorption by molecular vibrational resonances using AFM＇s superb sensitivity in detecting tip-sample force interactions. Such recent efforts successfully breech the diffraction limit of light to provide nanoscale spatial resolution of vibrational spectroscopy,which will become a critical technique for characterizing novel energy materials.

亚波长光栅与法布里-珀罗滤光片集成的高性能光谱偏振分光器

光谱偏振成像技术是一种新型的光学成像技术,它不仅提高了目标的信息获取量,还降低了背景噪声,可以捕获目标细节,检测伪装目标。本文提出了一种将亚波长光栅与F-P滤光片相结合的光谱偏振测量器件,该器件可以获得超高光谱分辨率和偏振消光比,并且光谱和偏振可以灵活调控。本文设计了一种光谱偏振同时分光器,可同时获得4个光谱通道的斯托克斯参数。仿真结果表明,其光谱分辨率为217,偏振消光比为106。实验结果表明,亚波长光栅的偏振消光比大于500,透射率为90%。全介质F-P滤光片的光谱分辨率为30,在长波红外波段的透射率为60%。该设计方法具有通用性,可用于可见光、红外甚至太赫兹等波段。得益于这些优点,器件在微型偏振光谱仪和全斯托克斯偏振检测等领域有很大的应用潜力。

俾路支褐煤有机结构特征及大分子模型构建

以巴基斯坦俾路支褐煤(BL)为研究对象,由元素分析得出BL化学式为C_(167)H_(130)O_(53)N_(2)S。经X射线光电子能谱(XPS)分析BL有机结构中氧、氮和硫元素存在形式。利用傅里叶变换红外光谱(FT-IR)研究BL有机结构中主要官能团特征,-CH和-CH^(2)为BL脂肪族结构中主要官能团。BL中苯环主要取代形式为三取代和四取代。运用核磁共振光谱(^(13)C-NMR)探究BL有机结构碳骨架结构。BL分子结构中,芳香桥碳与周碳之比X_(BP)为0.21,碳主要由芳香碳和脂肪碳2部分构成,其中脂肪碳质量分数53.23%,芳香碳占比41.93%。芳香结构以苯环和萘环为主,氧主要以羧基、羰基、醚氧和酚羟基形式存在,而氮主要以吡咯氮形式存在,硫主要为噻吩。建立BL二维分子结构模型,通过Materials Studio对其进行加氢饱和,构建BL分子模型三维立体结构,进一步优化所得分子模型,空间效果显著,得到能量最低的BL三维结构模型,发现范德华能是BL分子结构稳定的关键因素。通过计算得到的BL模型结构^(13)C NMR谱图与试验所测谱图基本一致,验证了所构建BL结构模型的合理性。

温度场下功能梯度圆锥壳-环板振动特性分析

针对功能梯度圆锥壳-环板组合结构振动问题,本文采用一阶剪切变形理论和Rayleigh-Ritz法分析了温度场下组合结构的振动特性。组合结构位移变量采用谱几何法来表征,考虑材料参数与温度相关并引入人工边界弹簧建立了组合结构振动特性分析模型。数值算例中,通过将文中求解结果与文献解和有限元法结果进行对比验证了模型的正确性,进而分析尺寸、材料、温度和连接位置等参数对结构振动特性的影响。研究结果表明:组合结构基频随厚度增加而增加,随着幂律指数、半顶角和温度场参数增加而降低,随环板内径和连接位置变化会呈现非单一变化趋势。

柠檬黄拉曼光谱、紫外可见吸收光谱的理论和实验研究

采用密度泛函理论(Density Functional Theory, DFT),在B3LYP/6-31+g(d, p)水平上对柠檬黄分子结构进行了优化,根据频率计算结果,绘制出拉曼光谱图并和实验获得的拉曼光谱谱图、表面增强拉曼光谱图进行了比对,实验和理论计算获得的拉曼光谱图基本上一致。基于势能函数分布的计算,对谱图信息丰富的500~2 000 cm^(-1)拉曼谱带的特征拉曼光谱进行了归属指认。基于含时密度泛函理论,计算了柠檬黄分子的激发态,理论计算得到柠檬黄分子的吸收光谱和实验采集得到的紫外-可见吸收光谱图进行了比对,分析了柠檬黄分子激发态的电子-空穴分布图。

多功能光谱仪定标方法

为了精确标定红外探测器的光谱响应函数,分别通过两点线性定标法、多点线性拟合定标法、非线性多项式拟合定标法以及远距离小面源定标法对多功能光谱辐射计进行标定,解算出辐射计的光谱响应系数和偏置系数,采用定标后的辐射计对不同温度黑体标准源的辐射亮度进行测量,并与黑体理论辐射亮度进行对比。结果表明,多点定标可减小噪声引起的随机误差和非线性响应引起的系统误差;当被测目标温度变化范围较小时,宜采用多点线性拟合定标,以减少噪声引起的随机误差带来的影响;当被测目标温度变化范围较大时,宜采用多点非线性拟合定标,以减少非线性响应引起的系统误差带来的影响;当被测目标温度较高时,光谱辐射计入瞳处信号较大,宜采用远距离小面源法标定,测量误差低于2%。定标后的测试精度优于国内外同类仪器。

Preconcentration of trace elements by adsorption onto a niobium wire for electrothermal atomization atomic absorption spectrometry with a tungsten tube atomizer

In the present method of trace elements wire has been developed work, a new preconcentration by adsorption onto a niobium for electrothermal atomization atomic absorption spectrometry （ETAAS） with a tungsten tube atomizer. Detection limits （pg. mL-1） by this method combined with ETAAS were 45 for bismuth, 7.0 for cadmium, 20 for copper, 1.3 for gold, 36 for lead, 65 for manganese, 9.5 for rhodium and 19 for silver.

热环境下功能梯度圆柱壳振动特性分析

应用谱几何法研究了热环境下功能梯度圆柱壳自由振动和瞬态振动特性。采用边界弹簧技术模拟圆柱壳结构的任意经典或者弹性边界约束条件,并结合一阶剪切变形理论建立了考虑温度场作用的功能梯度圆柱壳结构能量泛函。采用谱几何法与周向傅里叶谐波函数乘积和的形式描述圆柱壳的位移容许函数,以克服不同边界条件下壳体位移函数微分在边界上存在的不连续问题。在此基础上,将位移容许函数代入至结构能量泛函,并采用Ritz法获得结构振动分析模型。数值分析结果表明,所构建分析模型能够快速准确预测功能梯度圆柱壳结构的振动特性。研究了幂律指数、温度、载荷等参数对功能梯度圆柱壳振动特性的影响规律,为其他数值分析方法研究提供参考。

两种樱桃番茄冷藏后风味品质分析

为探究‘千禧’和‘吉甜一号’樱桃番茄冷藏中挥发性风味物质种类及相对含量差异,采用电子鼻和顶空固相微萃取–气质联用法分析4℃冷藏16 d后樱桃番茄(‘千禧’和‘吉甜一号’)风味品质的变化。结果表明:电子鼻分析结果显示两种樱桃番茄冷藏前后发生明显变化的挥发性物质是无机硫化物、氮氧化合物和芳香物质,采用HSSPME-GC-MS技术共检测出93种挥发性物质,包括27种醛类物质、23种醇类物质、4种酯类物质、11种酮类物质、3种呋喃类物质、9种烷烃类物质、12种烯烃类物质和4种其他物质。与0 d相比,‘千禧’和‘吉甜一号’冷藏后总挥发性物质相对含量分别降低了7.08%和3.68%。两种樱桃番茄的主要挥发性物质己醛和反-2-己烯醛相对含量在冷藏后下降,反式-2-戊烯醛、庚醛、1-戊醇、6-甲基-5-庚烯-2-酮和1-戊烯-3-酮等经冷藏后相对含量均增加。与‘千禧’相比,‘吉甜一号’经冷藏后可以保留较高的醛类、酯类和酮类等樱桃番茄主要挥发性物质含量,故‘吉甜一号’更利于采后储运和低温冷藏,可为高品质樱桃番茄采后储运技术提供理论依据。