用智能波长校正的扫描式电感耦合等离子体光谱仪测定高炉渣中7种…

本文利用作者所在实验室发现的，光栅单色仪的出射光谱线峰漂移与温度变化以及波长变化间的非线性函数关系，以及在此基础上所开发的扫描式ＩＣＰ－ＡＥＳ光谱仪的智能波长校正装置，取代传统的局部恒温系统，测定了高炉渣中的Ｓｉ，Ｃａ，Ｍｇ，Ｍｎ，Ｆｅ，Ｔｉ，Ａｌ７种元素成份，测定结果与标样的鉴定值一致，测量的相对标准偏差（ＲＳＤ）为１．ｘ％。智能波长校正装置的波长校正结果与谱线峰描迹结果的比较表明，该智能波长校     

扫描式电感耦合等离子体光谱仪谱线峰位移的机理研究

通过对扫描式电感耦合等离子体原子发射光谱仪(ICP-AES)出射光谱线峰位移(Δλ)的机理研究,发现温度的变化、波长的变化以及光谱仪机械的系统误差是产生谱线峰位移的主要因素,首次测量了谱线峰位移与波长变化之间的非线性函数关系曲线Δλ-λ,以及谱线峰位移与温度变化之间的非线性函数关系曲线Δλ-T,并用多项式方程表达了这些函数关系。本研究还发现,不同的光栅单色仪有近似相同的Δλ-λ函数关系曲线,但是Δλ-T的函数关系曲线却很不相同。利用这些非线性函数方程式,设计开发了扫描式ICP-AES光谱仪的智能波长校正装置(IWC),用它取代传统的局部恒温系统及谱线描迹法进行样品分析的结果表明,智能波长校正的ICP光谱仪(ICP-IWC)谱线峰定位精度高,具有省时、安全、结构简单的特点,有广阔的应用前景。     

应用遗传算法和PLS的近红外光谱预测玉米中淀粉含量的研究

以普通玉米籽粒为试验材料,在应用遗传算法结合偏最小二乘回归法对近红外光谱数据进行特征波长选择的基础上,应用偏最小二乘回归法建立了特征波长测定玉米籽粒中淀粉含量的校正模型．试验结果表明,基于11个特征波长所建立的校正模型,其校正误差（RMSEC）、交叉检验误差（RMSECV）和预测误差（RMSEP）分别为0.30％、0.35％和0.27％,校正数据集和独立的检验数据集的预测值与实际测定值之间的相关系数分别达到0.9279和0.9390,与全光谱数据所建立的预测模型相比,在预测精度上均有所改善,表明应用遗传算法和PLS进行光谱特征选择,能获得更简单和更好的模型,为玉米籽粒中淀粉含量的近红外测定和红外光谱数据的处理提供了新的方法与途径．     

三波长校正光度法测定水果蔬菜中多菌灵残留量

研究了三波长光度法测定水果蔬菜中多菌灵残留量的最佳测定条件,在pH8．3的条件下,测定278,281和290nm波长处的吸光度,计算出校正吸光度,校正吸光度与多茵灵含量在0～50μg范围内呈线性关系,相关系数为0．9991,方法检出量为0．773μg;样品的加标回收率在93．5％～101．0％范围内,测定结果满意。     

多波长线性回归法校正火焰原子吸收光谱干扰

用多波长线性回归法校正了火焰原子吸收分析中Ｇａ４０３．２９８ｎｍ对Ｍｎ４０３．３０７ｎｍ的吸收线重叠干扰，对合成样中Ｍｎ和Ｇａ含量的测定，结果令人满意。     

Te掺杂n型GaAs材料的光致发光研究

对Ｔｅ掺杂ｎ型ＧａＡｓ材料在３００～６０Ｋ之间的辐射复合进行光致发光（ＰＬ）研究。用发射波长为５１０．６ｎｍ和５７８．２ｎｍ的溴化亚铜激光器为激发光源。在所选取的狭缝宽度下谱仪的分辨率约为２ｎｍ。所提供的数据全部经过系统灵敏度校正并进行分峰拟合。对ＰＬ谱中一些主要特征进行讨论，认为Ｔ１，Ｔ２，Ｔ３三个发射带分别对应着导带价带（Ｔ１）和施主受主（Ｔ２，Ｔ３）的跃迁，它们随温度变化的情况与带隙宽度及电子填充状态随温度变化有关。此外，还注意到ＰＬ谱的长波端（～９５０ｎｍ）呈上扬趋势，表明可能在低能区域存在一个与深能级复合有关的宽发射带     

单扫描极谱-偏最小二乘法同时测定丁基锡混合物

在pH6．0的乙酸-乙酸钠缓冲液中，三丁基锡、二丁基锡和一丁基锡有各自的极谱峰电流，但彼此之间存在相互干扰，难以同时进行极谱测定。文中运用偏最小二乘的多元校正能力，对三种丁基锡混合物极谱图进行多元校正，获得了较好的定量分析结果。回收率为96．2％～101．2％，相对标准偏差为3．2％～11．9％。     

混合线性分析法同时测定安痛定注射液中三组分含量

将一种新近发展的多元校正方法——混合线性分析法，用于安痛定注射液中氨基比林、安替比林、巴比妥含量的同时测定。在220～250nm内取16个波长测量7组标准混合溶液的吸光度矢量作为校正集，以最小二乘法求得系数矢量作为各组分的纯光谱，用混合线性分析法进行数据处理。氨基比林、安替比林、巴比妥的标准回收率分别为99．0％～100．3％、99．0％～100．8％和98．5％～101．1％。用于安痛定注射液中氨基比林、安替比林、巴比妥三组分含量的测定，经t检验，其测定结果与标准法相比，两者间无显著性差异。     

溴甲酚绿为内标二苯碳酰二肼光度法测定水体中六价铬的研究

采用溴甲酚绿为内标，二苯碳酰二肼(DPC)光度法测定水体中的六价铬。铬与DPC显色铬合物和内标物的最大吸收波长分别为540nm和440nm，校正后的A^Cr540／A^Br440值与Cr含量之间呈良好的线性关系，相关系数为0．9997。对于高度污染的工业废水，可取显色溶液进行任意稀释测定。应用本法对电镀废水进行了测定，其相对标准偏差为1．2％～2．4％，加标回收率为98％～104％。本方法测定结果与标准方法测定结果无显著差异。     

反相高效液相色谱法测定罗红霉素的含量

以Kromasil C18柱为色谱柱、0．067mol/L磷酸二氢铵缓冲液一乙腈(体积比为65：35)为流动相，选择210nm为检测波长，用反相高效液相色谱法测定罗红霉素的含量。罗红霉素的浓度在0．5～8．0mg／mL范围内与色谱峰面积呈良好线性关系，线性相关系数为0．9999，平均回收率为100．97％，测定结果的相对标准偏差为0．36％(n=9)。该方法操作简单、快速，可用于罗红霉素含量的测定。     

分光光度计波长校准用低压汞灯的研制

基于辉光放电原理,采用小功率点光源及高频开关电源设计分光光度计波长校准用WSHg-B型低压汞灯,并提出汞灯辐射光谱波长不确定度的分析方法。实验结果表明,WSHg-B型低压汞灯在200～700nm波长范围内,具有分布均匀的线光谱,相对强度稳定,适用于各类通用紫外可见分光光度计的波长校准,还可用于分辨率及光谱带宽的测试。     

湿度计量标准平台的研制

研制了湿度计量标准平台,包括精密露点测量、标准湿度发生、湿度传感器测试校准装置3个系统。各系统通过计算机软件控制,能够按照设定步骤工作,既可完成对常规湿度测量仪器的检定测试,又可对智能湿度传感器进行通讯并对其校准。     

双波长K系数-标准加入-导数分光光度法同时测定重油中的钴镍

本文提出了一种同时测定两组分混和物的新方法，即双波长Ｋ系数－标准加入－导数分光光度法，该法同时进行两组分的标准加入，以两个组分的峰值波长为测定波长，又互为参比波长，利用Ｋ系数法以一套吸光度数据同时完成两个组分的测定。本文以ＯＰ－５－Ｂｒ－ＰＡＤＡＰ为显色体系，同时测定了重油中的钴、镍，结果令人满意。本方法简便，灵敏度高。     

A versatile standard for bathochromic fluorescence based on intramolecular FRET

A perylene and a terrylene tetracarboxylic bisimide dyad was prepared in which an efficient energy transfer from the former to the latter is observed. The absorption spectrum of this compound covers a broad range. Bathochromic fluorescence with a high quantum yield was obtained independent of excitation wavelengths (λ < 655 nm). The dyad can be recommended for the use of calibrating fluorescence spectrometers, as well as a fluorescence standard in the bathochromic region.     

Parametric models to compute tryptophan fluorescence wavelengths from classical protein simulations

Fluorescence spectroscopy is an important method to study protein conformational dynamics and solvation structures. Tryptophan (Trp) residues are the most important and practical intrinsic probes for protein fluorescence due to the variability of their fluorescence wavelengths: Trp residues emit in wavelengths ranging from 308 to 360 nm depending on the local molecular environment. Fluorescence involves electronic transitions, thus its computational modeling is a challenging task. We show that it is possible to predict the wavelength of emission of a Trp residue from classical molecular dynamics simulations by computing the solvent‐accessible surface area or the electrostatic interaction between the indole group and the rest of the system. Linear parametric models are obtained to predict the maximum emission wavelengths with standard errors of the order 5 nm. In a set of 19 proteins with emission wavelengths ranging from 308 to 352 nm, the best model predicts the maximum wavelength of emission with a standard error of 4.89 nm and a quadratic Pearson correlation coefficient of 0.81. These models can be used for the interpretation of fluorescence spectra of proteins with multiple Trp residues, or for which local Trp environmental variability exists and can be probed by classical molecular dynamics simulations. © 2018 Wiley Periodicals, Inc.     

A microfabricated capillary electrophoresis chip with multiple buried optical fibers and microfocusing lens for multiwavelength detection

We present a new microfluidic device utilizing multiwavelength detection for high-throughput capillary electrophoresis (CE). In general, different fluorescent dyes are only excited by light sources with appropriate wavelengths. When excited by an appropriate light source, a fluorescent dye emits specific fluorescence signals of a longer wavelength. This study designs and fabricates plastic micro-CE chips capable of performing multiple-wavelength fluorescence detection by means of multimode optic fiber pairs embedded downstream of the separation channel. For detection purposes, the fluorescence signals are enhanced by positioning microfocusing lens structures at the outlets of the excitation fibers and the inlets of the detection fibers, respectively. The proposed device is capable of detecting multiple samples labeled with different kinds of fluorescent dyes in the same channel in a single run. The experimental results demonstrate that various proteins, including bovine serum albumin and beta-casein, can be successfully injected and detected by coupling two light sources of different wavelengths to the two excitation optic fibers. Furthermore, the proposed device also provides the ability to measure the speed of the samples traveling in the microchannel. The developed multiwavelength micro-CE chip could have significant potential for the analysis of DNA and protein samples.     

Calibration of wavelength-dispersive X-ray spectrometer for standardless analysis

An experimental procedure for calibrating wavelength-dispersive X-ray spectrometer is presented. The detection efficiency was determined from the ratio of fluorescent radiation measured using the flow-proportional and the scintillation counter. The relative reflection efficiency of the analyzing crystal for various wavelengths was determined from the X-ray measurements of standard samples. The absorption correction for the atmosphere in the spectrometer chamber was also experimentally examined. All parameters (with the exception of reflection efficiency of the analyzing crystal) can be calculated from the X-ray measurements of unknown samples.     

基于表面等离子体子共振的白蛋白免疫传感器的研究

采用自行组装的全波长表面等离子体子共振(SPR)传感装置,以对金和蛋白抗体均有较强吸附作用的A蛋白作为基底膜,测试了A蛋白在金膜表面结合的动力学常数,其结果为2.3×10⁵L/(mol·s).研究了在A蛋白基底膜上白蛋白抗体的定向自组装程度和速率.观测了白蛋白抗体与抗原之间免疫反应的动力学过程,并优化了实验条件.结果表明,白蛋白抗原的浓度在0.02～10mg/mL范围内与信号的响应值呈良好的线性关系.将此SPR传感器用于糖尿病肾病患者尿蛋白的检测,结果较好.     

Short-wave near-infrared spectroscopy analysis of major compounds in milk powder and wavelength assignment

In this study, short-wave near-infrared (NIR) spectroscopy at 800–1050 nm region was investigated for the analysis of main compounds in milk powder. Through quantitative analysis, the feasibility is further demonstrated for the simultaneous measurement of fat, proteins and carbohydrate in milk powder. Two models, partial least-squares and least-squares support vector machine, were compared and utilized for regression coefficients and loading weights. The affect of standard normal variate spectral pretreatment to model performance was evaluated. Based on the resulted coefficients and loading weights, interesting wavelength regions of nutrition in milk powder are screened and the assignment of all specific wavelengths is firstly proposed in the details associated with chemical base. Instead of the whole short-wave NIR spectral data, these assigned wavelengths which can be reliably exploited were used for the content determination. Compared with other spectroscopy technique, assigned short-wave NIR spectral wavelengths did a good work. Determination coefficients for prediction are 0.981, 0.984, and 0.982, respectively for three components. The proposed wavelength assignment in the short-wave NIR region could be used for the component contents determination of milk powder, and could be as a guidance to interpret the spectra of milk powder.