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。     

建立统一的紫外、可见分光光度标准装置的探讨

介绍由低压石英汞灯、镨钕滤光片、透射比标准滤光片、杂散光滤光片等组成标准装置开展紫外、可见分光光度计的检定问题     

建立统一的紫外,可发光光度标准装置的探讨

介绍由低压石英汞灯、错钕滤光片、透射比标准滤光片、杂散光滤光片等组成标准装置开展紫外、可见分光光度计的检定问题。     

国产紫外分析灯的改装

在薄层层析、纸上层析等分析工作中,经常需要在紫外光下观察斑点的位置。紫外光源通常是用高压汞灯或低压汞灯,通过适当的滤光片得到以365nm 或254nm 波长为主的汞光谱线。目前不少单位都备有国产的紫外分析灯。这种灯使用500W 的玻璃外壳高压汞灯及透过365nm 的滤光片,得到365nm 波长的紫外光,只能用以观察由365nm 紫外光激发的萤光,不能用以观察对较短波长紫外光的吸收斑点或由较短波长紫外光激发的萤光斑点,并且此灯的紫外光强度也较弱,在使用上有很大的局限性。我们将这种紫外分析灯进行改装,改用石英外壳的汞灯,并使之既能在高压状态工作,又能在低压状态工作,并改成具有两种紫外滤光片。改装后的紫外灯,一灯多性能,既能得到较强的365nm 的紫外光,又能得到较短波长的254nm 的     

发射光谱仪检定规程中存在问题的探讨

从直读光谱仪的光路结构入手,对JJG 768–2005《发射光谱仪》中直读光谱仪部分的波长示值误差、检出限以及重复性和稳定性等检定项目和方法进行了讨论。研究发现,规程存在波长示值误差部分表述不准确、检出限和重复性、稳定性技术指标不详尽等问题。针对上述问题,建议修改"波长示值误差"这一表述,并将其作为后续检定的非必检项;在检出限检定部分对标准物质铁的含量加以要求,并注明元素分析谱线的波长值;对重复性和稳定性选用的标准物质作出元素含量范围的规定,以防造成误判。     

ICP-AES法测定石灰石、白云石中的Al_2O_3,CaO,TFe_2O_3,MgO,MnO,SiO_2,TiO_2

采用无水碳酸钾＋硼酸处理样品,电感耦合等离子体发射光谱法同时测定石灰石及白云石中7种组分,筛选了不同仪器参数条件,对各组分分别选用2条相对谱线强度适中的谱线进行分析,并以元素平均值的模式输出数据结果,测定的相对标准偏差小于0.60%.经对国家一级石灰石及白云石标准物质分析验证,结果与标准值吻合.     

北京有色金属研究总院：空心阴极灯生产线简介

空心阴极灯是一种广泛应用于原子吸收光谱分析,原子荧光光谱分析,分子吸收光谱分析以及其他需用线光谱光源和基准波长等仪器中的锐线光源。我院致力于空心阴极灯的研制和应用四十年,在长期的生产实践中积累了丰富的经验。生产普通空心阴极灯（AS系列）具有特征谱线光谱辐射强度高,稳定性好,背景低,寿命长等特点。该产品质量可靠并已打入国际市场。     

可变波长紫外—可见光检测器的研制和应用

本文介绍可变波长紫外－可见光检测器的研制和应用。采用凹面全息光栅、光导纤维分束器等新技术，以及锥形流通池设计，构成双光束光学系统，以功率ＭＯＳ场效应晶体管新型功率器件构成灯电源电路，单片微机控制系统完成时各个机械部件的控制，以及提供固定波长、时变波长两种工作模式。本文还以ＮＯ２－和Ｂｒ分离检测例证实时变波长工作模式，将显著地提高检测灵敏度。     

空气—氩气混合气冷却ICP—AES中钙,钡,铜,锌元素的谱线强度和信？…

研究了小功率空气－氩气混合气冷却ＩＣＰ中４种元素（钙、钡、铜、锌）、８和谱线的强度和信背比随冷却气组成及观测高工估算了折中条件下的检出限。对于离子线及激发电位较高的原子线,冷却气中引入体积分数为５－１０％空气后,谱线强度最大并大于Ａｒ－ＩＣＰ中数值;对于激发发电位较低的原子线,随着气中空气含量的增大其谱线强度逐渐减小,谱线的信背比则与激发电位及谱线波长有关。     

光胶做挡光层的紫外光刻掩膜用于高聚物芯片表面选择性光化学改性

紫外光谱研究表明,AZ正性光胶当厚度大于10μm时,在200～285nm的紫外光区几乎不透光。本研究据此研制了一种以固化后的AZ光胶做挡光层、石英玻璃做底板的紫外光刻掩膜。应用AZ光胶掩膜对聚碳酸酯(PC)表面进行以低压汞灯(主要辐射254nm紫外光)为光源的选择性光化学改性,在光照区域形成化学镀所需的催化中心后,采用化学镀技术,在PC毛细管电泳芯片上制备安培检测用的集成化金微电极。本掩膜材料简单,制作方便,无须洁净实验室和贵重的设备,成本低廉。     

Development of a New Type of Light Modulated DSC

A new type of the light modulated DSC was constructed. Optical fibers are used to separate the light source from the furnace. The sample can be handled accurately because the lamp and the intensity modulator are not above the furnace. Quality of the measured signal is much improved by extracting the analog signal from the electronic circuit board in the commercial DSC. Light intensities of the sample and reference sides are controlled independently from each other. A method to compensate for the asymmetry of the thermal system utilizing the independent control of the light intensity is proposed. This revised version was published online in July 2006 with corrections to the Cover Date.     

碳纳米微粒的共振散射光谱研究

液相碳纳米微粒的共振散射光谱实验表明,当碳浓度小于360mg/L时,它在400、470、510和940nm产生4个共振散射峰;浓度大于900mg/L时无共振散射、碳微粒浓度在0．45－45mg/L范围内与共振散射光强度I470nm成良好的性关系,研究了光源和扫描速度对液相碳纳米微粒共振散射光谱的影响。结果表明,光源的发射强度分布不一是产生共振散射光谱峰的一个重要因素,并结合已有的实验结果提出了界面共振吸收和黑白纳米微粒共振散射概念,解释了碳纳米微粒体系的共振散射光谱。     

Application of a xenon arc lamp as a light source for evaporative light scattering detection

The standard tungsten-halogen light source used in a commercial evaporative light scattering detector (ELSD) was replaced with a 180 W xenon arc lamp. The xenon arc lamp possesses a broader spectrum in the UV region than the halogen source. The influence of the UV transmittance of five selected solvents was studied with a size-exclusion chromatography column. This solvent parameter was not observed to influence the ELSD response between the two light source settings. With the solvents studied, better sensitivity was obtained with the xenon arc lamp than the halogen lamp. This high-energy source was applied to ceramide III analysis with an octadecyl-grafted silica column and methanol:tetrahydrofuran 97:3 as the mobile phase, and the sensitivity of the quantification of ceramide III increased 16-fold for injected amounts of 14∼140 ng. The molecular species in a sample of naturally occurring ceramides was analyzed using two C18 columns at 40 °C and gradient elution from 100% acetonitrile to 100% isopropanol in 30 min. The increased ELSD sensitivity achieved when using the xenon arc lamp allowed both the minor and major ceramide species to be observed, in contrast to the results achieved when the halogen lamp was used, where the increased photomultiplier voltage needed to observed the signals from the minor species caused the signals from the major ceramide species to occur above the detector response window.     

Microwave-assisted degradation of acid orange using a conjugated polymer,polyaniline, as catalyst

Microwave-assisted photocatalytic degradation of dyes is one of the emerging technologies for waste water remediation. Microwave effectively accelerates photocatalytic degradation, when microwave electrodeless lamp (MEL) substitutes traditional UV lamp as light source. This setup can be extremely simplified if MEL and photocatalyst can be replaced by a catalyst which can work under microwave irradiation in the absence of any light source. The present work reports for the first time degradation of acid orange 7 (AO) under microwave irradiation using polyaniline (PANI) as catalyst in the absence of any UV lamp as light source. The degradation/decolourization was carried out in neutral acidic and basic media and was monitored spectrophotometrically to evaluate the ability of microwave irradiation to degrade AO. Microwave irradiation showed excellent performance as it completely decolourizes AO dye solution in 10 min. With the advantages of low cost and rapid processing, this novel catalyst is expected to gain promising application in the treatment of various dyestuff wastewaters on a large scale.     

Construction of a light-emitting diode fluorescence detector for high-performance liquid chromatography and its application to fluorometric determination of L-3-hydroxybutyrate

This study employed a new light source, a light-emitting diode (LED), for fluorescence detection of high-performance liquid chromatography to measure the concentration of trace constituents in biological fluids. Using l-3-hydroxybutyrate ( l-3HB) as a tested trace compound, the function of the new system was compared with that of the current commercially available model. A detailed schematic diagram of the path of the detection rays in the LED detector is given. A voltage-stabilizer for the drive circuit was designed with an input of 10 V and an output of 8 V, and another voltage regulator was used to maintain a constant 8 V. Then the regulator was used to set the output voltage for the LED at 2.8 V by two external resistors. Replacing the xenon lamp with LED, this system provided higher photon density and a narrow spectrum at a wavelength of 491 nm. At room temperature (22.1°C), the average temperature of six places in the chamber of LED detector was 22.1°C compared with 51.1°C in the xenon detector. The spectra of the excitation light sources were measured. Compared with the xenon lamp, approximately 1.32 times higher excitation intensity was obtained by the LED source. The accuracy of detection of l-3HB in 50 μL of rat serum was 99.85-100.85%, and the intra-day and inter-day precision values were within 8.99 and 13.90%, respectively. The limit of detection of l-3HB was approximately 0.73 μM (signal-to-noise ratio 3). The sensitivity of the proposed LED detector was comparable to that of traditional fluorescence detectors using xenon arc lamps; however, the cost and operating temperature of LED lamps were far lower. This assay system could be further used to detect trace constituents in various samples.     

CuInSe2/氰桥混配物复合修饰光电极的制备及其光电性质

利用电沉积法在氰桥混配物预修饰的玻璃碳电极上再沉积CuInSe2半导体材料,制备了一种复合型修饰光电极(Eu-Fe-Mo/CuInSe2)。以含Cu2+、In3+、SeO23-及柠檬酸钠的酸性水溶液为电镀液,通过优化寻找到电镀液中最佳的Cu∶In∶Se料液比例,用恒电位电沉积法可以制备出具有良好光电效应的复合型修饰光电极。用SEM、EDS技术对复合修饰光电极的表面形貌及其修饰材料的元素组成进行了表征;以60 W的普通日光型白炽灯为光源,采用开路电压和计时安培法研究了该复合修饰光电极的光电性质。测得该光电极的响应光电压大于30 mV,响应光电流密度大于8.9×10-6A/cm2。实验结果表明,该复合修饰光电极呈现典型p型半导体的光电性质。     

一种新型MPEGD光源的光谱分析性能研究

报道了一种改进的微波等离子体增强放电（ＭＰＥＧＤ）光源，并将这种联光源用于固体导电样品的分析，详细研究了它对分析物的检测能力和增感作用，证明该光源在固体样品成份分析和表面逐层分析中有良好的应用前景。     

大型仪器功能开发(151~159)瓦里安300XP离子注入机改造及功能开发

在完全掌握瓦里安300XP离子注入机各部件的工作原理后, 将原离子源供电系统中500 W电流源和450 W起弧电源升级为1 500 W电流源和1 500 W起弧电源, 并集成到当前系统中.将现有不稳定的气体流量、离子源电源、分析器、源磁场和吸极高压塑料光纤隔离控制线路, 升级成多通道光纤通讯光端机隔离控制系统.将一个10 cm进样终端改造成15 cm的样品卡盘, 并开发了一套独立控制剂量监测系统.改造后, 硼最大束流超过150 μA, 且可调节. 15 cm圆片的片内及片间电阻不均匀性小于3.5%.利用大束流硼离子注入制备浓硼掺杂单晶硅结构层, 应用到微电子机械系统压力传感器、热电器件以及纳米谐振子器件中.     

4-乙烯基-1-环己烯二环氧化物阳离子单体光聚合性能研究

本文用实时红外光谱研究了4-乙烯基-1-环己烯二环氧化物(TTA22)单体的光聚合性能。分别考察了光引发剂浓度、光源、光强及增感剂浓度对其光聚合性能的影响。选用3,4-环氧环己基甲酸-3′,4′-环氧环己基甲酯(TTA21)作为参照,比较了不同单体的光固化性能。结果表明,随着引发剂浓度以及光强的增加,环氧基转化率及转化速率随之增加。LED光源下单体的转化率和转化速率低于UV汞灯。对TTA22和TTA21光固化后材料的热稳定性进行分析,结果显示TTA21的热稳定性优于TTA22的。