太阳CO 4.6微米红外成像观测

太阳红外光谱中蕴含着丰富的物理信息,其中CO 4.6μm波段是具有代表性的分子谱带,其形成于温度极小区附近,对研究太阳物理具有极其重要的意义。为获得CO 4.6μm波段太阳单色像,本文建立了一套全反射太阳红外成像观测系统。该系统采用定天镜跟踪引光,通过成像反射镜将太阳成像于3~5μm波段红外相机的焦平面上,该相机采用的是国产HgCdTe焦平面阵列器件。同时,为提高信噪比,提出了一种有效计算平场提取观测目标的方法,并利用该方法获得了CO 4.6μm波段的太阳单色像。     

钙钛矿阵列化组装及其多功能探测器的应用

钙钛矿材料优异的光电性能使其在高集成、 高性能、 多功能光电探测领域具有广泛的应用前景. 近年来, 科研人员致力于钙钛矿阵列化探测器的研究, 并取得了一系列重要的成果. 本文重点评述了钙钛矿材料的阵列化及其多功能探测器的制备和应用, 介绍了钙钛矿材料的结构分类、 阵列化集成方法及光电探测器的基本器件类型和性能指标, 并进一步阐述了基于钙钛矿一维阵列的高性能光电探测器及其多功能探测器的相关应用研究进展. 最后, 对该研究领域未来的发展方向进行了总结和展望.     

电位无标型糖化血红蛋白免疫微传感器

研制了基于标准CMOS工艺和微加工技术的电位无标型免疫微传感器,可实现糖化血红蛋白浓度与血红蛋白浓度的简便检测。该微传感器包括含有信号读出电路的场效应型微传感集成芯片和一次性测试试条。微传感集成芯片由本实验室设计并经新加坡Chartered半导体公司流片制备。一次性测试试条采用微加工技术制备于柔性塑料片上,包括敏感电极阵列和三维微结构测量池。基于自组装单层膜并引入纳米金颗粒的方法,在测试试条电极表面固定抗体。采用循环伏安法和交流阻抗法对电极表面的修饰过程进行了测试和分析。该传感器对糖化血红蛋白和血红蛋白检测的线性范围分别为4～24mg/L和60～180mg/L。     

光纤分导微梁阵列生化传感装置研制及检测应用

研制了一套基于光杠杆原理的微悬臂梁阵列传感器平台,并通过使用设计制作的微悬臂梁阵列芯片展示其在生物化学方面的检测应用.传感器平台使用光导纤维束分别与激光器耦合作为悬臂梁阵列的扫描光源,具有良好的检测稳定性,检测信号噪声水平约为2 nm;设计制作的微悬臂梁阵列芯片具有良好的平直度,温度响应均匀一致,各梁温度改变响应灵敏度偏差不超过5.0％.将整套传感系统被用于检测水溶液中的Hg2+,检测浓度范围为1 ～ 200 ng/mL;同一浓度下微悬臂梁阵列检测结果曲线一致性良好,平均偏差小于15％.在研制仪器平台上,分别实现了自制和国外商品化芯片对1.0和0.2 ng/mL样品的检测,结果表明,制作的微悬臂梁阵列芯片的检测灵敏度相对较低,需进一步改进悬臂梁阵列制作工艺.     

新型微梁阵列生化传感器的研制

为了消除单微梁生化传感系统中存在的温度漂移、溶液折射率变化等环境噪声影响,同时实现多种靶标分子的快速并行检测,设计制作了新型微梁阵列生化传感器.利用压电驱动激光束扫描微梁阵列,并通过光杠杆法实时读出微梁弯曲信号,即可得到在微梁表面发生的特异性生化反应的动力学曲线.对250 μm间距的两定点的9h扫描实验数据验证了系统光路的稳定性;同时进行了温度激励测试,升温6℃后微梁阵列弯曲信号基本保持一致(误差6.5％),验证了系统检测的可靠性.最后,利用自制毛细管阵列套合修饰装置,成功将克伦特罗抗体修饰到微梁阵列一侧的金表面上,对待测液中10μg/L克伦特罗标样进行了准确检测,验证了此传感系统在生化检测中的实际可行性.     

同位素内标稀释气相色谱-质谱联用法测定果蔬中的滴滴涕含量

建立了果蔬中滴滴涕(DDT)的气相色谱-质谱联用的测定方法。样品用乙腈提取,采用Florisil固相萃取柱净化,以HP-5ms色谱柱(30m×0.25mm×0.25μm)分离,在选择离子模式(SIM)下,以自行研制的p,p′-DDT-D8为内标进行定性定量分析。线性范围为1~1 000μg/L,检出限为0.02~0.05μg/kg,加标回收率为88.67%~101.73%,相对标准偏差(RSD)为1.6%~3.8%(n=5)。该方法为果蔬中滴滴涕的检测提供了一种可靠实用的方法。     

电子俘获材料在光记录中的应用

研究了自行研制的CaS(Eu,Sm)电子俘获材料的光学性质;利用～200μm厚的CaS(Eu,Sm)高聚物膜作为记录底片,进行了实物图象的拍摄实验。这种记录材料具有很多有吸引力的优点:不需要用化学溶液进行定影显影,可以实时读出,可快速擦除,能反复使用,具有大的线性范围等。实验表明,电子俘获材料是一种很有前途的光记录材料。     

高效液相色谱法检测一次性纸杯中的双酚A

建立了高效液相色谱法测定一次性纸杯中双酚A的分析方法。采用Diamonsil C18(250mm×4.6 mm,3μm)反相色谱柱,以甲醇-水溶液为流动相,光电二级管阵列检测器,检测波长为228nm。线性范围为0.1~100mg·L-1,相关系数为0.9996,方法的回收率为92.1%~96.4%,相对标准偏差为3.2%~5.7%。该方法简便、灵敏准确,能够满足双酚A的检测要求。     

新型红外测油仪中的光谱视网膜技术

将光谱视网膜技术应用于红外测油领域,研制出一种新的MFA-450型红外测油仪.介绍了所研制的超窄带、高透过率的中红外多波长滤光片和具有较高性能价格比、适合我国国情的红外热释电阵列检测器及相应检测电路和操作软件的开发.该仪器体积小、重量轻、无可动部件、稳定性好;测量精密度高(RSD<1％);灵敏度较现有同类仪器高1个数量级,检出限达到0.02mg/L(油/萃取剂);测量线性范围0.10～120.00mg/L,相关系数R2>0.999.     

一维Bi_2Fe_4O_9纳米棒阵列的无模板水热合成

以物质的量的比为1∶1的Bi(NO3)3·5H2O和Fe(NO3)3·9H2O为反应原料,以NaOH为矿化剂,利用水热法在Ti基板上成功制备出一维Bi2Fe4O9纳米棒阵列。对该纳米棒阵列分别进行XRD、FE-SEM、HR-TEM和UV-Vis测试,得到Bi2Fe4O9纳米棒的直径为100 nm,长度为3~4μm,并表现出良好的光吸收性能,禁带宽度约为1.9 eV,对甲基紫溶液的光降解率达到86%,其活性明显高于市售P25(TiO2)。该纳米棒阵列的生长方式完全遵循奥斯瓦尔德熟化(Ostwald ripening)单晶生长机理。     

Design and characterization of an intensified diode array data-acquisition system for spectrometric measurements

A computer-based data-acquisition system for an intensified diode array (IDA) detector is described. A unique combination of hardware and software provides many data-acquisition and calculation options useful for multiple-wavelength spectrometric measurements. The data-acquisition system is used to evaluate critically many characteristics of the IDA detector, including the dependence of the light and dark signals and noise on experimental variables, and the linearity, memory effects and resolution.     

Determination of adriamycin and daunorubicin in urine by high-performance liquid chromatography with laser fluorometric detection

A separation and detection scheme is presented for the determination of the antitumor drugs adriamycin and daunorubicin in human urine. Separation is accompished by reversed-phase high-performance liquid chromatography and the drugs are detected down to the low picograms level by laser excited fluoresence using a unique fiber optic based flow-cell. Excellent detector selectivity and linearity are reported, and some of the factors influencing the performance of the detector are discussed. Possible extension of the procedure to other biologically important determinations are mentioned.     

利用电流积分器和峰值保持单元改进固体电极上的多重峰测量和提高记录仪记录伏安图的精确性

本文推荐采用电流积分器和峰值保持(检测)器作为插入单元,以测量积分电量代替峰高测量,改进固体电极上的测量浓度范围。并采用峰值检测器提高记录仪的响应,使之适用于500～1000mV/s扫描速率下的伏安测定。本文以T(Ⅳ)作为例子证明上述优点。     

The optimization of HPLC-UV conditions for use with FTIR detection in the analysis of B vitamins

The water-soluble vitamins thiamine (B(1)), riboflavin (B(2)), pantothenic acid (B(5)), and pyridoxine (B(6)) are separated by high-performance liquid chromatography. The mobile phase, column temperature, and flow rate are optimized so that the chromatograph can be used with a Fourier-transform infrared (FTIR) detector. Reproducibility, linearity, and detection limits are evaluated for method validation. Finally, this method is successfully transferred to liquid chromatography-FTIR with a standard mixture.     

A 14 Parameter Study of UHPLC’s for Method Development Transfer and Troubleshooting

Five ultra-high pressure liquid chromatography (UHPLC) instruments were compared to one another by examining the overall system performance and key functions of the system parts including: pump, auto-sampler, thermo-stated column compartment, and the detector. The five UHPLC systems used in this study were: ThermoFisher Vanquish, Agilent 1290 Infinity I, Agilent 1290 Infinity II, Waters Acquity I-Class, and Shimadzu Nexera X2. The identities of the systems were blinded in the results and discussion section to use this study for scientific purposes only rather than for competition and marketing. The following tests were performed to evaluate and compare the five UHPLC systems: injector linearity and precision, sample carryover, sample (autosampler) temperature accuracy, column temperature accuracy and precision, pressure ripple, pump mixing accuracy, flow rate accuracy, detector drift and noise, detector linearity, wavelength accuracy, extra-column volume, and dwell volume determination. This study presents an approach on how to test the performance of UHPLC systems along with potential problems that analysts may face when using the UHPLC systems, examples of such issues are: retention time irreproducibility, low sensitivity, method transfer failure, etc.     

Analytical instrument qualification in capillary electrophoresis

Capillary electrophoresis (CE) is a well-established and frequently used technique in the pharmaceutical industry. Therefore an appropriate analytical instrument qualification (AIQ) is required for quality assurance. AIQ forms the basis of a quality management followed by analytical method validation, system suitability tests (SSTs) and quality control checks. Two parts of the AIQ, namely the operational qualification (OQ) and the performance qualification (PQ) are of particular interest in the daily routine of the laboratory. A new concept for OQ and PQ was developed to assure the correct function of a CE system. The significance of each parameter, possible test methods as well as acceptance criteria will be presented and discussed in detail. Especially temperature adjustment by the cooling system and the voltage supply must be tested for accurate and precise operation. The detector noise, wavelength accuracy and detector linearity have to be checked as well. Finally, the injection linearity, accuracy and precision need to be qualified. The proposed set of qualification procedures is easy to implement and was already tested on five CE instruments from three different manufacturers. A time- and cost-saving continuous PQ was derived, using results from method-specific SSTs and some additional experiments. This holistic concept continuously surveys the most relevant parameters, hence assuring the suitability of the used instruments and decreasing their downtimes.     

Ultraviolet photodetector based on ZnO nanorods grown on a flexible PDMS substrate

A flexible, reproducible, sensitive and low-cost ultraviolet (UV) detector has been fabricated based on zinc oxide (ZnO) nanorods grown on a patterned polydimethylsiloxane (PDMS) substrate. The substrate was seeded with ZnO nanoparticles synthesised via simple low-temperature hydrothermal method using pomegranate peel extract as a reducing agent. The produced ZnO-nanorods/PDMS (ZnO-NR/PDMS) samples were tested for their UV-sensing properties. Samples were characterised using scanning electron microscopy, X-ray diffraction, I–V characteristics, UV-Vis spectroscopy and photoluminescence measurements. The UV photoresponse mechanism of prototype UV detector was analysed. The detector exhibited quite high on/off ratios between photoresponse current and dark current. With the flexible PDMS substrate, the detector photoresponse was tested with and without bending and exhibited a very slight change in the photoresponse current. The detector current–time response was also tested under various UV light intensities for three test cycles to examine the detector stability, hysteresis behaviour and performance. It is anticipated that the fabrication of ZnO-NR/PDMS UV detector may have significant potential application in flexible optoelectronic devices.     

Microbore liquid chromatography and refractive index gradient detection of low-nanogram and low-ppm quantities of carbohydrates

A refractive index gradient detector is presented as a universal detector in the microbore high-performance liquid chromatography analysis of carbohydrates. Simultaneously, low-ng and low-ppm injected quantities of carbohydrates were detected at the 3 x root-mean-square baseline noise level. A typical microbore high-performance liquid chromatography chromatogram separating fructose from sucrose followed by refractive index gradient (RIG) detection is reported. Use of a position sensitive detector (PSD) in the RIG detector design is reported and experimental considerations discussed. Optimization of the PSD-based RIG detector is addressed. Potential for the device in industrial and clinical applications is considered.     

石墨炔修饰的ZnO薄膜紫外探测器

制备了石墨炔修饰的金属-半导体-金属结构的ZnO紫外探测器,研究了不同旋涂次数的石墨炔修饰对探测器性能的影响。实验结果表明,石墨炔修饰的探测器比未修饰器件的光电流提高4倍,暗电流降低2个数量级,同时探测器的响应度和探测率也明显提高,其中旋涂2次的石墨炔修饰的器件特性为最优。在10 V偏压下,旋涂2次的石墨炔修饰的探测器响应度高达1759 A·W⁻¹,探测率高达4.23× 10¹⁵ Jones,这是迄今为止报导过的溶胶-凝胶法制备的ZnO紫外探测器的最高值。经过对探测器各项性能的测试分析可知,石墨炔修饰的ZnO探测器性能的提高归因于石墨炔良好的空穴传输特性。暗环境下ZnO与石墨炔界面处形成p-n结,使探测器的暗电流大幅降低;光照条件下光生空穴在石墨炔中聚集,减少了电子空穴对的复合,有效提高了器件的光电流。由于石墨炔修饰减少了ZnO表面的氧分子吸附和解吸附过程,器件的响应速度也明显加快。