新一代多道X射线荧光分析仪的研制

介绍的新一代 2 0 4 8道X射线荧光 (XRF)分析仪是以Amptek公司研发的Si PIN电致冷半导体探测器为X射线探测器 ,以放射性同位素源为X射线荧光激发源 ;采用 16位高速ADC以及最新推出的EZ USB系列控制器来架构多道脉冲幅度分析器 ;主机采用超薄型简化配置的笔记本计算机 .在野外或室内无液氮冷却的条件下都能够实现对矿物等待测样品的测定 ,且一次可以对十余种元素进行定性、定量分析。其检出限能够达到 1～ 2× 10 -4,分析精度可达 2 %～ 8% .     

光纤氧传感器的研制及对溶解氧的测定

１　引　言 基于荧光熄灭的光纤氧传感器在环保、工业、医药、生化等领域有着广泛的应用前景。水中溶解氧的浓度是水质监测的一项重要指标,经典测定方法为碘量法。本文用自行合成的荧光试剂研制了光纤氧传感器,考察了增塑剂对膜响应特性的影响以及传感器的工作条件和干扰情况,同时对不同样品的溶解氧进行了测定,并与碘量法的测定结果进行了对比,经配对ｔ检验,结果无显著性差异。２　实验与结果２．１仪器和试剂　ＲＦ－５０００荧光分光光度计（日本岛津公司）,双臂石英光纤束（北京玻璃研究院加工）,ＬＭ－１型测氧仪（中国科学院…     

新型有机荧光探针分子的设计合成及在生物医学中的应用

近年来,荧光化学传感器以其高选择性、高灵敏度、实时原位监测、简便快捷等优点,受到人们的普遍欢迎.开发一些具有高灵敏度、高选择性、实时原位检测性能的荧光化学传感器,特别是开发一些具有实际应用价值的荧光化学传感器,一直都是人们追求的目标.论文根据分子识别和光化学传感的基本原理,结合生物医学检测的需要,设计了几种能够在水相中识别生物医学上重要生物活性分子的荧光探针分子.主要工作和结果概述如下.     

便携式智能多道石英晶体微天平的研制与应用

研制出一种能够用于气相和液相检测的便携式智能型多道石英晶体微天平。对其硬件结构、功能和模块化程序设计思想进行了讨论 ,并且给出了部分应用实验结果。本仪器具有精度高、稳定性好和性能、价格比较优越等优点。传感器阵列中的道数可以在 1～ 4之间进行选择。它为混合物测定和物质反应动力学的研究提供了有力的测试手段     

阳离子皮革加脂剂的研制及应用进展

本文综述了皮革化工材料中阳离子皮革加脂剂的研制及应用现状和最新进展,并预测了其今后的发展趋势。     

毛细管电泳多道电化学检测器的研制及其应用

报道了毛细管电泳多道电化学检测器的研制及其应用，安培检测器和电导检测器并联在同一毛细管电泳检测系统中，在同一缓冲体系，同一工作电极下对同一复杂的分析体系同时进行电导和安培检测；整个装置综合了电导检测和安培检测两种检测器的优点，性能优良，造价低廉，对实际样品的检测取得了令人满意的结果。     

氧—火焰离子化检测器的研制及应用

本文介绍选择测定复杂有机混合物中各含氧化合物的氧－火焰离子化（Ｏ－ＦＩＤ）检测器，该仪器是专门对氧响应的Ｏ－ＦＩＤ检测器，还报道了在Ｏ－ＦＩＤ检测器上对含氧化合物的定量校正工作。     

手持式智能光度计的研制及应用

本文研制了手持式智能光度计。该仪器集成了光源、进样系统和检测器,体积小巧,采用吸入式进样系统取代比色皿设计,试剂消耗量仅为比色皿的10%。使用该仪器进行了甲醛标准样品测定,标准曲线回归系数为0.9979,相对标准偏差1.02%(n=5)。用于水发牛百叶等三种水发产品中甲醛含量的测定,结果令人满意。     

磁性荧光多功能纳米探针的研制及分析应用

磁性荧光多功能纳米探针由于具有磁性分离、靶向识别、荧光成像及磁共振成像等优势,受到化学、生物及医学等领域研究者的高度关注。本文就近年来磁性荧光多功能纳米探针的研究进展作简要评述。引用文献38篇。     

氧分压对固体氧化物电解池性能的影响

High-temperature (700–900 ℃) steam electrolysis based on solid oxide electrolysis cells (SOECs) is valuable as an efficient and clean path for large-scale hydrogen production with nearly zero carbon emissions, compared with the traditional paths of steam methane reforming or coal gasification. The operation parameters, in particular the feeding gas composition and pressure, significantly affect the performance of the electrolysis cell. In this study, a computational fluid dynamics model of an SOEC is built to predict the electrochemical performance of the cell with different sweep gases on the oxygen electrode. Sweep gases with different oxygen partial pressures between 1.01 × 10³ and 1.0 × 10⁵ Pa are fed to the oxygen electrode of the cell, and the influence of the oxygen partial pressure on the chemical equilibrium and kinetic reactions of the SOECs is analyzed. It is shown that the rate of increase of the reversible potential is inversely proportional to the oxygen partial pressure. Regarding the overpotentials caused by the ohmic, activation, and concentration polarization, the results vary with the reversible potential. The Ohmic overpotential is constant under different operating conditions. The activation and concentration overpotentials at the hydrogen electrode are also steady over the entire oxygen partial pressure range. The oxygen partial pressure has the largest effect on the activation and concentration overpotentials on the oxygen electrode side, both of which decrease sharply with increasing oxygen partial pressure. Owing to the combined effects of the reversible potential and polarization overpotentials, the total electrolysis voltage is nonlinear. At low current density, the electrolysis cell shows better performance at low oxygen partial pressure, whereas the performance improves with increasing oxygen partial pressure at high current density. Thus, at low current density, the best sweep gas should be an oxygen-deficient gas such as nitrogen, CO₂, or steam. Steam is the most promising because it is easy to separate the steam from the by-product oxygen in the tail gas, provided that the oxygen electrode is humidity-tolerant. However, at high current density, it is best to use pure oxygen as the sweep gas to reduce the electric energy consumption in the steam electrolysis process. The effects of the oxygen partial pressure on the power density and coefficient of performance of the SOEC are also discussed. At low current density, the electrical power demand is constant, and the efficiency decreases with growing oxygen partial pressure, whereas at high current density, the electrical power demand drops, and the efficiency increases.     

La2Mo2O9在低氧分压条件下的电导率及热膨胀测试

The electrical conductivity and thermal expansion of La2Mo2O9 under low oxygen partial pressure were studied with the help of thermoelectric power and dilatometric measurements, respectively. The ionic conduction of La2Mo2O9 was predominant with the electronic transference number less than 0.05 above an oxygen partial pressure of about Po2=10^-7 Pa at 700℃, and below this pressure the electronic conduction became obvious. The defect reaction and small polaron hopping among molybdenum sites were proposed to explain the electronic conduction. Accompanying the phase transition, there was a sharp increase of thermal expansion, which became more serious under low oxygen partial pressure. The substitution of lanthanum by neodymium led to the increase of electrical conductivity but the decrease of phase stability.     

低氧分压区域熔炼NdBaCuO超导体

NdBaCuO在低氧分压下(1%O2+99%Ar)进行区域熔炼,区域熔炼温度明显降低,从而减少了液相(BaCuO2和CuO)在区域熔炼过程的损失。区域熔炼后NdBaCuO超导体中的非超导相Nd422含量明显降低,同时也降低了Nd对Ba的取代。在低氧分压下区域熔炼制备的Nd1+xBa2-xCu3Oy的超导电性得到明显改善。比较了区域熔炼Nd1+xBa2-xCu3Oy样品在不同温度下吸氧热处理的实验结果,得出350℃是最佳吸氧温度;用XRD分析了区域熔炼Nd1+xBa2-xCu3Oy样品的晶体取向;用标准四引线法测量了超导转变温度(Tc)和临界电流密度(Jc),比较了空气下和(1%O2+99%Ar)低氧压下区域熔炼Nd1+xBa2-xCu3Oy样品的Nd422相含量、Tc值、Jc值,证明在(1%O2+99%Ar)低氧压下区域熔炼Nd1+xBa2-xCu3Oy样品的Nd422相含量低,Jc值显著提高,达到28000A·cm-2(0T,78K)。     

基于微生物膜反应器的在线BOD测量仪及应用

以待检测水样为微生物源及有机物源,在优化的条件下,连续流经流通式管状反应器制备得到原位培养的微生物膜反应器;以此为生物降解有机物传感器,研制在线生化需氧量( BOD)监测仪,并开展了一系列现场测试应用。结果表明,在优化条件下,微生物膜反应器的培养时间为14 h,生物降解效率为18.5%,检出限为0.5 mg/L,检测上限可达20 mg/L。在线监测仪检测标样的准确度与长期稳定性的相对误差( RE)与相对标准偏差(RSD)分别为-0.8%和±3.2%,多组水样测量值与国标法(BOD5)的平均相对误差为＋5.6%。微生物膜反应器在近3个月的测试过程中,性能稳定,准确度可靠,线性范围宽,可满足对地表水的在线监测需求。     

氧载体的氧物种直接氧化甲烷制合成气

甲烷部分氧化制合成气由于合成气中n(H2)/n(CO)接近2,可直接用于甲醇合成或烃类F-T合成等后续工业过程而在国内外受到了广泛的关注。利用氧载体的氧物种在无气相氧下直接选择氧化甲烷制合成气是天然气化工利用的新方法,本文介绍了该方法的基本原理、概念工艺和对氧载体的性能要求,对应用于该方法的铈基复合氧化物的掺杂和助剂对选择氧化甲烷性能的影响、钙钛矿氧化物氧载体的氧缺陷、氧物种迁移、结构稳定性及其氧物种氧化甲烷的性能进行了阐述和分析,提出了控制氧载体表面状态是获得高合成气选择性的关键,并对该技术今后的研究重点进行了展望。     

一种智能型阻垢剂性能快速评定装置

针对我国目前指导水处理剂阻垢性能评定的化工行业标准HG/T2160-1991——鼓泡法及其评定设备的不足,基于国外上世纪末提出的电导滴定法,研制了一种一体化智能型阻垢剂性能的快速评定装置。该装置基于微机技术应用平台,实现了水处理剂阻垢性能评定的全程自动化:建立了滴定过程中电导率——滴定液容积变化曲线突降点位置的预测算法和相应软件,奠定了阻垢效果的智能评定基础;研制了数据采样间隔自动跟踪、匹配蠕动泵转速的自动滴定装置,提高了滴定分辨率和拐点位置确定精度;自制了高灵敏度、高精密度的半导体温度传感器及其测点位置调节部件,消除了滴定过程中温度对检测评定的干扰;定量确定了测定池系统表面积垢对检测评定的影响,拟定了相应清洗程序。与现有各评定方法和设备相比,本仪器的精准度高、重复性好、评定快捷、操作简便、容重小、能耗小,能更好满足水处理剂生产企业和众多行业用户对水处理剂阻垢性能评定的需求,有望成为鼓泡法评定设备的换代产品。     

阶梯式程序升温测定硬质合金混合料中总氧量和氧分量

利用氧氮分析仪的程序升温功能,使硬质合金中吸附氧与化合态氧得到有效分开,并利用碳化钨粉作间接标样,准确测定了硬质合金混合料中总氧量和氧分量。方法操作简便、测定迅速。     

低氧亲和力血红蛋白类氧载体的制备及大鼠动脉血压响应

氧亲和力是血红蛋白氧载体非常重要的参数之一,但其高低还没有统一的认识,有一种理论认为低氧亲和力是造成高血压的原因。为了进一步研究氧亲和力与血压之间的关系,本文制备了两种低氧亲和力的血红蛋白氧载体。用高碘酸钠氧化棉子糖（高碘酸钠：棉籽糖=6：1,摩尔比）,得到氧化均一的开环棉子糖;以其作为交联剂聚合脱氧猪血红蛋白,在聚合1 h得到了低氧亲和力（P50 = 43.1 torr）主要为分子内交联的64 kDa的血红蛋白,在聚合2 4 h得到了低氧亲和力（P50 = 51.5 torr）平均分子量为600 kDa的聚合血红蛋白;分别进行大鼠50%等容量换血实验,前者显著引起血压升高而后者血压平稳,证实高血压主要和64 kDa血红蛋白有关,低氧亲和力不是造成高血压的主要原因。     

用晶格氧为氧源的甲烷部分氧化制合成气

 采用热重分析技术在甲烷气氛下考察了储氧材料Fe2O3提供晶格氧的过程，用甲烷／氧切换反应和在线质谱检测方法研究了以Fe2O3晶格氧代替气相氧用于甲烷部分氧化制合成气的可能性．结果表明，Fe2O3在甲烷气氛下的还原过程包括Fe2O3→Fe3O4和Fe3O4→FeO→Fe，甲烷被氧化为CO2和H2O．在750℃下进行的CH4／O2切换反应结果表明，首先，约25％的CH4与Fe2O3中的晶格氧反应，生成CO2和H2O，然后，生成的CO2和H2O与剩余的约75％的CH4在Ni／Al2O3催化剂上进行蒸汽重整和C\r\nO2重整，从而按燃烧－重整机理实现甲烷部分氧化制合成气．选择合适的CH4／O2切换条件，可使甲烷高转化率、高选择性地生成合成气．     

Green Synthesis of Silver Nanoparticles Using Ionic Liquid and Application for the Detection of Dissolved Oxygen

The electrochemical synthesis of silver nanoparticles (nano‐Ag) has been successfully carried out on glassy carbon electrode (GCE) and indium tin oxide electrode (ITO) using 1‐butyl‐3‐methylimidazolium tetrafluoroborate (BMT) as green electrolytes. Further the electrodeposited nano‐Ag modified ITO electrode has been examined using atomic force microscopy (AFM), and X‐ray diffraction studies (XRD). The electrodeposited Ag nanoparticles on ITO were found in the size range of 5 to 35 nm. The nano‐Ag film modified GCE was further coated with nafion (Nf) and BMT (1 : 1 ratio) mixture and found to be stable in BMT and in pH 7 phosphate buffer solution (PBS). The nano‐Ag/BMT‐Nf film modified GCE successfully applied for the oxygen reduction reaction in neutral pH (pH 7.0 PBS). The proposed film modified GCE successfully reduces the over potential and show well defined reduction peaks for the detection of dissolved oxygen using cyclic voltammetry (CV) and rotating disc voltammetry (RDE). The film also applied for the detection of dissolved oxygen using electrochemical impedance spectroscopic studies (EIS).