希瓦氏菌介导制备还原氧化石墨烯薄膜及其增强的胞外电子传递

采用单室、三电极体系,通过希瓦氏菌(Shewanella)还原氧化石墨烯(GO)膜,制备了石墨烯(rGO)薄膜,并通过X射线衍射(XRD)和拉曼光谱(Raman)等手段表征了GO还原前后的结构和性质,证明了Shewanella菌可以有效将GO膜还原为rGO.以该生物还原得到的rGO薄膜为工作电极,可以有效改善Shewanella菌的胞外电子转移(EET).与空白的氧化铟锡(ITO)电极相比,rGO电极的阳极输出电流增大了13%,电量增加90%.该Shewanella还原法是一种温和制备rGO膜的方法,制得的rGO膜改善了微生物的EET效率.     

石墨烯修饰Y型TiO2纳米管光电极制备及其对氨氮催化氧化性能

采用三步阳极氧化法和一步循环伏安电沉积法制备了还原氧化石墨烯（rGO）修饰的Y型TiO₂纳米管阵列（rGO/Y-TiO₂ NTs）电极。通过场发射电子扫描显微镜（FESEM）、能量色散X荧光光谱（EDX）、X射线衍射（XRD）、紫外可见漫反射光谱（UV-Vis）及拉曼光谱（Raman）等对电极样品进行了表征。以rGO/Y-TiO₂ NTs电极为光阳极,测试了不同循环伏安沉积圈数对电极光电流响应的影响,考察了在1.0 V偏压下电极对氨氮的光电催化氧化性能。结果表明,高度有序的Y-TiO₂ NTs为锐钛矿型,具有大的比表面积,表面修饰平滑透明rGO薄膜后可显著提高其光电催化效率,沉积圈数为30时电极在30 min内对氨氮的光电催化氧化效率为95.9%。     

溶剂热/水热法制备MnOx@rGO纳米复合材料及其氧还原催化性能

氧化还原催化剂是燃料电池和金属空气电池中影响其阴极性能的关键因素. 采用溶剂热/水热法,以氧化石墨烯（GO）,MnSO₄和KMnO₄为原料可控制备了两种锰氧化物（MnO_x）和还原氧化石墨烯（rGO）复合材料（Mn₃O₄@rGO,MnOOH@rGO）并研究了其氧还原电催化性能. 通过X射线粉末衍射（XRD）、拉曼光谱（Raman）、扫描电镜（SEM）、热重（TG）等分析测试手段表征了Mn₃O₄@rGO与MnOOH@rGO的组成结构及形貌. 结果显示,在制备过程中GO被还原为rGO,乙醇和水溶剂中分别形成Mn₃O₄纳米颗粒与MnOOH纳米棒,MnO_x均匀生长在rGO表面. 采用伏安曲线和旋转圆-环盘电极技术测试了所制备复合材料的电化学性能,并与无rGO负载的Mn₃O₄和MnOOH进行对比. 结果表明,由于MnOOH和rGO的协同作用,MnOOH@rGO在碱性体系中表现出较好的催化活性及稳定性,可作为潜在的氧还原催化剂.     

还原氧化石墨烯负载零价铁的合成及对TNT废水处理

选取比表面积大且导电性能优良的还原氧化石墨烯（rGO）作为支撑材料,负载还原性强但极易团聚的纳米零价铁（nZVI）,制得还原氧化石墨烯负载零价铁（nZVI/rGO）复合材料.通过X射线衍射（XRD）、傅里叶变换红外光谱（FTIR）、扫描电子显微镜（SEM）与X射线光电子能谱（XPS）等测试手段对零价铁的负载情况、材料表面微观形貌与反应前后nZVI/rGO材料表面铁元素的含量与组成进行表征.考察了溶液初始pH值、材料投加量和理论零价铁负载量等因素对nZVI/rGO去除2,4,6-三硝基甲苯（TNT）的影响,研究了nZVI/rGO材料去除TNT的反应机理.通过正交实验可知,nZVI/rGO对含TNT废水的处理在较宽的反应条件范围内都可达到处理要求,在理论零价铁的负载量为3.0 g/g rGO,溶液初始pH为6,材料投加量为40 g/L时效果最佳,可将废水中TNT处理到检出限0.1 mg/L以下.     

PEDOT的固相聚合法制备及其在紫外光探测器中的应用

首先以2,5-二溴-3,4-乙撑二氧噻吩（DBEDOT）为单体，通过固相聚合法在掺杂氟的二氧化锡导电玻璃（FTO）基底表面制备聚（3,4-乙撑二氧噻吩）（PEDOT）膜，然后将其与氧化锌纳米阵列（ZnO NRs）修饰的FTO组装成有机-无机异质结紫外光探测器，并研究其紫外光探测性能。采用紫外-可见分光光谱（UV-Vis）、傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）、X射线衍射光谱（XRD）等测试方法对材料进行表征。结果表明，固相聚合法制备的PEDOT能有效提升ZnO NRs基紫外光探测器的性能。器件在紫外光照射下（365 nm,0.32 mW/cm2）表现出较高响应度（15.34 mA/W）、较短响应时间（上升时间为0.159 s，下降时间为0.162 s）和较好的稳定性。     

水热法制备Fe3O4/rGO纳米复合物作为锂离子电池阳极材料

以氢氧化铁为四氧化三铁的前驱体,氧化石墨烯（GO）为还原石墨烯（rGO）的前驱体,以水合肼和二水合柠檬酸三钠为混合还原剂,采用水热法制备了还原石墨烯负载四氧化三铁纳米颗粒（Fe₃O₄/rGO）的复合材料。通过透射电子显微镜（TEM）、X-射线衍射（XRD）和热重分析（TGA）对产物的形貌、结构和组成进行了表征。以锂片为对电极进行了扣式电池的组装,通过恒电流充放电和循环伏安法对其电化学性能进行了测试。材料具有均一的形貌,rGO具有较高的还原程度且可以在充放电过程中缓冲Fe₃O₄纳米颗粒的体积变化,使得Fe₃O₄/rGO纳米复合物具有较好的电化学性能。     

微波溶剂热法制备掺氮石墨烯用于碱性氧还原反应

采用微波处理氧化石墨烯（GO）与乙二醇（EG）、乙二胺（ED）混合液的方法制备氮掺杂石墨烯（NG）,使用旋转圆盘电极对NG催化氧还原在碱性溶液中反应进行研究,并考察了不同微波辐射时间、ED与EG之比对反应性能的影响。采用X射线衍射仪（XRD）、透射电子显微镜（TEM）、拉曼光谱（Raman）和傅里叶变换红外光谱（FT-IR）研究了NG催化剂的结构与性质。相比于未掺氮的石墨烯样品,NG表现出更正的起始电位和接近四电子的转移过程。NG中掺杂氮原子的键合方式通过XPS进行表征,结果表明起始电位的高低取决于石墨氮含量。此外,所有表征结果表明总氮含量与氧还原反应性能没有直接关系。     

石墨烯修饰Y型TiO_2纳米管光电极制备及其对氨氮催化氧化性能

采用三步阳极氧化法和一步循环伏安电沉积法制备了还原氧化石墨烯(rGO)修饰的Y型TiO_2纳米管(rGO/Y-TiO_2NTs)电极。通过场发射电子扫描显微镜(FESEM)、X射线能谱(EDS)、X射线衍射(XRD)、紫外可见漫反射光谱(UV-Vis DRS)及拉曼光谱(Raman)等对电极样品进行了表征。以rGO/Y-TiO_2NTs电极为光阳极,测试了不同循环伏安沉积圈数对电极光电流响应的影响,考察了在1.0 V偏压下电极对氨氮的光电催化氧化性能。结果表明,高度有序的Y-TiO_2NTs为锐钛矿型,具有大的比表面积,表面修饰平滑透明rGO薄膜后可显著提高其光电催化效率,沉积圈数为30时电极在30 min内对氨氮的光电催化氧化效率为95.9%。     

基于中空多孔金纳米/石墨烯复合纳米材料的葡萄糖氧化酶直接电化学及其生物传感研究

采用溶液相牺牲模板法制备中空多孔金纳米粒子（HPAuNPs）,并将该材料与还原氧化石墨烯（rGO）复合,用于葡萄糖氧化酶（GOx）在玻碳电极（GCE）表面的有效固定,构建GOx/HPAuNPs/rGO/GCE传感界面。利用扫描和透射电镜、X射线光电子能谱、X射线衍射谱、红外光谱及电化学等方法对材料的形貌与结构,GOx的固定化过程,以及传感器的直接电化学和电催化性能进行表征。结果表明,HPAuNPs和rGO的协同作用能有效促进GOx与电极之间的直接电子转移（DET）。基于GOx/HPAuNPs/rGO/GCE对葡萄糖的良好电催化性能,该方法有效实现了对葡萄糖的高灵敏度检测,其电流响应的线性范围为0.05～7.0 mmol/L,检出限（S/N=3）为16μmol/L。该传感器具有良好的选择性、重现性及稳定性,对实际样品血清中血糖的测定结果令人满意,回收率为98.0%～103%,相对标准偏差不大于5.0%。     

氧化石墨烯的可控还原及结构表征

采用氧化还原法, 通过控制还原时间制备了不同还原程度的石墨烯; 用红外光谱、 紫外光谱、 拉曼光谱、 X射线衍射、 热重分析、 电导率测量等多种手段系统研究了不同还原程度石墨烯的结构与性能; 采用透射电子显微镜、 扫描电子显微镜和原子力显微镜比较了氧化石墨烯和石墨烯的形貌. 结果表明, 随着还原程度的增加, 石墨烯中含氧基团减少, 紫外吸收峰逐渐红移, D带与G带的强度比增加, 热稳定性和导电性提高. 微观结构表征说明石墨烯比氧化石墨烯片的厚度增加, 褶皱增多.     

Operating the pulsed discharged detector in both the electron-capture and photoionization modes within the same GC analysis

Summary Since the electron-capture detector (ECD) is highly selective, it is imperative to use a more universal ionization detector in conjunction with the ECD in order to detect non-capturing or weakly capturing compounds. Also in an EC study of weakly or moderately strong electron-capturing compounds, it is necessary to identify the EC peak of the compound by identifying the major component with an ionization detector. In this paper we have shown that the pulsed discharge detector can be interchanged between the EC and the helium ionization modes within 4–6 s. The application of this procedure has been illustrated with a mixture of alkane/alkene chlorocompounds. The interchange between EC and argon photoionization modes has also been investigated. The change from EC to argon photoionization also occurs in 4–6 s but the reverse process requires 9 s.     

Response of CZT drift-strip detector to X- and gamma rays

The drift-strip method for improving the energy response of a CdZnTe (CZT) detector to hard X- and gamma rays is discussed. Results for a 10×10×3 mm³ detector crystal demonstrate a remarkable improvement of the energy resolution. The full width at half maximum (FWHM) is 2.18 keV (3.6%), 2.45 keV (3.0%), 2.86 keV (0.8%) and 3.89 keV (0.6%) at 60, 80, 356 and 661 keV, respectively. The resolution is limited by electronic noise below 100 keV.     

A dual spectrophotometric/contactless conductivity detector for CE determination of incompletely separated amino acids

A new application is described of a dual photometric/contactless conductivity detector to CE determination of incompletely separated compounds. These compounds are differentiated when one of them provides signals in both the cells of the detector, whereas the other yields a signal in only one cell. The technique has been applied to determination of proline and tyrosine in a dietary supplement.     

Element Specific GC-Detection by Plasma Atomic Emission Spectroscopy—A Powerful Tool in Environmental Analysis

Abstract

A new Plasma Emission Detector (FED) to be used in gas chromatography has been developed, consisting of a capacitively coupled helium plasma operating at 200 W and 27 MHz and a poly-chromator system. Elements such as H, C, N, O, S, F, Cl, Br and I can be simultaneously detected, giving way to new possibilities of measuring organic environmental pollutants.

1. Non-separated compounds can be easily measured with the FED, as long as the compounds contain different hetero-elements.

2. The calibration for a complex system as for example the chlorinated HC's demands only for a single standard.

3. The simultaneous detection of all elements of a separated compound allows the calculation of the total molecular formula.

The detection limits for different elements lie between 50 and 200 pg/sec at a signal to noise ratio of 3 to 1.     

Capillary electrophoretic system incorporating an UV/CL dual detector

We developed a capillary electrophoretic system incorporating an ultra-violet absorption (UV)/chemiluminescence (CL) dual detector, taking advantage of the CL reaction of luminol-hydrogen peroxide and the batch-type CL detection cell. UV detection was carried out using the on-capillary method while CL detection was performed using the end-capillary method. Examination of isoluminol isothiocyanate (ILITC) as a model sample revealed two main peaks with UV detection and one main peak with CL detection. The first peak in the UV detection data corresponded to the main peak in the CL detection data. We then determined that the ILITC sample included natural ILITC as well as an impurity that had absorption behavior but did not have CL properties and labeling ability. Furthermore, the components of a mixture containing glycine, glycylglycine and glycylglycylglycine, all labeled with ILITC, were well separated and detected using the present system. The present system easily, rapidly, and simultaneously produces useful information due to the presence of both UV and CL detectors.     

液相色谱仪检测器新规程的检定方法与特定条件汇总

介绍新版本液相色谱仪检定规程(JJG 705–2014)中3种变动较大检测器的检定方法,如荧光检测器、示差折光率检测器、蒸发光散射检测器。对检定不同厂家检测器设定的特定检定条件进行了汇总。     

Si drift detector in comparison to Si(Li) detector for total reflection X-ray fluorescence analysis applications

TXRF is routinely used and suited to inspect Si wafer surfaces for possible impurities of metallic elements at the level of pg and below. Lightweight, compact sized, high-resolution Silicon drift detectors (FWHM=148 eV at 5.9 keV) electically cooled and with high throughput are ideally as the new spectrometer and for clean room application. A KETEK 5 mm² Si drift detector was compared with a NORAN 80 mm² SiLi in a previously commercially available ATOMIKA 8010 wafer analyzer. Results are presented and show that almost the same detection limits for both detector types were achieved analyzing a droplet sample containing 1 ng Ni on a Si wafer. Also, the performance to detect low Z elements like Na, excited with monochromatic Cr K radiation in a vacuum chamber was tested and detection limits of 600 pg obtained.     

High Pressure Liquid Chromatography of Selected Sulfur Compounds

Abstract

High pressure liquid chromatography was used to separate and determine quantitatively the following groups of sulfur compounds: thiols, sulfides, disulfides, sulfones, isothiocyanates, thioamides, and thioureas. Amperometric and UV detectors were compared; for thiols, thioureas, isothiocyanates, and thioamides, the former was generally more sensitive. With the exception of alkyl and cycloalkyl sulfides, the liquid chromatographic method can be used for the analysis of the investigated sulfur compounds below the ppm range. The method developed was compared to gas chromatography with flame photometric detection. The latter was found to be superior for the analysis of alkyl and cycloalkyl thiols, sulfides and disulfides of molecular weight below 200, whereas the former was more suitable for the analysis of aromatic thiols, sulfides and disulfides, as well as thioamides, isothiocyanates, and thioureas. Both methods were equivalent for the analysis of aromatic sulfones.     

Flow cell within an LED: a proposal for an optical absorption detector

Droplets formed at the tip of a tube under the same conditions possess extreme uniformity of form, volume and weight. These properties of liquid drop formation have been known for a long time and consequently many applications for the drop have been found in instrumentation and chemical analysis methods. In the present paper, we report on the analytical use of a dynamic LED-based flow-through optical absorption detector with optical path length controlled by continuous dropping of a solution. This arrangement consists of a flow cell built within a high-intensity red LED (λ _max = 630 nm). The feasibility of the detector is demonstrated by colorimetric determination of methylene blue, and ammonium by Berthelot’s reaction, in a flow-injection system. For ammonium, the reaction forms a blue dye (indophenol) with a maximum absorption at 630–650 nm. The detection limit, considered as 3 times the signal of the blank, is better than 125 μg l^-1. The small flow cell represents a good combination of optical path length, low volume and fast washout. This detector can be used advantageously in automated methods and can represent a solution to problems of optical detection involving gas bubbles and precipitation of particles in turbidimetric applications.