生物质合成气一步法合成二甲醚的在线分析系统

建立了一套由生物质合成气一步法制取二甲醚的在线分析系统.针对生物质合成气一步法合成二甲醚特征,采用两台分别装有TCD和FID检测器的色谱仪分析反应产物.利用原料气中N2作为内标物,来确定TCD上检测到的永久性气体组分浓度;通过CH4作内标物,来确定FID上检测到的有机物组分浓度.TCD和FID之间通过CH4来关联,从而确定反应产物中主要组分的浓度.该系统在压力3 MPa,温度250℃,空速(流速与催化剂体积的比值)分别为1 000、2 000、3 000 h-1的条件下用C306和HZSM-5催化剂进行评价测试,发现系统分析效果好,重复性高,并且反应前后主产物碳平衡到达90%以上.     

Online preconcentration of recombinant Arg-Gly-Asp-hirudin using dynamic pH junction for analysis in human urine samples by capillary electrophoresis-mass spectrometry

A sensitive and effort-saving method was established and validated for the quantitative determination of recombinant Arg-Gly-Asp-hirudin (rRGD-hirudin) in human urine samples. The assay was performed on a uncoated fused silica capillary of 70 cm × 50 μm I.D. and a positive voltage of 30 kV was applied. The sample was injected under pressure of 50 mbar for 300 s and the temperature of capillary was kept 25 °C. Sheath liquid consisting of 30% methanol and 70% of 0.1% formic acid aqueous solution flowing at 7 μL/min was supplied to the CE-electrospray interface. Utilizing the dynamic pH junction technique, a lower limit of quantitation of approximately 35 nM was achieved (concentration coefficiency was about 100-fold) without complex sample preprocessing procedure. CE-MS conditions and parameters were also optimized to obtain better performance. The method has been successfully applied in clinical research of rRGD-hirudin.     

Online process control of acidic texturisation baths with ion chromatography

Etching of silicon with mixtures of hydrofluoric acid and nitric acid is a widely used process in silicon solar cell fabrication. One precondition for an optimized usage of the acidic etching baths is the exact knowledge of the chemical bath composition. In this paper, we investigated a fast and online-capable method for the total analysis of all bath constituents by ion chromatography. The chromatographical system consists of a low-volume injection valve, which injects the concentrated samples directly into the KOH-based eluent. After separation and detection of nitrate and fluoride, a post-column derivatization with sodium molybdate is applied to detect the hexafluorosilicic acid, which enriches in the texturisation bath during the etching process. The results of the presented approach are discussed and compared with already published chromatographical and titration methods found in literature.     

Kinetics of Thermal Decomposition of Lithium Hexafluorophosphate

With on-line coupled thermo-gravimetric analyzer-Fourier transform infrared spectrometer technique, the thermal decomposition of lithium hexafluorophosphate (LiPF₆) and its gas evolution at inert environment (H₂O<10 ppm) were studied under both non-isothermal and isothermal conditions. The results showed that the LiPF₆ decomposition is a single-stage reaction with LiF as final residue and PF₅ as gas product. In addition, its decomposi-tion kinetics was determined as 2D phase boundary movement (cylindrical symmetry) under both non-isothermal and isothermal conditions. Furthermore, the activation energy of LiPF₆ decomposition was calculated as 104 and 92 kJ/mol for non-isothermal and isothermal con-ditions, respectively.     

《聚合物改性》课程线上教学的探索

本文分析了新冠疫情形势下《聚合物改性》课程线上教学实施的问题.依托"QQ课堂"和"超星学习通"平台,通过"在线讲授理论环节"和"居家实验"相结合的形式,开展了融"理论+实践"为一体的《聚合物改性》课程在线教学.把需要在实验室完成的实验生活化,既锻炼了学生的动手能力又能尝试自己制作的美食,既激发了学生的学习兴趣,又进行了...     

应用在线近红外光谱分析复烤前后原烟及片烟的质量特性

应用在2012年"中华"专用分拣复烤生产线中采集的7个产地的复烤前原烟和复烤后片烟的在线近红外光谱为试验资料,通过建立不同产地近红外光谱的投影分析模型,并结合方差及相关分析等,研究烟叶复烤前后的均一性及相似性等品质特征的变化,为客观的掌握烟叶原料质量及卷烟产品配方提供技术支撑。本研究结果表明,从数量庞大的在线近红外光谱中,按等间隔采样时间筛选约1万条左右用于建模分析可行,取样代表性充分;经人工分拣、打叶、复烤后的各产地烟叶近红外光谱的均一性提高幅度可达10%~35%,烟叶品质的均质化程度显著提高;同时复烤后各产地烟叶所体现的相似性关系亦发生了变化,从整体上其相似性显著降低,即由产地体现的风格品质差异显著提升,为优质卷烟的原料配方设计提供了更大空间,体现了我国烟草企业生产优质中式卷烟需要消耗大量财力、人力进行烟叶复烤加工的必要性。传统的化学分析等手段需要花费大量的时间和精力,难以对整个加工环节进行控制,近红外光谱技术以其快速、无损的优势,不仅能够实现待测样品成分含量等的实时检测与质量控制,而且应用生产过程中的大量近红外光谱,可以从多角度进行有关产品品质信息的充分挖掘,是一种在众多行业特别是农产品和食品加工行业中极具应用前景的在线分析检测技术。     

Heterogene Katalyse

A technically simple experiment in heterogeneous catalysis useful for student's lab classes is introduced. Ammonia is oxidized via air using manganese iron oxides close to 200 °C. The consumption of ammonia is detected online via an ion‐selective electrode. The determination of the reaction order and the activation energy is demonstrated based on lab course conditions.     

圆形阵列无线传感器的鸟鸣声检测方法*

针对海岛湿地自然保护区鸟类等发声动物监测困难的问题,开发了基于物联网的圆形阵列无线传感器实时在线监测系统。鉴于保护区现场环境条件的特殊性,为保障传感器系统在野外长期稳定运行,需减少无鸣声数据的传输量来减轻系统负担,该文提出了基于子带能量谱熵比的动态双门限鸟类鸣声端点检测算法,对监测数据的有效鸣声段检测后实时回传到云平台。经过仿真和野外实测数据对比了不同信噪比下的鸣声检测性能,结果表明在暴风雨、风浪等海岛自然环境噪声下,鸟鸣声端点检测算法的准确率达90%以上,基本可实现海岛环境中的有效鸣声端点检测,提升了圆形阵列无线传感器系统的可靠性。     

传声器阵列声压级在线校准*

在户外环境中对某一目标噪声源进行声压级测量时,由于单个传声器不能在多声源干扰情况下有效监测目标信号,为了有效抑制非目标信号的干扰,通常利用传声器阵列进行波束形成从而对目标信号进行增强。MEMS传声器阵列由于体积小,价格低等优点而得到广泛使用,为了解决在户外进行噪声监测时,MEMS然而MEMS传声器阵列器件的工艺误差和灵敏度退化问题会导致波束形成滤波器的性能下降存在由器件工艺误差和老化所导致的声压级测量不准确问题,从而影响声压级的测量结果。为了解决这一问题,本文介绍了一种通过比较补偿参考传声器与传声器阵列之间的测量声压级之偏差进行从而实时在线校准的方法。该方法利用TDOA多声源定位方法在时频点上对实时采集的信号对所采集的信号在时频点上挑选有效目标信号进行有效挑选,并利用参考传声器的标准频响特性去修正阵列的声压级测量误差值。为了验证方法的可行性,本文通过实验比较了不同环境噪声干扰下的测量声压级差与无干扰条件下的测量声压级差的一致性,结果证明该校准方法在具有较好高的精确性和鲁棒性,并且可推广于任意一种阵型的传声器阵列声源定位装置噪声监测装置。     

Capillary electrochromatography of three β2-agonists in human urine using a lauryl methacrylate-based monolithic column

A new method of online concentration capillary electrochromatography using a lauryl methacrylate-based monolithic column was developed for determination of three β(2)-agonists including salbutamol, procaterol, and formoterol. The separation parameters including acetonitrile concentration, running buffer pH, and concentration were evaluated. To improve the sensitivity, an online concentration method with combination of the chromatographic zone-sharpening effect and field-enhanced sample-stacking effect has been developed in which the concentration parameters including injection voltage, injection time, as well as sample matrix were systematically studied. Under the optimized conditions, baseline separation of three β(2)-agonists was achieved within 4 min. When compared to the conventional sample injection, this online concentration technique increased their corresponding sensitivities up to 45-, 36-, and 320-fold, respectively. Furthermore, good repeatability was obtained with relative standard deviations (RSDs) for migration times within 0.84% and those for peak areas less than 6.35% (n = 5) in the experiment. The proposed method was successfully applied to the determination of above-mentioned β(2)-agonists in urine sample. The recoveries of spiked urine samples were between 82.4% and 109.1% with RSDs less than 9.97%.