供气相色谱仪使用的热导检测器的设计与实现

为了提高气相色谱仪用热导检测器的性能,设计了热导检测器的精密恒流源和差压检测电路。恒流源由场效应管IRF460、运算放大器AD8672和线性光耦HCNR201构成,低噪声电桥差压检测电路由2片AD8597构成。建立了差压检测电路的噪声模型,计算了噪声理论值。实际测试结果表明,该热导检测器的基线噪声达到4 μV, 50 min的基线漂移为15 μV,恒流源波动接近1 μA,优于现有热导检测器的技术指标。所介绍的设计方案和噪声分析方法对热导检测器的电路设计有较大的参考价值。     

高灵敏度热导检测器的试制

热导检测器在气相色谱中广为应用,多年来国外为了提高它的灵敏度和改善稳定性,对检测器(热丝、检测器体积和形状、内部流路的形状、精密温控、电气线路等)进行了详细的研究和改进。方波供电、铼钨丝、前置放大、气体输送调节器等方法都可以提高灵敏度。但这些都不涉及热导检测器本身结构的改进,而且均需一定的条件和专用的仪器设备,不易广泛采用。我们从改进检测器本身结构和吊丝方法出发提出了一种结构新颖、吊丝独特从而提高了灵敏度的方法。     

微型气相色谱的研究进展

具有高性能、智能化、低功耗、低物耗的分析仪器微型化研究已经是分析仪器的主要发展方向。气相色谱(GC)作为一种应用十分广泛的分离分析仪器,其微型化的研究一直受到科学界和工业界的重视。本文综述了近十几年来微型气相色谱(micro GC)的研究进展。对微型气相色谱的3个主要组成部分,即进样/富集装置、色谱柱和检测器,分别进行了详细的阐述,并简单总结了微型气相色谱的应用现状,对其发展趋势进行了展望。     

新型光离子化检测器的设计与应用

将自行研制的PID光离子化检测器安装于气相色谱仪上,无需复杂的样品前处理,便可快速分析环境中的苯系物、醛类等物质.概述了此检测器的基本原理,详细介绍了其结构、电路系统的设计及性能测试结果.采用喷嘴与电极一体化的设计理念,使电离室的体积缩小到30 μ L,灵敏度提高,同时易于加工；微电流放大器的设计选用低噪声、低温漂的精...     

745厂铼钨丝在热导检测器中的应用

热导检测器具有结构简单,操作方便,几乎对所有物质都响应等优点,到目前仍然是气相色谱中用得最多、最广泛的一种通用型浓度敏感检测器。同时,在提高检测器灵敏度、稳定性和最小检测能力方面一直为人们所关心,并不断取得改进和提高。采用先进的热敏材料来设计、制造较好的热敏元件是直接提高热导检测器性能的有效途径。 1973年起,我国曾先后向瑞典Luma公司、日本东芝公司引进了铼钨丝试用于上海分析仪器厂、北京分析仪器厂气相色谱仪中热导检测器,使原有灵敏度S值(对苯)从1000((mv·ml)/mg)左右提高到2000((mv·ml)/mg)左右。     

长链溴代氟碳烃的色-质谱分析

本文给出了50余种C_nF_mH_1Br_x的色谱相对保留时间和质谱数据。还给出了热导检测器上Br(CF_2)_nBr的峰面积的相对响应值和一些化合物的质谱总离子流大小的相对响应值。     

气相色谱结合分光光度计测定尿素醇解合成碳酸二甲酯产物

采用GDX-203色谱柱,热导检测器,异丁醇为内标,分析测定了尿素与甲醇合成碳酸二甲酯产出物中的原料甲醇(Me),产物碳酸二甲酯(DMC),氨基甲酸甲酯(MC),N-甲基氨基甲酸甲酯(NMMC)的含量.用对二甲氨基苯甲醛(PDAB)作显色剂,总吸光度差减去氨基甲酸甲酯吸光度后,测定产物中少量的尿素(Urea).分析的相对标准偏差低于3.5%,回收率在97%～103%.     

新型气相色谱检测器研制

气相色谱仪是近年来分析测试应用最广泛的仪器之一,气相色谱常用的热导检测器(TCD)应用面广,但灵敏度偏低,且热丝易于烧断,氢焰检测器(FID)灵敏度较高,却对多数无机气体无响应,且必须配备氢气源,使用中具有一定危险性,两者各有局限,为此,研究一种应用广泛,使用简便,高灵敏的气相色谱检测器,已成为广大色谱工作者长期研究的课题。本文所介绍的一种新型气相色谱检测器用催化元件配以专门设计的气路和电路组成,可与现行一些气相色谱仪匹配使用,已成功地进行了许多有机组分及无机气体的分析。1　检测原理汽化后的有机蒸汽或无机可燃气体…     

西兰花中13种有机含磷农药在不同色谱柱上的色谱保留行为

应用Agilent GC 6890气相色谱仪(附FPD检测器)对13种残留于西兰花中的有机含磷农药(OPP′s)在4种不同极性的毛细管色谱柱(即DB-1、DB-5、DB-1701及DB-35MS)上的保留行为作了研究。结果表明:采用由DB-5及DB-1701串联组成的色谱柱单元,西兰花中13种残留OPP′s可达到有效分离和测定。     

化工废水排污沟底泥中多种有机污染物的气相色谱分析

为测定某化工废水排污沟底泥中多种有机污染物,建立了气相色谱(GC)分析方法。GC测定用电子俘获检测器(ECD)及火焰电离检测器(FID)两种检测器。每种检测器测定时均用两个极性不同的色谱柱分离、定性,结果较为可靠。比较了底泥样品三种不同提取方法的效果。所提供方法操作     

气相色谱-微池电子捕获器检测尿液中的三唑仑

建立了气相色谱-微池电子捕获检测器(GC-μECD)检测尿液中三唑仑的方法。筛选了pH值、提取溶剂、涡旋时间,优化了液-液萃 取条件。在0.2～50 ng/mL范围内,线性关系良好,相关系数为0.9995;方法的检出限为0.1 ng/mL,日内和日间测定的相对标准偏差分 别为4.17%和5.31%,平均回收率为93.9%。该方法操作简便、灵敏度高、线性范围广、回收率高,完全能够满足日常检测工作的需要。     

基于微机电系统的微型气相色谱柱研究进展

气相色谱柱是气相色谱仪的关键部件,主要用于混合气体组分的分离。与传统气相色谱柱相比,基于微机电系统（MEMS）技术设计制作的微型气相色谱柱具有重量轻、体积小、功耗低、分离快速等优点,便于集成到便携式气相色谱仪中,适应了目前气相色谱仪微型化的发展趋势。该文综述了MEMS微型气相色谱柱的研究进展,首先阐述了MEMS微型气相色谱柱理论基础,随后对MEMS微型气相色谱柱沟道布局及柱内结构、固定相支撑层及固定相制备等方面进行了综述,最后对其发展趋势进行了展望。     

Study on Flow Induced Nano Structures in iPP with Different Molecular Weight and Resulting Strength Behavior

Polypropylene samples in a wide molecular weight range between approx. 100 kg/mol to 1 600 kg/mol were processed by injection molding to thin walled micro specimens with respect to study shear induced crystallization phenomena under high shear rate and subsequently possible self reinforcement effects. The specimens nano structures were investigated and related deformation behavior under tensile studied. Novel morphologies have been detect and their micromechanical mechanism interpret and summarized.     

UV and thermally stable polystyrene‐MWCNT superhydrophobic coatings

A facile method for ultraviolet (UV) and thermally stable polystyrene‐multiwalled carbon nanotubes (PS‐MWCNT) superhydrophobic coatings was demonstrated by a simple spray coating method. The superhydrophobicity was understood by an increase in micro/nano roughness with the addition of MWCNTs. Surface morphology of the coatings showed protrusion like structure. The wetting behavior of the coatings was studied as a function of temperature, and it is observed that the coatings were superhydrophobically stable up to 250 °C. A transformation of superhydrophobic to superhydrophilic state is achieved at 300 °C. The coatings remained superhydrophobically stable when it was subjected to UV‐irradiation and water immersion of 50 h. Thermogravimetric analysis showed a small shift (10°) towards higher temperature region with an addition of MWCNTs, suggesting the presence of weak interactions between PS and MWCNT, which is also supported by Fourier transform infrared spectroscopy, Raman and X‐ray photoelectron spectroscopy studies. Both hydrophilic and superhydrophobic coatings find potential applications in our daily life. Copyright © 2016 John Wiley & Sons, Ltd.     

Direct Writing of Conducting Polymers

Described herein is a new printing method—direct writing of conducting polymers (CPs)—based on pipette‐tip localized continuous electrochemical growth. A single barrel micropipette containing a metal wire (Pt) is filled with a mixture of monomer, supporting electrolyte, and an appropriate solvent. A droplet at the tip of the pipette contacts the substrate, which becomes the working electrode of a micro‐electrochemical cell confined to the tip droplet and the pipette. The metallic wire in the pipette acts as both counter and reference electrode. Electropolymerization forms the CP on the working electrode in a pattern controlled by the movement of the pipette. In this study, various width poly(pyrrole) 2D and 3D structures are extruded and characterized in terms of microcyclic voltammetry, Raman spectroscopy, and scanning electron microscopy.

     

金刚石复合界面扩散系数的电子探针研究

结合金刚石与硬质合金复合材料的研究，对含轻元素的界面扩散问题提出了能谱仪与波谱仪原位互补分析研究的方法，从扩散深度和扩散浓度分布两种角度探讨了扩散系数的电子探针测定；同时讨论了该方法在金刚石与硬质合金复合钻头上的应用。     

Pressure‐Assisted Spinning: A Versatile and Economical,Direct Fibre to Scaffold Spinning Methodology

Spinning composite polymer fibres by means of electric fields has been investigated for well over a century. These spun fibres have been explored across many areas of research, spanning the physical to the life sciences; however, electrospinning has the hazardous nature of the high voltage at the spinning needle. We demonstrate here a competing direct fibre to scaffold preparation method, completely determined by an applied pressure. Our technique reported here removes the hazardous high‐voltage element from the fibre/scaffold formation technique and has the ability to form uniaxial fibres and scaffolds comparable to those fabricated by electrospinning. We refer to this fibre generation approach as “pressure‐assisted spinning (PAS)”, which will have a tremendous impact in a range of applications, spanning the physical through to the life sciences. PAS joins the techniques for fibre to scaffold generation with a view to significantly and globally contributing to the micro‐ and nanosciences.

     

分散微固相萃取-超高效液相色谱-高分辨质谱法测定葡萄酒和啤酒中多菌灵和噻菌灵

基于强阳离子交换填料（PCX）,采用分散微固相萃取前处理技术,结合超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用技术,建立了一种快速测定葡萄酒和啤酒中多菌灵和噻菌灵的方法。通过对分散微固相萃取技术中PCX用量、洗脱溶剂中氨水的体积分数、乙腈的体积分数和洗脱体积的优化,实现了样品中多菌灵和噻菌灵的有效净化。经BEH C₁₈（50 mm×2.1 mm,1.7 μm）色谱柱分离后,通过静电场轨道阱质谱靶向单一离子监测（targeted single ion monitoring,tSIM）结合数据依赖的二级质谱扫描（data dependent tandem mass spectrometry,ddMS²）采集模式进行定性定量分析。待测物多菌灵和噻菌灵在一定浓度范围内均呈良好线性关系,相关系数R²≥0.9999。在葡萄酒和啤酒基质中,多菌灵和噻菌灵的检出限分别为0.02和0.01 μg/L,定量限分别为0.06和0.03 μg/L。在0.1、1.0、100 μg/L 3个添加水平下,多菌灵和噻菌灵的加标回收率分别为95.6%~110.2%和87.5%~102.8%,日内精密度（RSD_r）分别为1.8%~5.2%和1.3%~4.8%,日间精密度（RSD_R）分别为4.3%~8.7%和4.8%~9.4%。该方法快速、简便、灵敏,适用于葡萄酒和啤酒中多菌灵和噻菌灵的残留检测。     

Detection of ethanol in human body fluids by headspace solid-phase micro extraction (SPME)/capillary gas chromatography

Summary Ethanol has been found extractable from human whole blood and urine samples by headspace solid-phase micro extraction (SPME) with a Carbowax/divinylbenzene-coated fiber. After heating a vial containing the body fluid sample with ethanol, and isobutanol as internal standard (IS) at 70°C in the presence of (NH₄)₂SO₄, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial to allow adsorption of the compounds. The fiber needle was then injected into a middle-bore capillary gas chromatography (GC) port. The headspace SPME-GC gave intense peaks for both compounds; a small amount of background noises appeared, but did not interfere with the detection of the compounds. Recoveries of ethanol and IS were 0.049 and 0.026% for whole blood, respectively, and 0.054 and 0.085% for urine, respectively. The calibration curves for ethanol showed excellent linearity in the range of 80–5000 mg L^–1 for whole blood and 40–5000 mg L^–1 for urine; the detection limits for both samples were 20 and 10 mg L^–1, respectively. The data on actual determination of ethanol after the drinking of beer are also presented for two subjects.