氦气分析用杂质成分气体标准物质研制

采用称量法研制了氦气中微量氖、氢、氧、氮、甲烷、二氧化碳和一氧化碳7种杂质成分气体标准物质,介绍了称量法制备技术、稀释气中相关杂质的定量等过程,并分别用F检验和回归曲线法对研制的气体标准物质进行了均匀性和稳定性检验。结果表明,研制的氦气分析用杂质成分气体标准物质具有良好的均匀性和稳定性,气体标准物质定值结果为10μmol/mol,定值结果的相对扩展不确定度为1%(k=2)。     

超纯气体中微量水的气相色谱分析

超纯气体制备和用超纯气体做保护气的许多工业部门,对气体中微量水是需要经常分析的。目前常用的大都是露点法,其缺点是仪器只能专用;而用高灵敏度热导检测器气相色谱仪,不但可方便地测出超纯气体中的微量水,而且还可以测定超纯气体中的微量气体杂质及作其它有机物分析之用。气相色谱仪操作简单,定量也较方便准确。     

气相色谱法分析超高纯六氟化钨中杂质气体

采用气相色谱-放电离子化检测器分析超高纯六氟化钨中微量杂质气体的含量。自行设计了一套反吹双通路分析系统,当六氟化钨中的气相杂质进入检测器后,将六氟化钨及时反吹出去,避免六氟化钨对仪器的腐蚀。通过正交试验确定了气相色谱仪的最佳工作参数,确定了采用不同的色谱柱进行分析时,仪器的最佳反吹时间。据此提出了气相色谱法分析六氟化钨中的四氟化碳、二氧化碳、六氟化硫、氧气、氮气和一氧化碳等痕量杂质气体。     

静态箱法气相色谱法自动检测农田N2O排放

Ｎ２Ｏ自动观测系统由微机控制电路和气路，使采样箱、气相色谱仪（ＧＣ）和积分仪自动工作，系统可连续采样分析，自动存储色谱数据，并可同时测定存储温度和辐射等气象数据，系统从放置于田间可自动开关箱盖的采样箱中，依次抽取空气样品，经除水、ＣＯ２处理后送入气相色谱仪分析Ｎ２Ｏ浓度，箱中浓度随时间的变化计算Ｎ２Ｏ的排放通量。     

烷类特种气体分析装置的研制及其应用

研制烷类特种气体分析专用的多维气相色谱仪，特制的热导检测器，具有手动－自动功能。设计了输气－配气装置和多维气相色谱流程。以微机控制，可按编辑程序清洗系统。检查本底，自动进样，显示或打印谱图和分析结果。可检测多种烷类特种气体组份及其中氧，氮，一氧化碳和甲烷等痕量杂质。     

氩气回路中甲烷和二氧化碳杂质的分析方法研究

本文1：1地模拟了正在建造的中国实验快中子反应堆的气体回路，建立了一个工程上可行的、50m长的、有多条固定管线和阀门的快堆覆盖气体放射性氩气取样系统、计算机控制的阀门进样以及氩气中杂质CH4和CO2的间断性在线分析方法。通过热导检测器出口气体可以排放入通风系统的办法，避免了使用氢火焰离子化检测器以后，放射性气体氩气扩散排放到气体分析实验室产生工作环境的放射性污染问题。其检出限、测量精度和准确度满足了中国实验快堆规定的氩气中杂质CH4和CO2的分析要求。并达到了美国试验和材料协会（ASTM）在快堆覆盖气体杂质的标准中提出的分析氩气中杂质CH4和CO2的标准。     

放电离子化气相色谱仪在高纯度氢分析中的应用

论述放电离子化（DID）检测器气相色谱仪的工作原理．通过高纯氢中杂质分析,从检测限、重复性、再现性以及线性范围4个方面阐述了放电离子化气相色谱仪在高纯度氢检测分析中的应用．     

变压器油中溶解气体分析专用气相色谱仪的检定与校准

为解决检定变压器油中溶解气体分析专用气相色谱仪时遇到样品进样量计算不准,检测器对甲烷气体标准物质无响应,专用软件分析方法不能更改等问题,建立变压器油中溶解气体分析专用气相色谱仪的检定与校准方法。当进样模式为一次进样双柱分流时,按分流比计算分流到检测器的样品体积,其它进样模式按进样体积计算进样量;因色谱软件禁止积分导致CH_4在热导检测器上无响应时,应采用有证标准物质中的H_2或O_2进行检定与校准。以7890B型专用气相色谱仪为例,详细说明了变压器油中溶解气体分析专用气相色谱仪的检定与校准流程。该法为检定人员检定该类专用仪器时提供了参考。     

丙烯酰胺气相色谱分析

丙烯酰胺是聚丙烯酰胺的单体,共中杂质对聚合有很大影响。主要杂质有甲醇、丙烯腈、丙烯酸和β-羟基丙腈等。我们采用两根柱子对同一样品做两次分析而得到全分析结果。 (一)仪器与试剂仪器:上海分析仪器厂100型气相色谱仪、氢火焰离子化检测器。试剂:乙腈、丙烯醛、甲醇、丙烯腈均为分析纯又经一次蒸馏。乙醛30.8％,丙烯酸98.7％,β-羟基丙腈86.7％。     

气相色谱仪检定结果的不确定度评定

气相色谱仪检定结果的不确定度主要来源于流速稳定性、柱箱温度稳定性、基线噪声、定量重复性和标准物质进样量的不确定度。以TCD检测器为例进行分析,对气相色谱仪检定结果的不确定度进行评定,相对扩展不确定度为5%。     

Membrane Microreactors for the On-Demand Generation,Separation, and Reaction of Gases

The use of gases as reagents in organic synthesis can be very challenging, particularly at a laboratory scale. This Concept takes into account recent studies to make the case that gases can indeed be efficiently and safely formed from relatively inexpensive commercially available reagents for use in a wide range of organic transformations. In particular, we argue that the exploitation of continuous flow membrane reactors enables the effective separation of the chemistry necessary for gas formation from the chemistry for gas consumption, with these two stages often containing incompatible chemistry. The approach outlined eliminates the need to store and transport excessive amounts of potentially toxic, reactive or explosive gases. The on-demand generation, separation and reaction of a number of gases, including carbon monoxide, diazomethane, trifluoromethyl diazomethane, hydrogen cyanide, ammonia and formaldehyde, is discussed.     

Application of the headspace analysis to systems with unknown partition coefficients

Summary Possibilities for the quantitative determination of volatile constituents in solutions by headspace analysis are investigated in cases where the partition coefficients (K) depend on the composition of the object under study. The timeconsuming work of revealing and taking into account the effect of the analytes and the other present constituents on the magnitude of K can be eliminated if simultaneously with determining the analyte content in the equilibrium gas one also measures the partition coefficients characteristic for the solution under study. These quantities can be obtained by repeated analysis of the equilibrium gas after partial removal of the volatile solution constituents. At small K (0.1 to 10) the required change of analyte concentration in the solution can be attained by single replacement of the equilibrium gas by pure gas, and at large K, by passing a known volume of pure gas through the solution under study under equilibrium conditions. The paper establishes the range of applicability of each version, provides the necessary equations and presents the results of an experimental check in the case of determining alcohol admixtures in water solutions.     

气相色谱法与化学法测定混合烷基铝中烷基置换反应的总速率

研究乙烯对混合烷基铝（C2-26)中烷基的置换反应的分析方法,采用水解反应产物,准确测量产生气体的体积,用气相色谱法分析其中乙烷的含量,用化学法测定水解水相中的铝含量,计算出置换反应的转化率为82．89％,反应速率为0．4502mol(C2H3)/mol(Al)/sec。建立的方法简便,快速,精密度良好,可应用于其他有机铝化合物的置换反应。     

空心活性碳纤维SNACF的碳化-活化机理的研究

本工作借助红外光谱、元素分析、比表面积测定等技术研究了空心活性碳纤维SNACF的碳化-活化机理。发现它与制备NACF的过程有明显不同:碳化过程中有硫氰酸气体释出,有带磺酸基的焦油状物排出,同时,含氮气体(HCN、NH_3)的释出量减少且释出温度提高;活化过程中可以获得更大的比表面积且活化时间可缩短。这与其原料的织构特征及化学成分有密切关系。     

Power‐to‐Gas

The power‐to‐gas concept is a promising technology to chemically store energy and therefore a feasible approach to mitigate the challenges of energy transition. Heterogeneous catalysis plays a crucial role in CO₂ conversion to methane using nickel based catalysts. A thorough catalyst characterization facilitates the synthesis of optimized catalyst systems. The determination of reaction kinetics is fundamental for industrial reactor design.     

The semantic smart laboratory: a system for supporting the chemical eScientist

One goal of eScience is to enable the end-to-end publication of experiments and results. In the Combechem project we have developed an innovative human-centred system which captures the process of a chemistry experiment from plan to execution. The system comprises an electronic lab book replacement, which has been successfully trialled in a synthetic organic chemistry laboratory, and a flexible back-end storage system. Working closely with the users, we found that a light touch and a high degree of flexibility was required in the user interface. In this paper, we concentrate on the representation and storage of human-scale experiment metadata, introducing an ontology to describe the record of an experiment, and a storage system for the data from our lab book software. Just as the interfaces need to be flexible to cope with whatever a chemist wishes to record, so the back end solutions need to be similarly flexible to store any metadata that may be created. The storage system is based on Semantic Web technologies, such as RDF, and Web Services. It gives a much higher degree of flexibility to the type of metadata it can store, compared to the use of rigid relational databases.     

The route to a feasible hydrogen-storage material: MOFs versus ammonia borane

The replacement of fossil fuels is one of the greatest challenges that chemistry and material sciences will have to face in the near future. While hydrogen seems to be the most likely candidate for this, a material able to store the hydrogen itself is sorely needed. Intense research in the past decade has narrowed down the field of possible concepts to two materials: ammonia borane with chemically bound hydrogen atoms and metal-organic frameworks with physisorbed hydrogen molecules. Herein we want to give an overview of the strengths and weaknesses of each concept, discuss the challenges that need to be overcome, and try to compare the future capabilities of these two materials.     

Energy-efficient methods for production methane from natural gas hydrates

Gas hydrates now are expected to be one of the most important future unconventional energy resources. In this paper, researches on gas hydrate exploitation in laboratory and field were reviewed and discussed from the aspects of energy efficiency. Different exploiting methods and different types of hydrate reservoir were selected to study their effects on energy efficiencies. Both laboratory studies and field tests have shown that the improved technologies can help to increase efficiency for gas hydrate exploitation. And it also showed the trend that gas hydrate exploitation started to change from permafrost to marine. Energy efficiency ratio(EER) and energy return on energy invested(EROI) were introduced as an indicator of efficiency for natural gas hydrate exploitation. An energy-efficient hydrate production process, called "Hydrate Chain Energy System(HCES)", including treatment of flue gas, replacement of CH4 with CO2, separation of CO2 from CH4, and storage and transportation of CH4 in hydrate form, was proposed for future natural gas hydrate exploitation.In the meanwhile, some problems, such as mechanism of CO2 replacement, mechanism of CO2 separation,CH4 storage and transportation are also needed to be solved for increasing the energy efficiency of gas hydrate exploitation.     

氮中低含量一氧化碳气体标准物质的定值方法

介绍氮中低含量CO气体标准物质定值的方法，对气体滤光相关分析法进行了探讨，给出了该方法的实验务件和精密度。将气体滤光相关分析法的测量值与重量法配制值、气相色谱法分析值进行了比对。气体滤光相关分析法重现性好，分析结果准确、可靠，     

分子结构对聚酰亚胺膜分离CO_2/CH_4性能的影响

气体在致密高分子膜中的渗透过程与高分子的链段活动性和自由体积有关,高分子的链段活动性越大,气体的扩散越容易,气体的透过速度越快,高分子自由体积增大,气体的溶解系数增大,扩散速率加快,透气速率上升．因此,为了得到高选择性和高透气性的分离膜,可对其化学结...