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学科主题: 物理化学
题名: Long-Term Real-Time Monitoring Catalytic Synthesis of Ammonia in a Microreactor by VUV-Lamp-Based Charge-Transfer Ionization Time-of-Flight Mass Spectrometry
作者: Xie, Yuanyuan1, 2;  Hua, Lei1;  Hou, Keyong1;  Chen, Ping1, 2;  Zhao, Wuduo1, 2;  Chen, Wendong1, 2;  Ju, Bangyu1;  Li, Haiyang1
通讯作者: 李海洋
刊名: ANALYTICAL CHEMISTRY
发表日期: 2014-08-05
DOI: 10.1021/ac501576f
卷: 86, 期:15, 页:7681-7687
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology ;  Physical Sciences
类目[WOS]: Chemistry, Analytical
研究领域[WOS]: Chemistry
英文摘要: With respect to massive consumption of ammonia and rigorous industrial synthesis conditions, many studies have been devoted to investigating more environmentally benign catalysts for ammonia synthesis under moderate conditions. However, traditional methods for analysis of synthesized ammonia (e.g., off-line ion chromatography (IC) and chemical titration) suffer from poor sensitivity, low time resolution, and sample manipulations. In this work, charge-transfer ionization (CTI) with O-2(+) as the reagent ion based on a vacuum ultraviolet (VUV) lamp in a time-of-flight mass spectrometer (CTI-TOFMS) has been applied for real-time monitoring of the ammonia synthesis in a microreactor. For the necessity of long-term stable monitoring, a self-adjustment algorithm for stabilizing O-2(+) ion intensity was developed to automatically compensate the attenuation of the O-2(+) ion yield in the ion source as a result of the oxidation of the photoelectric electrode and contamination on the MgF2 window of the VUV lamp. A wide linear calibration curve in the concentration range of 0.2-1000 ppmv with a correlation coefficient (R-2) of 0.9986 was achieved, and the limit of quantification (LOQ) for NH3 was in ppbv. Microcatalytic synthesis of ammonia with three catalysts prepared by transition-metal/carbon nanotubes was tested, and the rapid changes of NH3 conversion rates with the reaction temperatures were quantitatively measured with a time resolution of 30 s. The high-time-resolution CTI-TOFMS could not only achieve the equilibrium conversion rates of NH3 rapidly but also monitor the activity variations with respect to investigated catalysts during ammonia synthesis reactions.
关键词[WOS]: SINGLE-PHOTON IONIZATION ;  ION FLOW TUBE ;  VACUUM-ULTRAVIOLET LAMP ;  TRACE GAS-ANALYSIS ;  PHOTOELECTRON IONIZATION ;  SIFT-MS ;  ONLINE ;  CARBON ;  PRESSURE ;  BREATH
语种: 英语
WOS记录号: WOS:000340081100075
Citation statistics: 
内容类型: 期刊论文
URI标识: http://cas-ir.dicp.ac.cn/handle/321008/143969
Appears in Collections:中国科学院大连化学物理研究所_期刊论文

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作者单位: 1.Chinese Acad Sci, Dalian Inst Chem Phys, Key Lab Separat Sci Analyt Chem, Dalian 116023, Peoples R China
2.Chinese Acad Sci, Grad Univ, Beijing 100039, Peoples R China

Recommended Citation:
Xie, Yuanyuan,Hua, Lei,Hou, Keyong,et al. Long-Term Real-Time Monitoring Catalytic Synthesis of Ammonia in a Microreactor by VUV-Lamp-Based Charge-Transfer Ionization Time-of-Flight Mass Spectrometry[J]. ANALYTICAL CHEMISTRY,2014,86(15):7681-7687.
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