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s e m1成像-加利福尼亚大学riverside（ s e m1 imaging- universityof california, riverside）.doc

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Infrared Characterization System #2: Transmission IR Catalysis Micro-Batch Reactor (Hector) Manual Francisco Zaera Group prepared by Ilkeun Lee September 2014 Table of Contents 1. General Considerations/Overview of Equipment 4 2. FT-IR Instrument and General Operation 5 a. Spectrometer General Description 5 b. FTIR Performance Characterization 5 i. Measuring Spectral Signal-to-Noise 5 ii. Maximizing Absorbance Signal 5 c. Main FTIR Parameters 5 d. Detector 6 i. Types 6 ii. Substitution 7 iii. Preparation 7 iv. Maintenance 7 e. Optical Alignment 9 f. Transmittance spectra 9 i. Choice of Background Spectra 9 g. OPUS Software 9 i. Spectra Acquisition 9 ii. Data Processing 11 h. Maintenance 12 i. IR Source 12 ii. HeNe Laser 14 iii. Gas Purging 16 3. Gas Handling System (need update) 17 a. Design 17 b. General Operation Procedure 18 c. Gas and Liquid Sample Handling 18 d. Maintenance 18 e. Valves 19 f. Pressure Gauges 19 g. Mechanical Pumps 19 4. Transmission IR Cell 20 a. General Description 20 b. Initial Setup 20 i. NaCl Window Assembly 20 ii. Purge Installation 21 iii. Thermocouple 21 c. Alignment 21 i. Alignment 21 d. Sample Preparation, Mounting, and Processing 21 i. Sample Preparation and Loading 21 ii. Sample Heating 22 iii. Sample Pretreatment 22 iv. Collecting Background Spectra 23 v. Sample Spectrum 23 e. Maintenance 24 i. Leak Checking 24 ii. Replacing the O-ring 24 iii. Cleaning and Replacing NaCl Windows 25 iv. Cleaning the Transmission IR Cell 25 v. Heating and Temperature Measurement 25 5. Typical Experiment Sequence 25 a. Initial Steps 25 b. Sample Loading 25 c. Optimization of IR Cell Position 26 d. Background Spectra Acquisition 26 e. Adsorbate Gases Introduction 26 f. Sample Spectra Acquisition 27 g. Final Steps 27 6. Suggested Training for Beginner 27 7. Reference Materials Contacts 28 a. Reference Materials 28 b. Contacts 28 1. General Considerations/Overview of Equipment Please read this manual carefully befo