Micro_Reaction_Sampler_E
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Leading the way in material characterization “On-line micro reaction sampler” The on-line micro reaction sampler is a device that allows a small amount of a sample and reagent to react under semisupercritical or supercritical fluid conditions in a small glass capsule (id 2 mm, length 30-35 mm), and is fitted to a MultiFunctional Pyrolyzer, then reaction products formed are analyzed online directly by GC. Features • Reactions under high pressure and high temperature in a closed system Supercritical fluid conditions Polyamides that can hardly be analyzed by normal reactive pyrolysis GC or PyGC can be analyzed by organic alkali derivatization under high pressures and high temperatures. After reaction in a sealed glass capsule, the products can be analyzed online directly by introducing them to a GC separation column without working up the reaction mixture. • High pressure reactions using a small amount of sample and reagent • Online GC analysis of reaction products Temperature and pressure isothermals with varied volumes of methanol Only a few milligrams of sample and reagent are required for the online micro reaction sampler; therefore, it is safe to handle. The figure on the right shows the calculated relationship between the pressure and temperature inside of a glass capsule, when 1, 3 and 5 µL of methanol are added to the glass capsule (volume: 76 µL). Methanol becomes a supercritical fluid above the critical temperature and critical pressure (T=239ºC, P=8.1 MPa). A supercritical fluid has unique properties and often gives quite different results from those of normal conditions. Typical applications of the micro reaction sampler Reactive pyrolysis of nylon 6.6 Reactive pyrolysis of fat (butter) Polyamide (e.g. nylon) is one of the polymers that are difficult to analyze using ordinary reactive pyrolysis GC or Py-GC. However, performing the analysis at elevated pressures significantly enhances the organic alkali hydrolysis and derivatization process. The figure below shows the chromatograms of nylon 6.6 obtained by 1) flash pyrolysis, 2) conventional reactive pyrolysis, and 3) reactive pyrolysis at elevated pressure. Only the chromatogram 3) has large peaks which are indicative of the nylon 6.6 structure. Methyl esterification of vegetable oils and animal fats which are the common sources of biodiesel fuel can be studied using the micro reaction sampler. 1) Flash pyrolysis Py: 600ºC, Eco-Cup The top chromatogram was obtained using conventional reactive pyrolysis (350ºC). The bottom chromatogram was obtained using the micro reaction sampler. While the ratios of the methyl esters of the aliphatic acids are comparable, the ratios of methylated glycerol are quite different. 1) Reactive pyrolysis in open system GC: 40→320ºC (20 ºC/min) Column: UA5-30M-0.25F Py: 350ºC, Eco-Cup Reagent: tetramethylammonium hydroxide (TMAH), 5 µL dimethyl- trimethyl- 2) Conventional reactive pyrolysis Py: 300ºC, Eco-cup Reagent: tetramethylammonium hydroxide (TMAH), 5 µL 2) Reactive pyrolysis using the micro reaction sampler 5 3) Reactive pyrolysis using the micro reaction sampler Py: 300ºC, reaction time: 1 hr Reagent: TMAH, 5 µL Py: 100ºC, reaction time: 1 hr Reagent: TMAH, 5 µL Glycerol dimethyl- Dimethyl adipate Tetramethyl hexamethylenediamine

Operating principal The operating sequence described earlier is shown below: Cross-section of the On-line micro reaction sampler On-line micro reaction sampler and glass capsule before and after crushing Rotating knob After Crushing rod Slides up and down Sampler base He Expanded view Reaction chamber Sealed glass capsule Sample and reagent sealed in glass capsule Four side-openings for flushing the reaction products. Pyrolysis tube Using on-line micro reaction sampler (1) Place sample and reagent in a glass capsule. (2) Insert the glass capsule into the capsule holder until it hits the...