使用光纤探针的红外光谱监测反应-JASCO

通过使用FTIR监测反应过程，广泛分析了化合物的反应机理和动力学特性。反应过程的监测已应用于有机合成、酶反应和电化学的研究以及反应器中的原位测量；通过将纤维探针装配到反应系统中。带有光纤接口的VIR-100/200/300系列光谱仪可以控制多达6根独立的光纤（使用软件控制），从而允许使用单个FTIR监测多个反应器。此外，由于VIR-200/300光谱仪提供快速扫描测量（最长间隔25毫秒），它们可以实时监测相对快速的化学反应，如酶。光纤探头可以根据用途从透射、反射或ATR中选择。在本申请说明中，使用快速扫描测量了油和应用于ATR棱镜表面的表面活性剂之间的反应过程。实验：将食用油施加到ATR棱镜的表面，放入含有表面活性剂的搅拌小瓶中，并使用快速扫描监测反应过程。结论：在本报告中，使用具有快速扫描的ATR纤维探针监测双相反应。VIR系列可用于广泛的领域，包括需要使用套箱的领域，如锂离子电池材料的评估、使用多探针的远程测量反应器以及工艺和制造中的测量，充分利用了紧凑的尺寸、坚固性和高度可配置的样品室等特点。Application Note050-AT-0223-E Monitoring of Reaction Processusing a Fiber Probe2/3Application Note Monitoring of Reaction Process using a Fiber Probe Introduct i on The reac ti o n mechanism a n d dynam i c c h a r acter i st i cs of chemical compounds h a ve b ee n widely a n a l yzed by monitoring the r eac ti on process using F T IR. Moni t oring of the r eact i on process ha s been appl i ed to r e s e arc h i n organic synt h esis， enzymatic reactio n s a n d electrochemistry as we l l as in-situ meas u rement in reactors； by fi t ting a fiber probe into the reaction system. The VIR-100/200/300s eri e s spec t rom e t e r s wit h a fi be r interfac e c a n control u p to 6 FT/IR-4000 and 6000 Series Spect r o m eters separate f i bers (wit h softwa r e co n trol)， allowing the monitoring of multip l e r eactors using a single F T I R. Moreover， si n ce the VIR-200/300 spectrometers offer ra p id scan measuremen t (a t up to 25msec i ntervals)， th e y ca n m onitor i n real -t ime relatively fast chem i cal r eac ti ons such a s f or enzymes. A f ibe r p robe ca n be selected f r om transm i ssio n ， r ef l ectance or ATR according to the purpose. In t hi s application note， the r eact i on process b etween oi l and a s u rfacta n t a p pli e d to the surface of an ATR prism was mea s ured us in g rapid scan. Measurement Conditions Instrument VIR-200 Detector Mid-band MCT Accessory Fiber connection unit Resolution 4cm1 Fiber Probe Chalcogenide (Remspec) Interferometer Drive System Rapid scan Measurement Method ATR (ZnSe prism) Measurement Interval 80 msec Light Source High-intensity ceramic source Max. Measurement Time 80 sec Beam Splitter KBr/Ge Figure 1. VI R -200+ F i b e r con n ec ti o n u ni t Experime n tal Figure 1 shows the configu r a ti on of the system used i n t h is measurement . Since ATR analyzes the interface between the ATR p r i sm a nd a solut i on ， th e me a s u re m ent c a n be made e a sily b y put t ing th e tip o f t h e ATR pri s m i nto t h e sol u tio n without any adjustmen t of opt i cal pathlength which is usually r equired for t ransmission measurement. A cha l cogenide ATR f i b er (ma n ufactured b y Remspec) wi th Z n Se prism was used. Cooki n g oil was applied to t h e surface of the ATR pr i s m ，pl a ced in to a st i rred vial containing sur f actant and the react i on process wa s monitored u si n g rapid scan. Results and Discussion Figure 2 cha n ge in spectra wi th time as 3D data . In this meas u rement， t h e ATR pr i sm was placed into t h e sur f actant solution 25 seco n ds after t h e start of t h e measuremen t . A dec r ease in i ntensity of the -CH peak (at 2925 cm') att r ibu t ed to oil a nd an increase in intensity of t h e -OH peak (at 1639 c m l ) attribu t ed to the sur f a ctant were observed as t ime elapsed. Figu r e 3 spectrum (for surfactant and oil) after the reaction between the oil and surfactant at the su r face of the ATR prism and a spectrum (sur f actant only) m e asu r ed on the ATR p ri s m wit h ou t oil. As s h own i n th e r esults (pink area)in Fig ur e 3， it can be seen that t he peak shape of the sur f ac t an t spectrum only was b r oader when compared with the spectrum of surfactant and oil. T hi s i s co n sidered to be due to t he ordered structure of surfactant form i ng micel l s by the i n te r ac ti on of hydrop h o b ic groups betwe e n the surfact a nt and oil ， and t h e disorder e d struc t ure of the surfa c ta nt whe n oil i s not prese n t. Figure 2. 3D sp e ct r u m o f re a c t i o n p roc e ss Figure 3. S pect r um of s u rf actan t after m easu rem en t a n d s p ectr u m of sur f ac t ant o nly F i gure 4 time-dependent c h a n ge in the -CH peak a n d -OH peak. I t was fou n d t h at the intensity of the -CH peak slowly an d gradual l y dec re as e d afte r in c r e as e d r apidly wh en t he ATR pr i sm t ouched th e surf a ctant. Conv e rs e ly， t he int e ns i ty of the -OH peak rapidly increased after about 25 seconds from th e sta r t of t h e measurement and the n slowly increased .This phenomenon indicates that the solubil i zat i on (emulsification) and dispe r sion was occurring i n two steps at the surface of the ATR prism. This high -speed reac t ion process was s u ccessfu l ly observed u sing rapid -scan. It is also ex p ected t hat the molec u la r behavior at a solid-liquid i n terface as well as t h e monitoring of ordinary chem i cal react i ons can be analyzed u sing t his system. T h i s syst e m ca n also be appl ie d to t he r e s e arc h of li p osomes and t he i r us e i n d r ug d eli very syste m s (DDS)， as wel l as the b asic study of surfactants and emulsions. Fig. 4 Time-dependent change of Oil(-CH) &H2O(-OH) group) Figure 4. Time-d epen d en t cha n g e of Oil(-CH ) & H，O(-OH ) grou p) Co n c l u s io n In th is r epor t， a b i-phasic reaction was moni t ored using an ATR f i ber probe with rapid-scan. The VIR Ser i es can be uti li zed i n a wide range of f ie l ds in c lu d i ng those t h a t require the use of a glove b ox， suc h as the eval u at i on of l i t h ium-i on battery mater i a l s， r emote measureme n t reactors using multi-probes and measurement i n process and manu f actu r ing， making ful l use of t he f eat u res such a s compact si z e， ro b ustn e ss and highly conf i gurable sample compartme n t .