Quantitative Raman reaction monitoring using the solvent as internal standard
Quantitative Raman reaction monitoring using the solvent as internal standard
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DOI：
10.1021/ac0401523
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发表时间：
2005-03-01
影响因子：
7.4
通讯作者：
Westerhuis, JA
中科院分区：
文献类型：
--
作者：
Aarnoutse, PJ;Westerhuis, JA
尽管它的潜力，使用拉曼光谱的实时定量反应监测仍然是相当有限的。荧光、激光不稳定性、低强度和内滤波效应的问题往往超过窄频带、玻璃纤维的使用以及水和玻璃的低散射的优点。本文提出了一种以溶剂为内标的Heck反应的实时定量监测方法。以这种方式，所有乘法失真，例如，可以校正激光的激光强度变化或吸收率。我们还表明，有限的荧光量不会妨碍分析。最后，我们提出了一种新的方法来校正内滤波器效应，即，反应介质的拉曼散射光的吸光度。反应混合物的同时吸收测量使得能够针对内滤波器效应精确校正拉曼信号。因此，对于反应监测应用，拉曼光谱仪应配备有吸光度测量装置。
Despite its potential, the use of Raman spectroscopy for real-time quantitative reaction monitoring is still rather limited. The problems of fluorescence, laser instability, low intensities, and the inner filter effect often outscore the advantages as narrow bands, the use of glass fibers, and low scattering of water and glass. In this paper, we present real-time quantitative monitoring of the catalyzed Heck reaction by using the solvent as internal standard. In this way, all multiplicative distortions, e.g., laser intensity variations or absorbance of the laser light, can be corrected for. We also show that a limited amount of fluorescence does not hamper the analysis. Finally, we present a new method to correct for the inner filter effect, i.e., the absorbance of Raman scattered fight by the reaction medium. Simultaneous absorption measurements of the reaction mixture enable accurate correction of Raman signals for the inner filter effect. Thus, for reaction monitoring applications, a Raman spectrometer should be equipped with an absorbance measurement device.