TY - JOUR
T1 - Off-line reaction monitoring of the oxidation of alkenes in water using drop coating deposition Raman (DCDR) spectroscopy
AU - Abdolahzadeh, Shaghayegh
AU - Boyle, Nicola M.
AU - Draksharapu, Apparao
AU - Dennis, Andrew C.
AU - Hage, Ronald
AU - De Boer, Johannes W.
AU - Browne, Wesley R.
PY - 2013/6/7
Y1 - 2013/6/7
N2 - The application of drop coating deposition Raman (DCDR) spectroscopy to the field of reaction progress monitoring is addressed in this contribution. Although, DCDR spectroscopy has seen recent application in the study of biological fluids, its application in other areas has not yet been explored. Here we apply the technique to the catalysed oxidation of alkenes to epoxides in aqueous solutions at concentrations <10 mM. The effect of surface characteristics, background interferences, homogeneity of distribution of analytes, drying time, as well as instrumental limits of detection and calibration are discussed. We demonstrate that reproducible spectra can be obtained routinely, with relatively little variance, with short acquisition times and samples volumes of 2-10 μl and as little as 1 μg of analyte. The utility of the technique compared with online reaction monitoring by 1H NMR and Raman spectroscopy is demonstrated in the excellent correlation between data obtained off and on-line.
AB - The application of drop coating deposition Raman (DCDR) spectroscopy to the field of reaction progress monitoring is addressed in this contribution. Although, DCDR spectroscopy has seen recent application in the study of biological fluids, its application in other areas has not yet been explored. Here we apply the technique to the catalysed oxidation of alkenes to epoxides in aqueous solutions at concentrations <10 mM. The effect of surface characteristics, background interferences, homogeneity of distribution of analytes, drying time, as well as instrumental limits of detection and calibration are discussed. We demonstrate that reproducible spectra can be obtained routinely, with relatively little variance, with short acquisition times and samples volumes of 2-10 μl and as little as 1 μg of analyte. The utility of the technique compared with online reaction monitoring by 1H NMR and Raman spectroscopy is demonstrated in the excellent correlation between data obtained off and on-line.
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U2 - 10.1039/c3an00330b
DO - 10.1039/c3an00330b
M3 - Article
C2 - 23589804
AN - SCOPUS:84877676980
SN - 0003-2654
VL - 138
SP - 3163
EP - 3171
JO - Analyst
JF - Analyst
IS - 11
ER -