کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
5407326 | 1393212 | 2007 | 7 صفحه PDF | دانلود رایگان |
عنوان انگلیسی مقاله ISI
Precision and sensitivity optimization of quantitative measurements in solid state NMR
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موضوعات مرتبط
مهندسی و علوم پایه
شیمی
شیمی تئوریک و عملی
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چکیده انگلیسی
This work presents a methodology for optimizing the precision, accuracy and sensitivity of quantitative solid state NMR measurements based on the external reference method. It is shown that the sample must be exclusively located within and completely span the coil region where the NMR response is directly proportional to the sample amount. We describe two methods to determine this “quantitative” coil volume, based on whether the probe is equipped or not with a gradient coil. In addition, to improve the sensitivity and the accuracy, an optimum rotor packing design is described, which allows the sample volume of the rotor to be matched to the quantitative coil volume. Experiments conducted on adamantane and NaCl, which are representative of a soft and hard material, respectively, show that one order of magnitude increase in experimental precision can be achieved with this methodology. Interestingly, the precision can be further improved by using the ERETIC⢠method in order to compensate for most instrumental instabilities.
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Magnetic Resonance - Volume 188, Issue 2, October 2007, Pages 260-266
Journal: Journal of Magnetic Resonance - Volume 188, Issue 2, October 2007, Pages 260-266
نویسندگان
Fabio Ziarelli, Stéphane Viel, Stéphanie Sanchez, David Cross, Stefano Caldarelli,