Difference between revisions of "Chem341:NMR workshop"
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==Introduction== | ==Introduction== | ||
| − | Nuclear Magnetic Resonance (NMR) is a property of the nucleus of an atom, concerned with what is known as nuclear spin (I). This is equivalent to the nucleus acting like a miniature bar magnet. Although isotopes can have a variety of values for I (including zero), the most useful for spectroscopy are those nuclei which have I = 1/2 . Fortunately this includes hydrogen 1 ( | + | Nuclear Magnetic Resonance (NMR) is a property of the nucleus of an atom, concerned with what is known as nuclear spin (I). This is equivalent to the nucleus acting like a miniature bar magnet. Although isotopes can have a variety of values for I (including zero), the most useful for spectroscopy are those nuclei which have I = 1/2 . Fortunately this includes hydrogen 1 (<sup>1</sup>H), carbon 13, fluorine 19 and phosphorus 31, so that some of the commonest elements in organic chemistry can be analyzed using NMR. |
| − | When a nucleus with I = 1/2 is placed in a magnetic field, it can either align itself with the field (lower energy) or against it (higher energy). If radio waves are applied, nuclei in the lower energy state can absorb the energy and jump to the higher energy state. We can observe either the absorption of energy, or the subsequent release of energy as the nucleus "relaxes" back to the lower energy state. Traditionally this was done by scanning slowly through a range of radio wave frequencies (this is called continuous wave, CW). However this has largely been replaced by the faster Fourier Transform (FT) method where one big, broad pulse of radio waves is used to excite all nuclei, then the results are analyzed by computer. | + | When a nucleus with I = 1/2 is placed in a magnetic field, it can either align itself '''''with''''' the field (lower energy) or '''''against''''' it (higher energy). If radio waves are applied, nuclei in the lower energy state can absorb the energy and jump to the higher energy state. We can observe either the absorption of energy, or the subsequent release of energy as the nucleus "relaxes" back to the lower energy state. Traditionally this was done by scanning slowly through a range of radio wave frequencies (this is called [http://en.wikipedia.org/wiki/Nuclear_magnetic_resonance#Continuous_wave_.28CW.29_spectroscopy continuous wave], CW). However this has largely been replaced by the faster [http://en.wikipedia.org/wiki/Fourier_transform_spectroscopy Fourier Transform] (FT) method where one big, broad pulse of radio waves is used to excite all nuclei, then the results are analyzed by computer. |
| + | [[File:341nmr1a.GIF|center|Diagram showing how the nuclear spin aligns with or against the field, and absorbs/emits a photon]] | ||
==Chemical shift== | ==Chemical shift== | ||
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In a real molecule, the effective magnetic field "felt" by a particular nucleus (Beff) includes not only the applied field B0, but also the magnetic effect of nearby nuclei and electrons. This causes the signal to absorb at a slightly different frequency than for a single atom; it is convenient to reference this resonant frequency to a standard (usually [http://en.wikipedia.org/wiki/Tetramethylsilane tetramethylsilane], TMS, defined as zero). When we plot the output from this absorption, we obtain a series of peaks known as an '''NMR spectrum''' (or "spectra" if you have more than one spectrum) such as the typical example shown in Fig. 2. The difference (in parts per million, ppm) from the zero point is referred to as the '''chemical shift''' (δ). A typical range for δ is around 12 ppm for <sup>1</sup>H and around 220 ppm for <sup>13</sup>C. It is customary to have the zero point at the right hand end of the spectrum, with numbers increasing to the left ("downfield") as shown in Fig. 2. Typical chemical shift values are shown in Tables 1 & 2, and also Fig. 3. | In a real molecule, the effective magnetic field "felt" by a particular nucleus (Beff) includes not only the applied field B0, but also the magnetic effect of nearby nuclei and electrons. This causes the signal to absorb at a slightly different frequency than for a single atom; it is convenient to reference this resonant frequency to a standard (usually [http://en.wikipedia.org/wiki/Tetramethylsilane tetramethylsilane], TMS, defined as zero). When we plot the output from this absorption, we obtain a series of peaks known as an '''NMR spectrum''' (or "spectra" if you have more than one spectrum) such as the typical example shown in Fig. 2. The difference (in parts per million, ppm) from the zero point is referred to as the '''chemical shift''' (δ). A typical range for δ is around 12 ppm for <sup>1</sup>H and around 220 ppm for <sup>13</sup>C. It is customary to have the zero point at the right hand end of the spectrum, with numbers increasing to the left ("downfield") as shown in Fig. 2. Typical chemical shift values are shown in Tables 1 & 2, and also Fig. 3. | ||
| − | + | [[File:341nmr1b.GIF|thumb|center|800px|Chart of common chemical shift values ]] | |
| + | Figure 2: A typical <sup>1</sup>H spectrum and <sup>13</sup>C spectrum: | ||
| + | |||
| + | [[File:P tert butyltolueneH.gif|thumb|center|900px|<sup>1</sup>H NMR spectrum of para-(tert-butyl)toluene]] | ||
| + | |||
| + | [[File:P tert butyltolueneC.gif|thumb|center|900px|<sup>13</sup>C NMR spectrum of para-(tert-butyl)toluene]] | ||
| + | |||
| + | Exercise 1. Predict approximate chemical shifts for all the carbon and hydrogen atoms which are explicitly shown in the following molecules: | ||
[[Category:Chemistry 341]] | [[Category:Chemistry 341]] | ||
Revision as of 23:30, 16 September 2009
This is a workshop introducing the basics of NMR spectroscopy for students of organic chemistry. It is taught as part of the Chemistry 341 course at SUNY Potsdam.
Introduction
Nuclear Magnetic Resonance (NMR) is a property of the nucleus of an atom, concerned with what is known as nuclear spin (I). This is equivalent to the nucleus acting like a miniature bar magnet. Although isotopes can have a variety of values for I (including zero), the most useful for spectroscopy are those nuclei which have I = 1/2 . Fortunately this includes hydrogen 1 (1H), carbon 13, fluorine 19 and phosphorus 31, so that some of the commonest elements in organic chemistry can be analyzed using NMR.
When a nucleus with I = 1/2 is placed in a magnetic field, it can either align itself with the field (lower energy) or against it (higher energy). If radio waves are applied, nuclei in the lower energy state can absorb the energy and jump to the higher energy state. We can observe either the absorption of energy, or the subsequent release of energy as the nucleus "relaxes" back to the lower energy state. Traditionally this was done by scanning slowly through a range of radio wave frequencies (this is called continuous wave, CW). However this has largely been replaced by the faster Fourier Transform (FT) method where one big, broad pulse of radio waves is used to excite all nuclei, then the results are analyzed by computer.
Chemical shift
In a real molecule, the effective magnetic field "felt" by a particular nucleus (Beff) includes not only the applied field B0, but also the magnetic effect of nearby nuclei and electrons. This causes the signal to absorb at a slightly different frequency than for a single atom; it is convenient to reference this resonant frequency to a standard (usually tetramethylsilane, TMS, defined as zero). When we plot the output from this absorption, we obtain a series of peaks known as an NMR spectrum (or "spectra" if you have more than one spectrum) such as the typical example shown in Fig. 2. The difference (in parts per million, ppm) from the zero point is referred to as the chemical shift (δ). A typical range for δ is around 12 ppm for 1H and around 220 ppm for 13C. It is customary to have the zero point at the right hand end of the spectrum, with numbers increasing to the left ("downfield") as shown in Fig. 2. Typical chemical shift values are shown in Tables 1 & 2, and also Fig. 3.
Figure 2: A typical 1H spectrum and 13C spectrum:
Exercise 1. Predict approximate chemical shifts for all the carbon and hydrogen atoms which are explicitly shown in the following molecules:
