NMR Spectroscopy Flashcards

1
Q

What does NMR stand for?

A

Nuclear Magnetic Resonance

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2
Q

Give one use of NMR?

A

MRI scans

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3
Q

What kind of nuclei does NMR work with (and examples)?

A

Those with an uneven number of nucleons, meaning they will spin e.g. 1H, 13C

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4
Q

What percentage of carbon atoms are 13C?

A

1% - but modern instruments are sensitive enough to detect this

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5
Q

What defines the resonant frequency of a 13C atom?

A

The chemical environment that it is in; the amount of electron shielding it has.

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6
Q

What graph is produced by NMR spectroscopy?

A

Energy absorbed against chemical shift

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7
Q

What is chemical shift?

A

The resonant frequency of the nuclei, compared to that of a 1H atom in TMS.

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8
Q

What is the range of chemical shift for 13C NMR?

A

0-200ppm

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9
Q

What means 13C atoms show a different chemical

shift value?

A

Having different chemical environments (but equivalent atoms show the same peak)

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10
Q

What kind of environment leads to a greater chemical shift?

A

A C atom next to more electronegative atom

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11
Q

What does the number of signals mean? (13C NMR)

A

One signal for each carbon environment (each set of inequivalent 13C atoms)

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12
Q

What does the chemical shift mean? (13C NMR)

A

Greater shift from atoms closer to electronegative atoms or C=C

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13
Q

What does the area under the peak mean? (13C NMR)

A

no meaning

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14
Q

What does splitting mean? (13C NMR)

A

There is no splitting for 13C NMR

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15
Q

Why is it easier to get a spectrum of 1H NMR than

13C NMR?

A

Most H atoms are 1H- it is much more abundant than 13C.

This means almost all H atoms have spin so show up

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16
Q

What is the range of chemical shift for 1H NMR?

17
Q

What leads to a lower chemical shift value for H

NMR?

A

1H with more electrons around them i.e. further from electronegative groups/ atoms

18
Q

On a low resolution spectrum, what peaks would you expect to see for H NMR?

A

One peak for each set of inequivalent H atoms (each chemical environment shows 1 peak)

19
Q

What does the area under the peak represent (for H

NMR)?

A

The area under the peak is proportional to the number of 1H atoms represented by the peak

20
Q

What is the integration trace?

A

A stepped line that makes it easier to measure the area under the curve (height of line = area under that peak)

21
Q

What is TMS?

A

Tetramethylsilane

22
Q

What state is TMS at room temperature?

23
Q

Why is TMS used?

A

Can be added to sample to calibrate the NMR equipment.
It provides a peak at exactly δ=0ppm.
It is the reference point against which all δ are measured

24
Q

What are other advantages of using TMS?

A

Inert, non-toxic, easy to remove from the sample

as relatively volatile

25
When does splitting/spin-spin coupling occur?
Neighbouring hydrogen atoms (3 or fewer bonds away, or on the adjacent carbon) affect the magnetic field of 1H atoms and causes their peaks to split
26
What is the n+1 rule?
If there are n inequivalent 1H atoms on the neighbouring carbon then the peak will split into (n+1) smaller peaks
27
Why must solvents used for 1H NMR not contain any | hydrogen atoms?
Signals from the solvent would swamp signals from the sample, as there is much more solvent than sample.
28
Which solvents are used?
Deuterated solvents: CDCl3, D2O, C6D6 | CCl4 - tetrachloromethane
29
What does the number of signals mean? (H NMR)
One main signal for each set of inequivalent 1H atoms (for each hydrogen environment)
30
What does the chemical shift mean? (H NMR)
Larger δ for 1H atoms closer to electronegative atoms or C=C
31
What does the area under the peak mean? (H NMR)
Proportional to the number of atoms represented by that peak
32
What does splitting mean? (H NMR)
Number of smaller peaks = 1 + number of inequivalent hydrogen atoms 3 bonds away
33
Why does the peak from O-H bonds disappear if D2O is used as a solvent?
O-D bond is formed in preference to O-H due to labile protons that move/ swap from one molecule to another.
34
What are the units and symbol for chemical shift?
Parts per million (ppm) | Symbol: δ