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Chemistry A Level CIE Analytical Techniques

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Chemistry A Level CIE Analytical Techniques

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  • October 26, 2024
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Analytical Techniques

Proton Nuclear Magnetic Resonance (NMR)


-

nucleus of each hydrogen com behoves like a tiny magnet

-
Proton spils and creates magnetic field


-
sample placedIn M f . .




-Protons either line with field or spin
In opposite direction

-
small diff In energy by opposite spinning proton
, corresponds to energy carried by waves in radiowave


range of EM radiation spectrum


-
nuclei 'flip' between two energy levels

-only atoms with mass number is an obd number absorb energy In range of frequencies analysed




NMR


size of the gaps between nuclear energy varies slightly (depending on molecular environment)
-




↳ CH3OH ,
'H atoms in two diff Molecular environments

-
m . .
f


changed because easier than changing - of radiowaves

-
as m f . .
Changed ,
It nuclei In diff environments flip at diff field strengths measured


using reference compound (tetramethylsilane (TMS) =
Si(CH3)4) ,
Value zero

↳ >
gives only one sharp peak
inert ,
volatile liavid which is higher than most
that mixes well >
absorptions measured
All other
with organ ic compounds by shift away iMsline
from
On NMR Spectrum chemical -




Fiesinradiowaves
e In Ppm units
shift measured
n

Energy

-'Against It OH H
I

c -'
(

H - - C- It 3 environments


gre with
it

H
it

O H
i 1 : 1 : b


After I "'

Applied C C C -H 1 environment
H
- - -




it H
"It nuclei In
absorbs energy radiowave range

When they flip from lower energy level , lining cyclohexane 1 environment
C

up with applied m f .

.,
to higher energy level,


lining up against it
. 3 environments


.
2 2 : 1

, NMR measuring
Hydrogen Atoms



·
low resolution NMR


-

single peak for each non-equivalent hydrogen atom


-

heights of peak very

-
area under peak >
-
relative number of equivalentIt atoms responsible for chemical shift




·

high resolution NMR

-

ranges overlap

-
In some molecules , heavy shielding of hydrogen nuclei by lots of e-in surrounding

atoms , peaks shifted beyond usual range

signal NMR made up of cluster of
-


Peaks that appear as one on low grouped peaks , because

m .
f .
generated by spinning nuclei Interfere slightly with neighbouring nuclei (spin-spill couplings
-

exact splitting depends on number of hydrogen atoms on adjacent carbon aroms


-number of signals a peak splitsInto equals n + 1


CH3CH2OH
↳ num of t atoms atom
on adjacent carbon
i H It &
Split (triplet) +(3 + 1) + (3 + 1)
=
↓ .
CH3 TO 3 quadlet H -
C -
c -
C -




i itH
.
2 CH2-split +O 4 (auadruplet) 1 Poly when both sides have hydrogen
lif 1.2. 1.2. Zil


3 . OH not Usually split as 'H atom constantly exchanged with 'H atoms of other molecules



to find presence Of-OH , add D20 13H) -

heavy Water ,
Spectrum for ol will disappear
P T
:

both Odd hence can't be seen in spectrum
4 : I


·

Identifying-OH1-NH-signal

-
-
Oh appears as single peak as it exchanges rapidly with protons of water /acids before interference


CH3CH2OH + H2O CH3CH2OH + HOH

-
if heavy water used ,
-OH/-N-H disappear hence It in them are labile protons

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