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Summary - Unit 19 - Modern Analytical Techniques II
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MODERN ANALYTICAL TECHNIQUES #HIGH RESOLUTION MASS SPECTROMETRY
↳ measure relative mass to several decimal places
Mr > Mr
e .
g (H3CH0-44 0302 Mr
whole
.
.
whole no
. no
3348-44 0624 Mr
Mr 10 dp)
.
=
same .
SPECTROMET I
NMR
A odd no . of protons and neutrons 'M : I proton , Oneutron
CH3
>
-
gives good sign
↳ small mount
13C NMR High Res H NMR nuclear
13
C : G proton 7 neutron inert
I
.
,
spin isotope
↓ ↓ non-toxic
⑳
how carbon atoms volatile H
hydrogen atoms
, -Si-CH
are are
how
amanged arranged
-
easy to remove
↳ Hy
FACTORS AFFECTING NMR age
field
magnetic tetramethylsilane (TMS
shielding from surrounding e-
&
-
neighbouring atoms affect shielding
I
-
↑
·
Ot will reduce
shielding of 28 + MAG FORCE
2 .
.
g NO EXTERNAL FORCE EXTERNAL .
energy
full chain NMR
X
NOT just immediately ↑ fires ↓ ↓ ↓ ↓ ↓ ↓
bonded ↓ + X
r a d i owave s
=>
-I
4 Bo n un 44 F
444 Nuclei spin in random
111 more
H -
c - c -
c -
H -
c -
c -
c -
Bon - C c - -
Br Br - c -
C -
Br
directions
aligned with
MF So
I i
move is absorbing
i in in i in radio waves
nuclei Spin either :
in direction of the magnetic field
↓
-
field
what's
·
against direction of the magnetic
this is
2 carbon 3 carbon 2 1 measured
environments
hydrogen hydroges
environments enviroments environment
CARBON NMR SPECTROMETRY
This table will be provided :
H H
13
CNMR but
peal at 190 is a
carbonyl group
chemical Shif 6/ppm
I I puseaway
bite samea field could be :
/
3 40 C C
C C
-
H c
-
- - -
I I
-
↳highera 10-70 R-C-C)
O
(orBu) -
aldehyde
↳6 lower
20-50 -
net one
I H
L XTMS R- -
8
chemical
shift
25 -
60 R -
C - N peal at 60 is a C-O group but
208 ISO 100 so o 208
could be :
50-90
#
C -
O
A chem
alcohol
90 C C
-
-
150 =
-
ester
110-125 R-CEN
13
CNMR -
ether
110-168 n
ro
V
160-185 carboxylic acid
r -
- /ester
g
190-220 11
aldenyde/
OXTMS R C -
netune
-
200 ISO 100 So
ELEMENTAL ANALYSIS
HYDROGEN NMR SPECTROMETRY
n
>
-
determines %
composition
mass of elements that make a compound
integration trace : -
'H NMR 3 helps show the
> determines
H molecular/empirical
-
vario of formula
/
are a
I
G peaus ↳
x3 height for structure can be determined
T
H -
c -
C sometimes called
- ~ decimals
I O -
H
H -
1
THIN LAYER CHROMATOGRAPHY
5 CHRO
Oxims
-
of
in
20 IS 10
>
so
Mixin spots dissolve
C - more once the some -
-
is
Yu
near the top
H NMR singlet peal
~
Oh neighbouring the solvent level
allow to
dry
>
-
doublet pean-
I I
triplet peak-
1 h neighboringaa
n - c -
c -
O -
H quartet -
peau 3 I neighbouring
11
un
GAS CHROMATOGRAPHY
20 Is 10 s O
eator
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