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Hetcor: HET COR
Hetcor: HET COR
Introductory sequence: y z
90
90, t1 = 0 90 x
x
y
13C:
y z
90 90
90, t1 = J / 4 90 x
t1 {1H} x
1H: y
y z
90, t1 = 3J / 4 90 x
x
y
HETCOR (…)
• the amount of inversion depends on the JCH coupling.
• it will also depend on the 1H frequency (d).
• from SPI and INEPT -> polarization transfer (coherence transfer) to the 13C
1,2 3,4
13C
4
••
2 1H
1H ••••
• • • • 1,3 2,4
••••• 3
• • • • •
13C
1 I S
nucleo I insensible nucleo sensible,
del carbon del proton
• since the intensity of the 13C signal that we detect on t2 is modulated by the frequency of the
proton coupled to it, the 13C FID will have information on the 13C and 1H frequencies.
Heteronuclear polarization transfer – SPI (Old stuff)
2,4
13C
••••• 4
•••••
2
3,4
1H
1H ••••
••••
3
••
13C
1
1,2
pretty cool, if we consider that I S
we had started with
a 13C signal that looked like
this: 1,3 2,4
1,3
I
• The intensity of the 13C lines will depend on the 1H population inversion, thus on w1H.
Stacked plot for different t1 times:
w13C f2 (t2)
• The intensity of one of the 13C lines from the multiplet will be an equation that depends on
w13C on t2 and w1H on t1, as well as JCH on both time domains:
JCH w1H
f1
f2
• Not symmetrical, because one axis has 13C frequencies and the other 1H frequencies.
• JCH coupling splitting all the signals. JCH are in the 50 - 250 Hz range → overlap of cross-
peaks.
• Get rid of them without decoupling (if we decouple we won’t see 1H to 13C polarization
transfer…).
HETCOR with no JCH coupling
180 90
t1 / 2 t1 / 2 D1 D2
13C:
90 90
D1 D2 {1H}
t1
1H:
D average value.
HETCOR with no JCH coupling
•Methine carbon (1H magnetization):
z
y
90 (w1H - J / 2) t1 / 2
x x
(w1H + J / 2)
y
y y
18013C t1 / 2
x x
• If D1 is set to 1 / 2J both 1H vectors will dephase by exactly 180 degrees in this period:
y z
D1 90
x x
y
HETCOR with no JCH coupling (…)
•13C magnetization
z
y y
5
90 x D
2
x 3 5 x
5 3
y 3
w1H
f1
w13C
f2
la unica diferencia con el INEPT es
que se cambian los tiempos fijos por
tiempos de correlación
magnetization see
the slide above
HETCOR Disadvantage? We must acquire an "insensitive" nucleus. As we will
see later, HETCOR has nowadays been superseded by the more time-efficient
reverse methods.