1. The lead foil must have a thickness of 0,062 mm.
X-ray absorption equation: I(l) / I0 (l) = exp [(-m / p)l px]
The equation above is solved to the thickness x after applying ln,
x = (ln I0 - ln I)
p / m*p
= (ln 108
- ln 10) * 1/230 * 1/11,3 = 6,2 * 10-3
cm = 0,062 mm
3 Marks
Unfiltered incoming
X-ray radiation from a X-ray tube is "white" radiation, with a wide range
of different wavelengths. The equation above is wavelength specific so
every single wavelength has its own absoption coefficient which has to
be taken into account. In the normal case one would look at the wavelength
with the highest intensity and the shortest wavelength and calculate x
from the absorption equation. For secureness the main beam stop would be
slightly thicker than calculated.
The main beam stopper
for a monochromated beam could be thinner than with the non monochromated
beam, because the monochromator reduces the intensity and mostly absorbs
a large part of the incoming radiation with wavelengths away from the
maxima.
2 Marks
2. To
obtain narrow diffraction peaks from organic compounds they have to be
applied as a very thin layer onto the flat sample holder to avoid diffraction
from different areas in the sample which cause the peak broadening. In
doing this the diffracted intensity mostly is significantly reduced and
the peak heights become unreliable. A very thin layer causes another unwanted
fact. The sample holder itself might start to diffract, if it isn´t
made of a completely amorphous material such as glass. With single crystal
silicon one would get additional peaks from the sample holder. A much better
way would be to use another geometry, which allows transmission measurements.
Comment: Better to explain the transparency effect
very briefly - also correctly cut Si wafers do not give Bragg peaks unless they
are badly treated by the user
2 Marks
The ultimate way is
to use X-rays from a synchrotron source in an angle dispersive geometry.
The intensitiy of the synchrotron radiation itself is much higher than
that of a laboratory X-ray tube which is the basic advantage. This allows
to have a much higher absorption or exclusion of X-rays within the measurement
and still get sufficient intensity for high quality diffractograms.
Narrow peaks can be
measured with the use of an analyser crystal between the sample holder
and the detector. The analyser crystal is like a filter which passes on
only a small and to the analyser crystal specific angular range to the
detector. This brings a loss of intensity with it, but the gained peaks
are narrow and still intense enough to have reliable peak heights. The
measurement can be improved by longer collection times, which improves
the signal/noise ratio.
Another but similar
way is to exchange the analyser crystal against a set of foils
(Hart-Parrish),
that are built out of a set of parallel thin metal foils with distinct
length. As above this allows only a narrow angular range of the diffracted
beam to pass on to the detector. Again there occurs loss of intensity,
but as above there is enough intensity for a good diffractogram.
An important advantage
of these two ways is, that the organic sample can be applied onto the flat
holder in a really "thick" layer up to a few mm. By adjusting the detector
and the foils/analyser crystal in the right way the measured area in the
sample is defined. This prevents diffraction of the sample holder with
use of only thin layers. Also movements of the sample don´t disturb
the measurement.
Comment: Excellent answer, but
it would be a little too long in a written examination, where brevity is
often important. More importantly, you have given both possible methods for
exploiting the parallel nature of the incoming beam, but you
didn't specify that it was parallel
1 Marks
3. The rotating angle for the monochromator can be calculated from the Bragg-equation:
l = 2d sin Q
d spacing of Si 111 = 3.136 Å, and l changing from 0.65 to 0.75 Å. The equation is solved to sin Q:
sin Q1 = l1 / 2d = 0.65 / 2*3.136 and sin Q2 = 0.75 / 2*3.136
Q1
= 5.94 ° and Q2
= 6.87 °, D Q
= 0.92 °
4 Marks
hence the rotating
angle for the monochromator is twice the difference: D
2Q = 1.84 °
Comment: Rotating the monochromator
by q rotates the first bounce of the beam
by 2q
0 Mark
4. Again the Bragg-equation has to be used, but changed to calcualte with keV for l.
E = 12.398 / l [keV/Å]; l = 12.398 / E
This inserted into the Bragg-equation yields:
12.398 / E = 2d sin Q
After solving this equation to d the given values are inserted:
d1
(20 keV) = 12.398 / (2*E*sin Q)
= 12.398 / (2*20*sin 1.35°) = 13.155 Å
d2
(100 keV) = 12.398 / (2*100*sin 1.35°) = 2.631 Å
2+2 Marks
d values between these
two
calculated values can be measured with the given photon energy.
1 Mark
5. The
symmetry elements for the given symmetry operators are: