8 Performing a Measurement
60
D52IB001EN-G
8.6 Heating and Cooling the Sample
Sample heating/cooling can be done in two ways:
• You can enter the desired heating/cooling rate
and the target temperature manually into
CCU100 (see chapter chapter 6.4).
• You can use a computer with the software deliv-
ered by Anton Paar GmbH to control TTK 600.
TIP:
Usually, TTK 600 is integrated in the software
that controls the X-ray diffractometer. Read the in-
struction manual of your diffractometer control soft-
ware.
In order to heat the sample with manual control, pro-
ceed as follows:
1. Turn on the heater with the HEATER button.
2. Use the <scroll> button to select the set point
(SP). After this step the LED switches from Pro-
cess value to Set Point. Use the <Up> or
<Down> keys to select a set point temperature
between -190 °C and 600 °C.
3. The TTK 600 starts to heat/cool according to the
settings. The set-point temperature will be held
until the set-point is changed or the heater but-
ton is pushed (switching off the heater).
4. Wait until the set-point temperature has been
reached. Depending on your experimental con-
ditions, it may take some time until the sample
temperature is stable due to the required heat
transfer between sample holder and sample and
the heat conduction through the sample.
8.7 Carrying out the Measurement
To perform the XRD measurement, proceed as fol-
lows:
1. Check whether CCU 100 displays a tempera-
ture close to room temperature.
2. Turn off the heater and remove the sample
holder.
3. Prepare the sample and insert the sample
holder with the sample.
4. Close the lid.
5. Turn on the heater.
6. If necessary, align the sample height at 25 °C
before starting an experiment. This can be done
by measuring the peak position of a known
phase in the sample and re-adjusting the sam-
ple (chamber) height until the peak is at the cor-
rect 2
θ
-angle.
TIP:
If you measure powder samples and prepare
the sample as described in chapter 8.2.5, it is not
necessary to align the sample height.
7. Create the desired experimental conditions.
8. Heat or cool your sample to the desired tem-
perature.
9. Start the X-ray scan or batch program.
TIP :
Detailed information about diffractometer set-
up and X-ray scans are given in the instruction man-
ual of your diffractometer.
After you have finished your experiment, allow the
instrument to reach 25 °C before you open the
chamber and remove the sample.
WARNING
Risk of cryogenic burns.
Never disconnect the cooling device or any other
components of the sample cooling circuit during
operation. The liquid nitrogen cooling equipment
contains liquefied nitrogen. Liquefied nitrogen
can cause freezing of tissue, or cryogenic burns,
similar to frostbite to eyes or skin upon contact.
The compressed-air cooling components are
under pressure. Disconnected components
present a mechanical hazard.
CAUTION
Risk of injury.
During operation and even after turning off the
instrument, parts inside the sample chamber can
have extremely hot or cold surfaces. Make sure
that the sample holder is at room temperature
before handling it.
Summary of Contents for TTK 600
Page 2: ......
Page 74: ...Appendix B Sample Chamber Dimensions 74 D52IB001EN G Appendix B Sample Chamber Dimensions ...
Page 75: ...Appendix C Declaration of Conformity D52IB001EN G 75 Appendix C Declaration of Conformity ...
Page 77: ...Appendix D Spare Parts and Accessories D52IB001EN G 77 176383 COOLING MODE SWITCHING VALVE ...
