Insert the capillary into the threaded aluminium block such that the flat end of the ferrule sits on the back face of the threaded hole.

Whilst applying downward pressure onto the blocks to ensure that they are in contact with the base of the alignment jig, tighten the grub screw until they start to bite on the aluminium blocks. Over-tightening may result in the formation of burs that will obstruct the capillary assembly from slotting into the cell easily. If this occurs then sand down the blocks on a flat surface.

Undo the alignment screws for the sample position so that there is plenty of room in the track to insert the aluminium blocks.

Insert another spacer block (optional and not necessarily possible)

Ensure the Ethernet port on the unit is connected to a valid Ethernet port in the hutch.

Plug the unit in to the appropriate power supply for the required output power. Generally this will be mains voltage for the hydrothermal cell.

Connect the cell to the power unit via. the white Han A connector.

Each controller can control two loops. At this point the hydrothermal cell only uses one heating loop.

Ensure that the button in the top right hand corner for the heating loop (generally loop 1) is switched to "ON".

Set the Setpoint to a value around room temperature. Press enter for the change to be accepted and check if the green value to the right gets updated. If not then there may be a problem with communication to the device. Ensure the controller is switched on and that the button in the top right corner reads "ON". Check that the Ethernet port is functional.

Select an appropriate Ramprate. (The GUI reads C/s as units but this is actually °C min^-1)

Change the Manual mode option from "Manual" to "Automatic". This will allow the controller to modify the output power to maintain the setpoint.

The Output can be left at 0 when in automatic mode. If in manual mode then the output power can be changed manually. This is sometimes useful for cooling the cell, but remember to change the mode back to automatic before heating the cell again. The green value to the right will update as the controller increases/decreases the power output.

The Temp value is the read-back from the control thermocouple (1 mm K-type in the top of the cell)

The PID values can be modified and tailored to the experiment.

The Temp value on Loop 2 is generally set up to be the read-back from the 0.5 mm K-type thermocouple in contact with the sample.

Start a data collection. Once you have enough data points at ambient temperature change the Setpoint to the required temperature. Do not exceed the temperature previously agreed with the beamline staff for the PID values being used.

If the cell doesn't start to heat check the following;

• That you are on the correct tab for the control loop being used (normally Loop 1)
• The relays on the power supply are engaged (blue light on)
• The cell is plugged in.
• The power supply is plugged in and switched on.
• The setpoint has actually been sent to the device (green value to the right reads correctly)
• The loop is switched on
• The mode is set to automatic.
• The ramprate is correct.