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14. Serial Crystallography: CFEL TapeDrive

Version 31.1 by ahenkel on 2021-12-07 23:47

TapeDrive_beschriftet-tile.jpg




14.1 Revert from Crystallography to TapeDrive (P11 staff/CFEL)

  • remove vortex
  • beamstop to out-position?
  • remove goniometer. The airbearing should be stopped (p11/servermotor/eh.1.01)
  • move cryojet out of the way, ramp the cryo up and shut it down. Close the compressed air to the shield flow. The biggest cable kinks and needs to be disconnected.
  • stop refill of the robot dewar and empty the dewar, warm up.
  • Disable backlight (unplug Festo connection). Is this still needed?
  • mount the 10 um diode and connect (via connector on the granite). This is connected to the leftmost Keithly (power up, check that settings are gain E06, Filter on, Rise time 1 ms. Keithly is connected to the oscilloscope and the delay generator, delay generator is connected to oscilloscope and detector, see diagram in P11 wiki. Insert here the setting for oscilloscope. Make sure to connect the multi-trigger to the back of the detector instead of the standard trigger, when starting to use the chopper (pull the thin ring with ‘grip’ area to detach). Cables are labeled. Make sure before using the chopper that the channels are enabled.
  • move goniotower to X ~ 17 000

Mounting of the TapeDrive is done by the CFEL group. Electronics and control units are combined on a small shelf, that requires only one power and network plug-in. The shelf will be placed left-sided (looking upstream) to the detector tower. The ElveFlow and control laptop as well as several necessary consumables are placed on a cart, which is to be positioned on the right (looking upstream) against the robot platform. The CFEL chiller is placed on the right of the platform and connected to the TapeDrive GASnozzle.


  • adjust focus of the tape by moving X in goniometer tower until you see it in the overview camera. Final adjustment should be done when there is flow. Latest value is about 4500 in X and also 5000 in Z (higher soft limit changed from 2976,63 to 6000). Better to use the back illumination in the GUI to focus the tape - old instruction, not sure if this is the case. Back illumination is the external light source in the detector tower (the crystallography backlight should be disable for tapedrive).
  • Check the Minimum Detector Distance; the detector should not collide with the tapedrive while driven to 154 mm but it has to be verified. Also check that all cables and capillaries are taped away when the users start, so that nothing protrudes further than the tapedrive itself. Soft limit can be edited in eh.3.11 Atk panel.
  • Reconfirm the alignment of the beamstop, once everything, including the nozzle, is in place. Modify config.ini for beamstop in- and out-position to both mach in (27 000). This way the beamstop will not be driven out when the hutch is opened, to avoid that the users forget to drive it in when restarting after entering the hutch.


Prepare necessary controls for data collection:

  • ATK panels:
    • p11/simplon_filewriter/eh.01
    • p11/simplon_detector/eh.01
      • count time = 0.0075
      • trigger (ints if working without the chopper, # or triggers is 1, exts if with the chopper, # or triggers = number of images). Exts is also the standard trigger in normal crystallography. If GUI is used to take images (e.g. for beamstop alignment) the trigger mode will be forced by that and needs to be reverted manually for the users to continue.
      • numer of images = 100 000
      • number of images in container = 1000
      • mode 16m/4M
      • detector distance = 200 mm (usually)
    • p11/detectortower
    • p11/motor/eh.09
  • remote access to TapeDrive control laptop:
    • open terminal, execute command:          xfreerdp +clipboard /size:1920x1080 /u:Cfelusr /v:cfeld-pcx22611
                                                                   password: written on control laptop
  • Cameras:
    • haspp11ethcam1 → detector tower camera to monitor nozzle
    • haspp11ethcam4 →  goniometer camera to monitor tape from above
  • OnDa (on haspp11user04): 
    This starts both GUIs (Frame Viewer & Crystallography GUI) and onda-monitor, the server component. The tool has a bunch of parameters which you can list with ./onda-runner.py —help.
    • 16M mode →    cd /home/p11user/CfelSoft/202103_onda
                               ./onda-runner.py onda-config/onda-config-Eiger16M.toml
    • 4M mode   →    cd /home/p11user/CfelSoft/202103_onda
                               ./onda-runner.py onda-config/onda-config-Eiger4M.toml


14.2 Sample characteristics and preparation

suspension of microcrystals, at least 200 µL with 20% crystal density(more is always better), size range: 2-30 µm, tip: bring some mother liquor for washing, filtering, diluting etc.

Preparation:

  • filter through 30 µm cell filter (green) into Eppendorf or Falcon (original!) tube

20211201_095534.jpg


14.3 Connecting sample to ElveFlow, sample exchange

    • ===

After filtration, screw the ElveFlow connector to your Eppendorf or Falcon tube. Make sure that the yellow-ish line goes to the bottom of your tube. You can adjust the length by unscrewing the blue fitting on top and pushing/pulling the yellow-ish line. Don't forget to tigthen the blue fitting afterwards!

Be aware to which channel and nozzle line your sample is connected.

            Red → Channel 1, crystal line (nozzle capillary without marks/with red marks)

            Green → Channel 2, substrate line (nozzle capillary is marked in black)

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After finishing data collection, flush all lines by connecting an Eppi or syringe filled with ddH2O.

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14.4 TapeDrive operation

    • ===

The TapeDrive is controlled through kamzik. To open kamzik, start the server. A terminal will open and shortly after a small window.
Now start the client. Same thing, a terminal will open, shortly after a small window.

Click 'Devices' in the client session to open the control window.
screen.PNGserver client.PNG

Tape

  • Click on the 'main tape' icon
  • Change the velocity by typing anything from 0.3-3.0 mm/s
  • Common velocity is 1.0-1.5 mm/s
  • kamzik displays the used tape in m and %. At 98% the tape will automatically stop since the rolls need to be exchanged at this point.

  • kamzik_tape.PNG

Sample nozzle

  • Click an the 'nozzle' icon.

  • The nozzle position can be adjusted in xyz by clicking on the arrows up and down. (Double arrow = 10 steps). Step size can be varied, 1mm steps are rather big and should be used carefully.
    The absolute position is not calibrated and therefore changes after each restart of kamzik.

    !!! During data collection make sure in which direction you are moving, do not move nozzle into beam !!!

    Adjust the nozzle position by eye until it nearly touches the tape and roughly meets the X-ray interaction point. Then, move to the control hutch to use the on-axis microscope for fine adjustment. Move the nozzle tip to the beam position (red X) and write down the absolut nozzle position. From there move the nozzle in +x to your desired distance.Different distances combined with the tape speed result in several delay times for time-resolved experiments.


    direction

    recommended step size
    for visual adjustment

    recommended step size
    during data collection

    +x

    away from X-ray interaction point

    1.0 - 0.5 mm

    0.1 - 0.2 mm

    +y

    up

    1.0 - 0.5 mm

    0.1 - 0.2 mm

    +z

    towards detector tower, away from tape

    0.5 - 0.2 mm

    0.1 - 0.2 mm
    be careful with -z, tape could be pushed out of focus



  • kamzik_nozzle.PNG

Temperature control/Chiller

  • The chiller circulates fluid through the gas





Once the hutch is interlocked, set remote control to the TapeDrive laptop by opening a terminal and executing the following command:

                                        xfreerdp +clipboard /size:1920x1080 /u:Cfelusr /v:cfeld-pcx22611
                                        password: written on control laptop (changes every 6 months)



14.5 Tape roll exchange

The tape stops automatically at 98% used length, if you need to change the rolls for orther reasons, stop the tape (velocity = 0.0 mm/s).

  • Remove the (almost) empty feeder roll by pulling it upwards.
  • Cut the tape with some cm overlap to glue to the new roll. Do not discard empty roll!
  • Get a new tape roll (bottom left on the cart). Polypropylen 15 µm
  • Cut the first cm of the new tape roll, directly before the black sticky part.
  • Use this sticky part to attach the end of the old tape to the new roll. Place new roll on roll holder.
  • Open magnetic tape stabilizer.
  • Start the tape (3mm/s). Once the connetion side (black sticky part) has arrived at the collector roll, stop the tape (0mm/s).
  • Again, cut the tape directly in front of the black mark. Replace the the old roll with the empty one. Old roll can be discarded.
  • Attach new tape to the empty roll by using the black sticky part.
  • Close tape stabilizer.

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14.6 Nozzle exchange


14.7 Data collection


14.8 Troubleshooting

  • Tape stopped

  • Nozzle motors are not responding

  • Sample flow is not responding to higher pressure