SPB/SFX User Proposal 3333 Shift 2 Summary

X-ray delivery

• 9.3 keV, 1.7 mJ, 202 pulses @ 564 kHz

• 2 pulse trial @ 2.8 kHz (2.2MHz / 800). Doubled data rate for high viscocity jet. Seemed to work quite well although not expected to be a regular use mode!

Optical laser delivery

• Only 819 nm ns laser for the jet visualization

Achievements/Observations

• Data calibration issues solved (thanks to DRC / ITDM experts)

• Silicon wafer post sample attenuator was dismounted. elog: 45

• High viscosity jet delivery @ 10 Hz and 2.8 kHz (2 pulses / train @ max spacing)

• Photosystem-II (@ 41 mm AGIPD Z motor value, adaptive gain) elog: 85,86, various sample preparations

Issues

• ONDA restarts required

Instrument status

• Sample chamber and AGIPD turbos OFF, rough pumping ON

• shutters etc. closed

To do for next shift

• Catcher and shroud (inc windows) could do with a clean before any alignment (PEG delivery)

• Proceed with PCS users

SPB/SFX PCS user proposals (day 1)

X-ray delivery

• 9.3 keV, 1600 uJ/ pulse

Achievements/Observations

• PCS user time (day 1) completed. Several runs from different user groups with visible diffraction patterns, likely not sufficient for full datasets
• Additonal data for nozzle alignment sub-project (Lysozyme)

Issues

• ONDA setup a little fiddly (default data stream name not correct?)

Instrument status

• AGIPD HV off.
• AGIPD gate valve closed and pinned.
• Attenuators set to thickest diamond.
• Vacuum valves closed.
• Sample chamber turbos off
• Laser lamp off

To do for next shift

• clean catcher (watch out for guidance on user sample handling)
• align laser for in-house work
• remaining PCS project if viable

SPB/SFX In-house research 4978 

X-ray delivery

• 9.3 keV 202 pulses / train, relatively stable intensity 1.9 mJ / pulse, some decrease in intensity across train

Optical laser delivery

• PP laser 1030nm 3rd harmonic (343nm) @ 282 kHz, 101 pulses / train

Achievements/Observations

• PP laser timing for 100nm time point
• PP laser / x-ray overlap with buffer + caged compound
• de-oxy Myoglobin + caged compound data with and without PP laser activation of caged compund

Issues

• suspicion of leaking plunger in the last reservoir of the evening

Instrument status

• Shutters closed
• XTD9 atteunators @ thick CVD diamonds

SPB/SFX In-house research 4978 shift 2

X-ray delivery

• 9.3 keV 202 pulses / train, relatively stable intensity 2.0 mJ / pulse at start of train, ~30% decrease in intensity across train
• BKR made an attempt to inprove slope around 18:00, small improvement but degraded again over time
• One short interruption

Optical laser delivery

• PP laser 1030nm 3rd harmonic (343nm) @ 282 kHz, 101 pulses / train

Achievements/Observations

• PP laser timing for 10nm time point
• PP laser / x-ray overlap with buffer + caged compound
• de-oxy Myoglobin + caged compound data with and without PP laser activation of caged compound

Issues

• several nozzle changes requried throughout the day
• significant sample debris on windows from nozzle 'events' requried mid-run shroud and window clean

Instrument status

• AGIPD HV off
• Shutters closed
• in-line vacuum valves closed.

To do for next shift

• shroud / catcher clean needed
• alignment etc.
• in-line crystallisation project

SPB/SFX In-house research 4978 shift 3 - end

X-ray delivery

• 9.3 keV 352 pulses / train, relatively stable intensity ~1.9 mJ / pulse
• beam down ~30 min

Optical laser delivery

• None

Achievements/Observations

• Collected several runs for the in-line crystallisation project but some difficulties to inject, probably a coating issue
• Saw a lot of crystals

Issues

• Realised that there seems to be a vacuum leak from the load lock valve. Optimal pressure is only achieved when the load lock pump is running.

X-ray delivery

• 12.4 keV 200 pulses / train, relatively stable intensity ~0.8 mJ / pulse
• took some time in changing X-ray energy (from 19.16 keV to 12.4 keV)

Optical laser delivery

• 420 nm PP laser
• ns laser for jet imaging

Achievements/Observations

• M1 & M2 offset mirror optimized
• NKB focus roughly optimized (we used defocused X-ray beam, about 2um)
• Collected several runs for inside nozzle pump excitation project (both adaptive gain and fixed MG modes)
• Nozzle damage with PP laser tested (before and after the night shift)

Issues

• AGIPD FPGA (2nd hemisphere) issue (requied a power cycle)

Laser synchronization is gone, unlocked from 04.05.2023, 22.47. E-mail was sent to lbsync-expert@desy.de and c.c. to las-op@xfel.eu.

X-ray delivery

• 12.4 keV 200 pulses / train, relatively stable intensity ~0.8 mJ / pulse

Optical laser delivery

• 420 nm PP laser
• ns laser for jet imaging

Achievements/Observations

• M1 & M2 offset mirror optimized again (not really optimum but acceptable)
• NKB focus checked and defocused to have about 2um beam
• Collected a few dark runs and about 30 runs with PP laser in adaptive gain mode

Issues

• AGIPD Fixed MG mode issue
• PP-laser sync issue, but it was solved quickly, thanks to Lbsync team
• Beam pointing in the FEL Imager was quite off in the beginning of the shift 
• Hit rate too low (~0.3%)

X-ray delivery

• 12.4 keV 200 pulses / train, relatively stable intensity ~1.2 mJ / pulse

Optical laser delivery

• 420 nm PP laser
• ns laser for jet imaging

Achievements/Observations

• NKB focus checked and defocused to have about 3um(H) x 6um(V) beam
• Collected a few hours data with PP laser on both jet and nozzle excitations (AGIPD in adaptive gain mode)

Issues

• IRU Chamber LED was ON until 2:51am 
• Nozzle damage found after ~1 hour measurement 
• Hit rate seems too low still (less than 1%)
• Nozzle exploded close to the end of the shift 

X-ray delivery

• 9.3 keV, 1.8 mJ, 202 pulses most fo the day. Pronounced (~30-40%) slope across the train.
• Pointing initially far off the reference crosshair. One hour required at the start of the shift to go to 9.3 keV and align the beam to the crosshair.

Optical laser delivery

• NA

Achievements/Observations

• Collected diffraction from user calibration sample for detector geometry.
• Screened a variety of user samples and collected datasets with those showing clear diffraction.

Issues

• Pressure spike in MKB_PSLIT area.
• Various issue with several user nozzles.

X-ray delivery

• 9.3 keV, 1.6 mJ, 202 pulses msot of the day.
• Slope across the train reduced comapred to yesterday, now about 25%.
• Changes in number of pulses in SASE3 not always automatically picked-up by kickers adaptation and requiring a nudge from BKR to restore performances.
• Beam down for ~35 minutes early morning, but otherwise stable delivery.

Optical laser delivery

• NA

Achievements/Observations

• Collected SFX data from 10 user samples, including at different detector distances for a few of them. Up to 10% hit rate observed.

Issues

• Still issues with nozzles: gas leak, EtOH leak.
• Multiple ASICs of AGIPD exhibit a jumping offset. Power cycle initiated at the end of the shift.

X-ray delivery

• 9.3 keV, 1.4-1.8 mJ and 12 keV, 1.1 mJ. 202 pulses most of the day.
• Reduced slope after afternoon tuning, down to 20%.
• Change to 12 keV with file prepared earlier this week did not work (no lasing). Tuning to 12 keV took 40 minutes.
• 30 minutes downtime in the morning.

Optical laser delivery

• NA

Achievements/Observations

• Optimised slits to protect the nozzle from X-ray damage.
• Collected data with a dozen of user samples. High hit rate and resolution achieved with some of them.

Issues

• No major issues.

X-ray delivery

• 9.3 keV, 1.8 mJ, 202 pulses most of the day.
• Attempted tuning to 14.8 keV during the first hour fo the shift did not work out. More time will be spent tomorrow morning tuning to that photon energy.
• Overall stable delivery. Only a magnet failure at 20:25 resulted in a drop of energy and was quickly recovered. Interestingly, during that time the slope through the train was reduced.

Optical laser delivery

• NA

Achievements/Observations

• Collected diffraction data from multiple samples, including mixing at different delays. Smooth sailing with the same nozzle for the entire day.

Issues

• Run controller and data manager crashed around 23:00 just as we were about to collect data from the last sample. Both devices were reinstantiated.

X-ray delivery

• 9.3 keV, ~1 mJ, 1-30 pulses, stable delivery

Optical laser delivery

• None

Achievements/Observations

• Direct beam trajectory alignment
• Alignemnt of IRD and microscopy screens
• rough alignment of XPD WFS

Issues

• beam down for sometime
• AGIPD slow data configuration issue, solved by DRC+Cal OCD

X-ray delivery

• 9.3 keV, 800 uJ, 1-200 pulses, stable delivery

Optical laser delivery

• None

Achievements/Observations

• CRL chamber alignment
• CRL lens stack alignment
• XPD WFS alignment with CRL focused beam

Issues

• Some of the CRL lens stacks needs realignment

X-ray delivery

• 9.3 keV, 800 uJ, 1-200 pulses, stable delivery

Optical laser delivery

• None

Achievements/Observations

• HWFS direct beam measured
• CRL focus measured with YAG screen and camera
• Setup for CRL heating measurement installed

Issues

• Difficulties with operation and syncrhonization of FLIR IR camera

X-ray delivery

• 10.7 keV, 1.2 mJ, 1-200 pulses, stable delivery

Optical laser delivery

• None

Achievements/Observations

• Crystal alignment for X-ray microscopy except one crystal
• Sample camera and Cu mesh were aligned to X-ray position

Issues

• We found strange strip on the beam in XTD0 screen

X-ray delivery

• 10.7 keV, up to 339 pulses at 1.1 MHz.
• Large slope through the train, up to 70% with 339 bunches. BKR was not able to find the cause so far, we agreed to pursue this further tomorrow.

Achievements/Observations

• Timing optimisation of FLIR camera.
• Heating measurement of Al and Be CRLs with FLIR camera and thermocouples.

X-ray delivery

• 10.65 keV, 128 pulses at 1.13 MHz and 16 pusles at 141 kHz.
• Slope reduced at the start of the shift. Approximately 20% slope after that with the patterns used for data collection today.

Optical laser delivery

• NA

Achievements/Observations

• Spectrometer setup and aligned. Collected first data with GOTTHARD II.
• Measured multiple static samples with Bragg magnifier.

Issues

• No issues.

X-ray delivery

• 10.65 keV, 128 pulses at 1.13 MHz and 16 pusles at 141 kHz.
• Overall stable delivery.

Optical laser delivery

• 800 nm, 50 fs, 1-226 pulses at 1.13 MHz.
• A few issues with minor impact on operation this week. Detail communicated to LAS.

Achievements/Observations

• Continued characterisation of crystals (thermal measurement, interferometry, imaging) under different beam conditions ranging from direct to focused beam.
• Spectral measurement in parallel to crystals characterisation.
• Imaging of static samples with Bragg magnifier.

Issues

• DAQ configuration failing multiple times. Repeating the same sequence of actions yield variable results.
  • Several times with unhelpful message "Failed to execute "assign" action".
  • On one occasion with the message "Assignment for data-source/group 'SPB_CFEL_JF1M/DET/JNGFR09:daqOutput'/'SPB_CFEL_JF1M_9' not specified." even though we used this group before without any issues.
• JUNGFRAU 1M acquisition could not be stopped. Restarting control and receiver servers and associated devices resulted in the control device being stuck in INIT state. Detector had to be power cycled to solved the issue.