shift summary from Saturday 15.04.2023:

Tasks:

- Calibration of Euler MDL

- Vibrometer measurements at M3 using the RY piezo

Beam was aligned to MID popin

we used values stored in MID setpoints 'B' but went there manually, using the EulerMDL

M1 - X value was corrected, as we found the center of the beam/mirror to be at 6.4mm - calculated beam angle after M1 is 2.14mrad

M2 - values slightly differ from saved setpoints but were quite well met using EulerMDL to reach the same beam position

M3 - we had to remove it a bit further from the beam, as it seemed to intercept it, when we first tried to get the beam through. This might in the end not have been necessary

End of shift:

beam aligned to MID

preabsorber in

SRA fully open

X-ray delivery

• 12.0 keV, 1.3 mJ, 1-168 pulses @ 564 kHz
• Decaying intensity between 1:20 and 2:40, otherwise stable delivery.

Optical laser delivery

• 1030 nm compressed, THG
• Stable delivery

Achievements/Observations

• Optimised PP laser THG conversion efficiency.
• PP laser spatial and temporal overlap with water jet.
• Collected lysozyme diffraction for detector geometry.

Achieved

1. Brought the 800 nm of optical pump laser to the hutch after the intervention. 
2. Found the rough spatial and temporal overlap between the X-ray and pump laser with MID X-ray eye. 
3. Found the sufficient photo-induced effect on the user sample (HfN) with one unpumped X-ray pulse and 12 pumped X-ray pulses. 
4. Installed the lambda/2 wave plate and controlled the optical laser polarisation at the sample surface.
5. Bragg peak analysis via Extrafoam provides an intuitive and prompt result during the measurement, which is very useful for deciding the following procedure of measurement. 
6. A measurement scan for 3D reciprocal mapping has been collected using the Karabacon macro for varying the time delays and omega angles.

Issues

1. The Jungfrau detector dropped approximately 60% of trains in the saved data.

Report

1. The optical pump laser was not able to be brought to the first X-ray pulse. The first unpumped X-ray pulse data is used as a reference, which is useful to this experiment. 

X-ray delivery

• 12.0 keV, 1.3 mJ, 1-168 pulses @ 564 kHz.
• Stable delivery.

Optical laser delivery

• 1030 nm compressed, THG.
• Stable delivery.

Achievements/Observations

• Collected static and TR-SFX data.

Shift Summary

1. Collected optical laser-induced dynamics in HfN and STO/SRO samples.
2. Jungfrau detector transferred data without data dropping issue. 

X-ray delivery

• 12.0 keV, 1.3 mJ, 1-168 pulses @ 564 kHz
• Cryo issue at 3:33

Optical laser delivery

• 1030 nm compressed, THG.
• Stable delivery.

Achievements/Observations

• Collected TR-SFX data. Smooth sample jetting.

Issues

• Beam down, shift ended earlier.

Quick aligment of the instrument with quiet good HXRSS performance after cryofailure

Checking of t0 to the optical PP laser

Test of energy scanning macro (Undulator + HXRSS)

Cool down of sample and measurement of first delay points until cryo failure 2

Beam loss due to cryo plant failure

SPB/SFX User shift 1 3333

X-ray delivery

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

Achievements/Observations

• Silicon wafer post sample attenuator (240um, ~10% transmssion @ 9.3 keV) was mounted in-front of the AGIPD detector. elog: 3

• Beamline is aligned for the NKB trajectory and the x-ray focus size of 300 nm being achieved. elog: 4

• Copper flat field including 240 um silicon wafer attenuator. elog : 7

• Lysozyme and Photosystem-II data (@ 41 mm AGIPD Z motor value) elog: 5

• Fixed medium gain used initially, later switched to adaptive gain to allow high gain for peaks behind Si attenuator mask. Switch of both calibration pipelines..

• data at full transmission. Move to medium gain for water ring outside Si attenuator

• Several blocked nozzles, at least potentially caused by never filtered sample.

Issues

• Problems with post calibration analysis, observing 'disk quota error' - SPB/SFX RC to investigate with instrument data team and DRC

• problems with data calibration - SPB/SFX RC to investigate with instrument data team and DRC

Instrument status

• AGIPD off and warm

• AGIPD gate valve OPEN and pinned.

• Attenuators set to thickest diamond.

• Vacuum valves closed.

• He valve closed.

• Sample valves cleaned.

• ns laser off.

• Sample chamber and AGIPD turbos OFF, rough pumping ON

To do for next shift

• remove Si post-sample attenuator

• continue with user program (small crystals DFFN etc. see elog)

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.

Shift summary:

- get the beam with 23keV and 120µJ 

- falignment of mirrors m1 and m2 on the pt stripe at 23keV

- irst time lens alignment with CRL1 and CRL2, get beam size of 5µm at sample position for users

- took data for the calibration of the AGIPD detector quadrants with LaB6 and Al targets

- set-up trigger of in-vacuum camera and ns-laser to match x-ray arrival time

- could not move the AGPID detector

Beamline status:

- Lenses insert, DN500 closed, AGIPD HV off, Feedback running with 5 pulses and increased attenuation (2mm Si in XTD6 ATT and 0.8 Si OPT ATT additional).

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)

X-ray delivery:

- stable at 120µJ, mostly 63 pulses

- 1:30h downtime

- checked some alternativ lens configuration to test for smallest focus

- changed nozzle of liquid jet. The old one was strongly tilted at low flow rates

- overlap between x-ray / liquid jet achieved 

- first scans from pure water at different jet distances

Problems:

- still problems with AGIPD detector movements (Motor is a state that does not exist in Karabo, only a reset on PLC level seems to solve the problem for a short time)

- x-ray beam has hit part of the shielding resulting in some damaged pixels on the AGIPD.

achievements:

• inserted the magnet and measured delay scan at the maximum magnetic field with opposite directions
• data analysis showed that runs measured during the afternoon/evening led to sample degradation (the sample shows a dark spot, change in the scattering signal is also cearly visible)
• corrected spatial overlap
• moved to gresh spot and did delay scan at lower OL fluence (Tr = 35% instead of 70%)

problems:

• shortly before 23:00 the optical laser synchronization was lost for a bit more than 2 hours, then it came back shortly after 1 am at that time the PP laser phase shifter when optically lock moved from 1018 to 229.8 apparently on its own, and it was realized few hours later. We moved it back to the original value, but this was not sufficient, we had to move by several ns and we were not able to move where we wanted, Laser OCD was called a7 7:35.

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%)

- We get stable x-ray delivery with 130µJ.

- We could move the detector succesfully in and out of the LFoV configuration!

- We added a hole in in the black Kapton foil and increased the holes in the Kapton shielding of the jet. These were not positioned well, due to a misalignment of the ALAS. After this intervention we did not observe any scattering rings on the detector.

- We aligned the liquid jet and get a nice diffraction rings from water. 

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