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Rigaku FR-X Usage
Training on 2015.03.30
FR-X generator: 45 kV, 66 mA, 70 μ cross-section, 180 μ beam, 1.7 miliradians divergence
Pilatus 300K detector: 3 chips, shorter exposure time, no readout (no shutter closing), almost never overloaded (>1.5 millions), water circulation at room temperature, dry air
>thread
command on camserver gives the temperature and humidity level Green light at the back of the detector to check before use.
Cryostream should be at 100 K
Close 3 glass doors, push the green light on the left (HKL does get info on the shutter status)
Run HKL_3000_P300KChi (the other HKL_3000 version is for data integration only)
Collect/Connect to initialize
(also open an instrument server window in the background)
0.25° oscillation by default As a “rule of thumb” set the detector distance (in mm) to half the longest unit cell parameter (in Å) 1)
Align/Zero goniostat
resets all positions (parameters in /hkl_dc.ini)
2θ always swings away (clockwise)
Set the directory /data/user/project1_crystal1
dtdisplay
- middle click > zoom area
- middle click > reset zoom
- control + left click > move around
- measure /Measure Left 1x, 2x, 3x or 4x (to average)
Never collect at 2θ = 0, use at least 2θ = 2 to offset the center horizontally and avoid thus avoid missing data due to the gaps between detectors
Index
- Refine in triclinic (P1)
- Fit Basic
- Fit All
- Mosaicity (by default it cannot estimate well the mosaicity2), so you need to select)
- To process up to the corner, you need to index up to the corner!
Strategy
- HKL_3000 strategy only works for single axis
- Rigaku_Strategy is specially made for FR-X on the 4 axis
- Choose I want to make changes
- Completeness 99% (to reduce collect time)
- Redundancy 3.0 (4.0 by default)
- Distance (the distance from the first image is set)
- Suggested distance is not useful
- Edit preferences is possible
You can swing the slider on Time window to adjust/reduce the number of collected frames Don't forget to adjust the Mosaicity value! If anomalous data is required, adjust the redundancy accordingly
For some pins, Chi 60° may be too high and should be restricted to 50°
Close the window and choose Setup DC
to transfer the informations to HKL data collection window
Exposure time is not imported from the strategy and should adjusted manually
multi mode is useful to find the best detector distance and exposure time