Rigaku XtaLAB mini User manual

Cat. No. 2366A201
XtaLAB mini
Cryogenic gas suction attachment
Instruction manual
Manual No. ME12973A02

This manual describes the correct use of the product as well the usage precautions to be observed. To
obtain full-expected performance from the product, thoroughly read this manual.
Also, store this manual at an easily accessible place so that you can promptly refer to it whenever
it is necessary.
The contents of this manual are subject to change without prior notice.
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the written consent of Rigaku Corporation.
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ME12973A
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Table of Contents
1. Overview.....................................................................................................................................................1
2. Cryogenic gas suction attachment - installation and adjustment..........................................................2
2.1 Wiring the electric power supply cable .............................................................................................2
2.2 Fine alignment of the cryogenic gas suction pipe..............................................................................5
2.3 Evaluate operation and performance .................................................................................................6
2012. 02 (Second Edition)

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ME12973A
1.
Overview
The cryogenic gas suction unit has been developed as an attachment for the XtaLAB mini. The unit aims
at reducing the ice buildup on the sample while at cryogenic temperatures. The role of the unit is to
redirect the cold gas, flow and reduce the amount of ice accumulation.
* Please refer to or read other manuals including“XtaLAB mini system Maintenance Manual
(11568C*)” and “CrystalClear Ver. 2.0.0 for CCD system (for Small Molecules) (13292D*)”
for more information before using the system.
The components of the unit are illustrated as follows.
Suction pipe
Gonio cover
for cryogenic gas suction
Main body
Adapter
Fig.1. Cryogenic gas suction attachment components

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ME12973A
2. Cryogenic gas suction attachment - installation and adjustment
2.1 Wiring the electric power supply cable
(1) Turn on the power of the XtaLAB mini and water chiller system.
(2) Launch CrystalClear and login. After logging in the dialog window Open sample will be
displayed. Click the Cancel button.
(3) Click the Manual Instrument Control under the menu bar item Instrument.
(4) Click the Initialize button in the Manual Instrument Control dialog window to get
synchronization between goniometer and software.
(5) Move the Omega axis to 90 degrees.
(6) Close the CrystalClear software and turn off power to the XtaLAB mini and the water chiller
systems.
(7) Remove the collimator and beam stop from the XtaLAB mini and mount the protective cover
on to the face of the detector (Fig.2).
(8) Remove the nozzle of Low-Temperature Gas Cooler from the XtaLAB mini.
(9) Remove the X-ray enclosure of the XtaLAB mini.
(10)Remove the three screws on the goniometer cover (Fig.3) and remove the goniometer cover.
Fig.3 Screws on goniometer cover
Fig.2 Detector face cover
Detector face cover
(XtaLAB mini accessory)

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(11)Locate the cable from the gonio cover for cryogenic gas suction unit. Pass the cable through
the hole at the center of the Omega axis to reach the back side of the goniometer (Fig.4). Next
attach the gonio cover for cryogenic gas suction and the cryogenic gas suction tube.
(12)Confirm the cable at the rear side of goniometer goes through the hole along the Omega axis.
Pass the cable through the wiring duct (Fig. 5) near the USB ports at the rear of the XtaLAB
mini.
(13)Remove the USB extention port in the XtaLABmini rear to get a hole. Pass the adapter cable
through the hole. Connect the adapter cable with the cable of the gonio cover for cryogenic
gas suction described in step (12). (Fig.6)
Fig.6 Cable connection
Fig.4 Cable wiring -1
Fig.5 Cable wiring -2

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(14)Connect the adapter cable to the power outlet.
(15)Mount the suction pipe into the cryogenic gas suction. Refer to the Fig.7, the cooling gas
alignment guide must be positioned at the bottom of the suction pipe when switching on the
cryogenic gas suction at the left.
Mount the pipe such that the height from the top to the main body is around 56 mm. (Fig.8)
Fix the suction pipe into the main body using the slotted set screw. (Fig.9)
56 mm
Fig.8 Location of the suction pipe
Cooling gas alignment guide
Fig.7 Installation of suction pipe
Set screw to fix the suction pipe
Fig.9 Fixing the suction pipe

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(16)Mount the cryogenic gas suction on to the goniometer cover. Then, connect the cable to the
goniometer cover for the cryogenic gas suction. (Fig.10) Fix the cryogenic gas suction to the
goniometer cover without any screws as the stand of the suction is magnetic and securely
attaches to the metal cover.
(17)Turn on the switch of the main body of cryogenic gas suction and make sure that the fan is
running inside the main body and makes a little noise.
(18)Mount the X-ray enclosure of the XtaLAB mini.
(19)Mount the nozzle of Low-Temperature Gas Cooler to the XtaLAB mini main body.
(20)Remove the protective cover on the detector. Mount the collimator and beam stop.
2.2 Fine alignment of the cryogenic gas suction pipe
(1) Turn on the switch on the main body of cryogenic gas suction.
(2) Turn on the power of XtaLAB mini and the water chiller system.
(3) Launch CrystalClear and log into it. After login in the system, the dialog window Open
sample will be displayed. Click the Cancel button.
(4) Click on the Manual Instrument Control under the menu bar item Instrument.
(5) Click the Initialize button in the Manual Instrument Control dialog window to get
synchronization between goniometer and software.
(6) Move the Omega axis to -70 degrees.
(7) Mount the goniometer head, which holds the sample, to the goniometer.
(8) Launch RAXVIDEO and center the sample.
(9) Move the Omega axis to 90 degrees.
Fig.10 Installation of the main body of cryogenic gas suction
Cable to the goniometer cover
Goniometer cover
for cryogenic gas
suction

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(10)Adjust the position of cryogenic gas suction tube to direct the flow toward the sample center,
as illustrated in Fig.11. From the view point at the front of the equipment, adjust the center of
the cryogenic gas suction pipe to be aligned with the sample.
2.3 Evaluate operation and performance
(1) Click New Sample under File in the CrystalClear menu bar.
(2) Initialize Instrument and then, set up a measurement according to the following conditions for
one image within flow-bar step Initial Images.
Start Angle (˚) End Angle (˚) Width (˚) Exposure time (sec)
30 31 1.0 16
(3) Inspect the image and make sure there is not a shadow of the suction pipe in it. If it has a
shadow of the suction pipe, you will see something similar to the image in Fig.12. In such a
case, adjust the height of the suction pipe.
(4) Close CrystalClear. Turn off the power for all components. Shut down the system.
Shadow of the
suction pipe
Fig.12 Checking image
ON OFF
Cooling gas
alignment guide
Sample pin
Sample center
Fig.11 Adjust the position of cryogenic gas suction

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2012.02