Rigaku XtaLAB mini Manuel utilisateur

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.

This manual described in it may not be disclosed to a third party or copied, in whole or in part, without

the written consent of Rigaku Corporation.

In no event will Rigaku Corporation be responsible for the results of the use of this manual.

As a rule, one set of the instruction manual has to be purchased for each product.

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contact the sales representative who you purchased the instrument from for instruction manual

replacement.

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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

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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ME12973A

(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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ME12973A

(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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ME12973A

(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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ME12973A

(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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