Home

User Manual - Agilent Technologies

Contents

1. lt a 96 gt 4 37 gt q 75 gt oy el on oy p n g HAH ime y asi oy 4 E Figure 12 2 2 System and Component Dimensions Xcalibur Gemini Bena USER MANUAL Page 56 ADDITIONAL INFORMATION 12 2 2 Electrical Drawings Drawing no Title Number of pages EW 02 00 001 A KMW150CCD KMW200CCD ELECTRICAL BLOCK SCHEME 1 EC 02 01 001 A XCALIBUR GEMINI STEPPING MOTORS CABLE 2 EC 24 01 001 A XCALIBUR GEMINI ENCODERS CABLE 2 EC 01 02 001 A CCD POWER SUPPLY 230VAC SUPPLY CABLE 2 EW 03 02 001 A KMW3000C ELECTRICAL CONNECTION SCHEME 1 EC 04 02 001 A XCALIBUR GEMINI CCD POWER SUPPLY TO PC RS232 2 EC 02 05 001 B LCD MONITOR AND VIDEO MICROSCOPE POWER SUPPLY CABLE 2 EC 02 05 001 B LCD MONITOR AND VIDEO MICROSCOPE POWER SUPPLY CABLE 2 EC 24 08 001 A XCALIBUR GEMINI REMOTE CONTROL CABLE 2 EC 04 09 001 A XCALIBUR GEMINI INTERFACE RS232 CABLE 2 EC 04 02 002 A XCALIBUR GEMINI FIP60 TO INTERFACE CABLE 2 EC 01 09 002 A PC 230VAC SUPPLY CABLE 2 EC 04 02 003 B CCD DETECTOR TEMPERATURE AND COLLISION 2 EF 00 01 001 A XCALIBUR GEMINI FAN PANEL ELECTRICAL CONNECTION 1 EG 01 02 000 A ALL SYSTEMS INSTALLATION OD 1 04 01 CCD DETECTOR CONNECTIONS 1 OD 1 07 01 VIDEO MICROSCOPE KIT BLOCK DIAGRAM 1 OD 1 07 02 EC 05 05 002 B VIDEO MICROSCOPE TO BNC T ADAPTOR CABLE 1 OD 1 07 03 EC 05 05 001 B BNC T
2. ccccccscsscsssscsscsssssseeseesessecsesessessesaesessesansatsessnsaneaseess 16 Figure 4 1 3 View of Gemini diffractometer cccceccsssssssscsscsesscseeecseeecsesecseceesececsesacsesaesessacessusesensassesasensanes 17 Figure 4 1 4 Goniometer phi kappa omega and theta axe S ccccecessecessescesceecsecseseessessesseseeseeseeseneeneenss 18 Houre C 1 1 LOCATION OF SWINCICS esicirocninan rahn SAS 21 Figure 8 6 1 Goniometer Head AdjUStment c cccccccsssssscsscscescssercseeecsececseceeseceesesacsesaesessacesensesensassesasensanes 39 Figure 8 6 2 Video Microscope AdjUStMents cccccccescssescsscscsscseerssssecseeecseceesececsesacsesassesseessusesensatsesasnsanes 39 Figure 8 7 1 View of the access plate and pump out port of the Eos CCD detector eee 43 Figure 8 7 2 View of the pump out port of the Atlas Titan CCD detector ccc ceeesteseeeeeeeeen 43 Figure 12 2 1 Xcalibur Gemini Suggested Layout ccceesccesssssessesecsecseseceesesacsessesecsscessesesensassesasensanes 55 Figure 12 2 2 System and Component DIMENSIONS ccccccecescsscscesceecesceeeeseeseeceeeeseeseusessesnsanseseesensensaneess 56 Xcalibur Gemini Version 2 4 USER MANUAL Page viii HEALTH AND SAFETY INFORMATION 1 Health and Safety Information 1 1 General In normal operation the system is designed to operate safely All users of Xcalibur should be aware of potential hazards which exist in and around equipment of this type and the
3. ADAPTOR TO FRAME GRABBER CABLE 1 OD 1 07 04 EC 05 05 003 A BNC T ADAPTOR TO MONITOR CABLE 1 BCK 005 1 DETECTOR HEAD SUPPLY CABLE 1 BCK 006 1 DETECTOR HEAD COOLER CABLE 1 Xcalibur Gemini ele USER MANUAL Page 57 ADDITIONAL INFORMATION Gemini EG 01 00 013 A GEMINI ELECTRICAL PANEL EC 24 07 000 A GEMINI FRONT ELECTRICAL PANEL EC 24 07 010 A GEMINI FRONT PANEL EG 01 00 001 A GEMINI PCB CONNECTIONS EG 01 00 002 A GEMINI PCB CONNECTIONS EG 01 00 003 A GEMINI PCB CONNECTIONS EG 01 00 004 A GEMINI PCB CONNECTIONS EG 01 00 006 A GEMINI PCB CONNECTIONS EG 01 00 007 A GEMINI PCB CONNECTIONS EG 01 00 009 A GEMINI PCB CONNECTIONS EG 01 00 010 A GEMINI PCB CONNECTIONS EG 01 00 011 A GEMINI PCB CONNECTIONS EC 24 11 001 B GEMINI PROTECTION CABINET SENSORS EG 01 00 005 A GEMINI WARNING LAMPS EG 01 00 012 A GEMINI WATER PANEL Xcalibur Gemini ana USER MANUAL Page 58 ADDITIONAL INFORMATION Appendices Appendix 1 X ray Tubes Wavelengths 1 540598 2 1 544426 2 1 39225 1 1 00248 0 0 7093187 4 0 713609 6 0 632305 9 1 00605 Appendix 2 Standard Crystal Parameters Compound name Ylid 2 Dimethylsulfuranylidene 1 3 indandione Compound formula C11H10802 Cell constants a 5 947 a B y 90 b 9 026 A c 18 399 A Appendix 3 Temperature Scales Conversion To convert Fahrenheit to Celsius subtract 32 from F then multiply by C 5 9 F 32 5 9 To convert Celsius to Fahrenheit multiply
4. Version 2 4 September 2011 Agilent Technologies XRD Products 10 Mead Road Yarnton Oxfordshire 0X5 10U UK Tel 44 0 1865 291600 Fax 44 0 1865 291601 http www agilent com chem a Agilent Technologies Xcalibur Gemini including Ultra Single Crystal Diffractometers User Manual Notices Agilent Technologies Inc 2011 No part of this manual may be reproduced in any form or by any means including electronic storage and retrieval or translation into a foreign language without prior agreement and written consent from Agilent Technologies Inc as governed by United States and international copyright laws For Assistance and Support http www agilent com find assist Limitation of Warranty The foregoing warranty shall not apply to defects resulting from improper or inadequate maintenance by Buyer Buyer supplied software or interfacing unauthorized modification or misuse operation outside of the environmental specifications for the product or improper site preparation or maintenance No other warranty is expressed or implied Agilent Technologies specifically disclaims the implied warranties of Merchantability and Fitness for a Particular Purpose Warranty The material contained in this document is provided as is and is subject to being changed without notice in future editions Further to the maximum extent permitted by applicable law Agilent disclaims all warranties either
5. Do not operate the instrument in the presence of flammable gases or fumes Do Not Remove the Instrument Cover Operating personnel must not remove instrument covers Component replacement and internal adjustments must be made only by qualified personnel Instruments that appear damaged or defective should be made inoperative and secured against unintended operation until they can be repaired by qualified service personnel Environmental Information This product complies with the WEEE Directive 2002 96 EC marketing requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Do not dispose in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com environment product for more information Important Information This user manual applies to the Xcalibur systems manufactured in Poland by Agilent Technologies Product Xcalibur or Gemini Model X ray source ENHANCE and or ULTRA Configuration Detector Eos Atlas or Titan Electrical Ratings 1 N AC 230 V 50 60 Hz 4200 Watts Before attempting to operate the system PLEASE READ THE INSTRUCTIONS This product should only be used by persons legally permitted to do so If the equipment is used in a manner not specified in the User Manual the protection provided by the equipment may be impaired Important Health and Safety Notice W
6. Do not unpack the equipment until Agilent Technologies personnel are on site 4 Always lift packing cases from the bottom using suitable lifting equipment refer to list of component weights in the following section 5 Move packing cases into the designated installation site 6 Contact Agilent Technologies to notify them that the equipment is awaiting installation by a factory trained service representative 5 1 2 Unpacking 1 Retain all packing material until installation of the system is completed 2 Ensure that special tools are stored safely for use during maintenance periods Xcalibur Gemini ana USER MANUAL Page 20 HANDLING INSTALLATION STORAGE AND TRANSIT INFORMATION 5 1 3 Mechanical Handling 5 1 3 1 Weights Dimensions and Lifting Points Description NET Weight kg Kappa 106 goniometer X ray generator 40 Enclosure 90 Electronics 60 rack KMW200CCD 19 KMW3000C 56 Helijet 10 Cryojet 15 Autofill 5 controller ILM210 Helijet 5 controller ITC502 Helijet gas 12 flow controller GFC1 Xcalibur Gemini USER MANUAL Dimensions width x height x depth cm 43 x 64 x 47 A8 x 22 x 69 115 x 100 x 100 80 x 85 x 80 60 x 10 x 37 38 x 54 x 96 30 x 25 x 10 head only 15 x 35 x 15 head only 44x 10x 30 44x 10x 30 45 x 26 x 38 Centre of gravity Offset from centre of unit towards side of X ray tube mount Centre of unit N A Centre of unit
7. Refer to the third party ThermoNESLAB manual for information about this equipment if supplied Xcalibur Gemini USER MANUAL Version 2 4 Page 24 HANDLING INSTALLATION STORAGE AND TRANSIT INFORMATION 5 2 1 5 Low Temperature Option A suitable high vacuum pump ideally 70 Litres sec turbo is required to periodically evacuate the Cryojet head and the heater leg A KF16 fitting is required for this procedure To demonstrate the operation of the Cryojet 100 litres of liquid nitrogen are required The customer should supply a suitable table rack for both the ILM and the Cryojet controller 5 2 1 6 CCD Camera Pumping A high vacuum pump is required to periodically evacuate the CCD camera 5 2 1 7 Helijet Option The customer should provide a minimum of 50 litres of liquid helium and a minimum of 1 full helium gas cylinder of at least 99 99 grade helium gas in order for the operation of the Helijet to be demonstrated 5 2 2 Setting to Work 5 2 2 1 Equipment Required e Table for computer for integration with system e 1 set of Allen keys e Phillips screw drivers assorted sizes e Flat headed screw drivers assorted sizes 5 2 2 2 Personnel Required for Installation 5 persons for lifting of heavy components 5 2 2 3 Setting up Procedures Agilent Technologies personnel normally perform installation The duration of the installation is typically 4 working days to include assembly testing maintenance and s
8. oO NY O O A Q N Using the weekly maintenance sheet see appendix Record the date persons testing and sign off the outcome 8 8 Checking the Emergency stop Task Time 10 minutes When Once a month Tools None Procedure 1 With the diffractometer running at minimum settings for example 28 kV 1 mA press the red Emergency Stop button 2 The X ray generator should switch off immediately release the emergency stop button by twisting anti clockwise restart the X ray generator Return the generator X ray tube to required settings 3 Switch off the interface wait 5 seconds restart the interface and then in the Service Power Tool of CrysAlis r click on the radio button gon reinit and click Start 4 Using the monthly maintenance schedule see appendix record details of the test stipulating the date person testing outcome and signature Xcalibur Gemini ana USER MANUAL Page 41 MAINTENANCE INSTRUCTIONS 8 9 Checking the X ray Radiation Levels Task Time 20 minutes When Once a month Tools Appropriate Radiation meter for X ray energy levels Mo14 keV Cu 8 keV Procedure 1 With the X ray generator on at normal operational settings and the shutter closed use the radiation meter to sweep the area inside the cabinet and around the X ray tube housing fast shutter and collimator for any radiation leak 2 Close the protective enclosure doors and open the X ray shutter In the Service Power Tool of CrysAlis r
9. FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met Safety Summary General Safety Precautions The following general safety precautions must be observed during all phases of operation of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies Inc assumes no liability for the customer s failure to comply with these requirements Before operation review the instrument and manual for safety markings and instructions You must follow these to ensure Safe operation and
10. Outside top right of the protective enclosure X ray Mo generator power is X ray Mo on Orange light Outside top right of the protective enclosure X ray Cu generator power Is X ray Cu on Red light Shutter Outside top right of the protective enclosure X ray shutter open open Green Light Outside top right of the protective enclosure X ray shutter closed Shutter closed Red light only on Back light of flow gauge inside front right of He gas flow out of range systems fitted electronics rack through gauge X ray interlock with Ultra IS open Green light only Back light of flow gauge inside front right of He gas flow is within range on systems fitted electronics rack through gauge X ray interlock with Ultra is closed Red light Shutter Inside top protective cabinet on beamstop X ray shutter is open open Support near X ray shutter 6 2 System Start Up Safety devices in the diffractometer protect against damage to the system and the operator during start up The following initial switch on procedure should be followed 1 Plug in all mains power cords to their wall mounted sockets system computer monitor 2 Switch on KMW200CCD chiller using the power switch on the front panel open the front door of the electrical rack to access 3 Wait for the chiller to start up The error state lights on the front panel will flash three times when the chiller is ready Then check that the detector power supply box is switched
11. and green shutter lights The door of the cabinet should remain locked when the system is unattended to prevent unauthorised access to the system Xcalibur Gemini ana USER MANUAL Page 19 HANDLING INSTALLATION STORAGE AND TRANSIT INFORMATION 5 Handling Installation Storage and Transit Information 5 1 Reception and Handling 5 1 1 Delivery Carry out the following steps on delivery of the Xcalibur system 1 When the system arrives check that there is no visible damage with the delivery driver present lf damage has occurred contact the carrier and Agilent Technologies immediately 2 Check that shock watch and tilt indicators fitted to the outside of the packing cases have not been activated If the indicators have been activated notify Agilent Technologies immediately 3 Check the number of delivered boxes crates against the packing list If any items are missing contact Agilent Technologies within 3 days WARNING The packing crates are heavy and could cause serious injury and damage to the equipment if not handled correctly Use suitable lifting equipment and procedures Only lift the packing cases from the bottom CAUTION Do not remove the equipment from the packing crates until they have been moved to their designated installation site The equipment has been carefully packed to protect the equipment from damage in transit Removal of the packing equipment could make the equipment vulnerable to damage during transit
12. if the power supply voltage fluctuates more than 10 Locate the mains outlet on the wall behind the system The mains outlet should be of the circuit breaker type Outlet and connecting plugs are not supplied The mains plug should be readily accessible by the operator when the equipment has been installed In areas where the mains power supply is unreliable an uninterruptible power supply UPS is recommended The UPS should have specifications of 10 kVA with 3 phase input and single phase output For example the following unit from APC will run Xcalibur Gemini from a 400V 3 phase input for about 100 minutes APC Smart UPS VT 10kVA 400V w 3 Batt Mod Exp to 4 Start Up 5X8 Int Maint Bypass Parallel Capable 1 SYBT4 Battery Unit Xcalibur Gemini ama USER MANUAL Page 23 HANDLING INSTALLATION STORAGE AND TRANSIT INFORMATION Description X ray generator s CCD detector KMW200CCD cooler Goniometer Interface Cabinet lights sample illumination Computer and peripherals Cryojet controller option Autofill controller option KMW3000C Cooler Thermo chiller option Voltage V 1 N AC 230 10 90 130 180 260 100 240 90 130 180 260 1 N AC 230 10 100 240 100 240 100 230 1 N AC 230 10 208 240 Frequency Hz 50 60 50 60 50 60 50 60 50 60 50 60 50 60 50 60 50 60 50 60 Maximum nominal mains current A 24 2 5 2 5 2 5 2 5 2 5 2 0 6 5 2 1 4 Water Supp
13. on red lamp lights on the top 4 Allow 60 90 minutes for the CCD detector to cool the Peltier and chip to 40 C 5 Turn on the interface using the red switch located on the left hand side of the interface front panel On the MGC model ensure 4 green LEDs are illuminated on the right hand side of the interface panel These lights are labeled Power EXT I 0 Ready and Enable On the DC08 model wait 15 seconds for the LEDs to self test and then ensure 2 green LEDs are illuminated these are labeled Power and Ext Supply 6 Turn on the computer monitor 7 Switch on the PC and launch the CrysAlis e programme The goniometer should auto initialise If you have the interface DC08 model then the front panel green LED Goniometer Ready should light Xcalibur Gemini ama USER MANUAL Page 28 OPERATION 8 Switch on the KMW3000C chiller using the key provided Ensure that the external circuit water cooling is also turned on 9 Turn on the X ray generator switch on the generator back panel 10 To generate X rays open the X ray device server in the Crysalis re GUI Click on start and enter 28 kV 1 mA then press OK The generator should now ramp up to these settings If the X ray tube has not been running for gt 1 hour follow the warm up procedure suggested in the manufacturers manual 11 After closing all protection cabinet panels the system will enable the X ray shutter interlock to allow it to be opened after a com
14. until the set temperature is obtained Xcalibur Gemini ana USER MANUAL Page 44 9 Trouble Shooting TROUBLE SHOOTING 1 Shutter is not enabled X ray shutter will not open resulting in blank images in the software 2 Protective cabinet doors are not closed properly 3 Shutter open and or shutter closed lights defective 4 Protective cabinet doors were opened whilst the shutter was open and safety circuit was activated 5 X ray generator is turned off 6 Shutter signal cable Xcalibur Gemini USER MANUAL If you have interface model DC08 open front door of electrical rack and look for Shutter Enable green LED illuminated on front panel If it is not then proceed with the checks below Close doors properly If the interface is model DC08 then the front panel will show the green LED Shutter Enable Otherwise if the safety circuit is closed a green lamp is illuminated within the control electronics Access is via the left side panel of the electronics cabinet Check light connections and LED light display To check if LED arrays are working turn off the interface wait 5 seconds and turn back on the interface For a short period all shutter indicators should be illuminated i e open closed on the exterior of the cabinet and the Shutter Open red lamp inside the cabinet on the beamstop mounting In CrysAlis ro re start experiment Turn on X ray generator and start high voltage Ens
15. Authorised Operator 4 5 hours 2 CCD detector pump out Authorised Operator 30 minutes vacuum 7 6 10 000 Hours Maintenance Schedule Tools and Materials Set of Allen keys Set of flat headed screwdrivers Water receptacle e g Bucket Special tools special tool 1 and special tool 2 see section 8 for identification Xcalibur Gemini USER MANUAL Estimated elapsed time 4 5 hours 1 hour Estimated elapsed time 4 4 hours 3 6 hours depending on detector Version 2 4 Page 32 MAINTENANCE SCHEDULES Action Personnel Estimated task Estimated elapsed duration time 1 Changing the X ray tube Authorised Operator 30 minutes 30 minutes 2 Alignment of X ray optics Authorised Operator 2 hours 2 hours Xcalibur Gemini Hna USER MANUAL Page 33 MAINTENANCE INSTRUCTIONS 8 Maintenance Instructions AN 1 Read and understand the Health and Safety Information section of this manual before performing any maintenance procedures 2 Follow any local national or international rules and guidelines that apply to this equipment when performing maintenance tasks 3 Maintenance tasks must only be performed by authorised operators of the diffactometer Some procedures in this section require that commands are entered in the command line To open the command line 1 Launch Crysalis re 2 Click on the command line icon on the left hand side tool bar 8 1 Refining the Machine Para
16. ID Analogue to digital resolution True 18 bit System noise so called read noise lt 10 e RMS Dark current lt 0 05 e pix s Communication Gigabit Ethernet Pixel Sampling rate 5 6 MHz Readout time complete duty cycle including 0 22s 4 x 4 binning chip readout CDS analogue to digital 0 46s 2 x 2 binning conversion transfer detector PC disk storage 1 59s 1 x 1 binning Xcalibur Gemini amd USER MANUAL Page 10 SPECIFICATIONS 3 3 2 2 Eos CCD Detector Active area 90 92 mm diagonal Overall dimensions L x W x H 218 X 178 X 234 MM Pixel size on scintillator 31 um Scintillator material Gadox Fibre optic reduction 1 3 1 low distortion reduction taper 3 3 2 3 Atlas CCD Detector Active area 135 mm diagonal Overall dimensions L x W x H 243 X 178 X 234 MM Weight 16 kg Pixel size on scintillator 48 um Fibre optic reduction 2 1 low distortion reduction taper 3 3 2 4 Titan CCD Detector Active area 165 mm diagonal Overall dimensions L x W x H 262 x 192 x 241 MM Weight 20 kg Pixel size on scintillator 60 um Fibre optic reduction 2 5 1 low distortion reduction taper 3 3 2 5 PC CCD Interface Communication Gigabit Ethernet Drivers WinXP Typical host computer Intel Core 2 Duo class PC gt 2 GHz gt 1 0 Gb RAM 20 colour display Xcalibur Gemini ana USER MANUAL Page 11 SPECIFICATIONS 3 3 2 0 CCD Detector Maximum Theta and Resolution Eos on Xcalibur Maximum r
17. Just before home this flag will display 0 for about 2mm and when it changes back to 1 you should stop since this is home co Select Hsync all and click Start Note that at the end of the Hsync operation the Hsync flags should read 1 This is located on the text line below the parameter button Click on OK 9 Select gon reinit and start in the service power tool This will reinitialise all axes and leave the goniometer in its home position ready for operation Version 2 4 Page 50 TROUBLE SHOOTING 3 Emergency stop button pressed Eos Atlas Titan 1 Communication errors on Strange artefacts on Ethernet link between CCD and CCD images lines PC blocks chequer board Xcalibur Gemini USER MANUAL Release the emergency stop button by twisting clockwise and follow the instructions on the PC screen Power off interface wait 5 seconds and then power on Open service power tool select gon reinit and start in CrysAlis re This will reinitialise all drives and return the goniometer to the position it was at when the emergency stop button was pressed 1 Reset the CCD detector by switching off the Water Cooler power on the front panel waiting 10s and restarting 2 Check that the Ethernet link restarts shortly afterwards by checking Windows icon bar 3 Close and restart Crysalis r Version 2 4 Page 51 SPARES 10 Spares 10 1 Fuses ee P
18. MAINTENANCE INSTRUCTIONS CAUTION Failure to fit these o rings will result in water leakage which could damage both the X ray tube and the instrument 9 Fitting the new tube is the reverse procedure maintaining the same orientation of the tube 10 For disposal of used X ray tubes see the DISPOSAL chapter of this manual 11 Holding by its metal base remove the new X ray tube from Its protective box Ensure that the X ray tube is correctly mounted Incorrect mounting may result in exposure of personnel to X ray radiation 12 Slide the X ray tube into position on the diffractometer and secure with two screws 13 Fit the end cap with integral temperature sensor onto the top of Enhance and secure using the two fixing screws 14 Re fit the plate for mounting cryogenic devices 15 Re fit any cryogenic device 16 Switch on KMW3000C water chiller 8 4 Changing the Collimator of Enhance Task Time lt 1 min When Different sizes of collimator may be necessary for different experiments Three standard collimators of sizes 0 5 0 8 and 1 0 mm are provided with the diffractometer system A 0 3 mm standard length collimator and a short 0 3 and 0 5 mm collimator for use in high pressure experiments are available by special order Different lengths of collimator are used for Mo and Cu sources the longer collimators are for the Mo source Tools None Procedure 1 Ensure that the X ray shutter is closed and all interlocks a
19. Page 63
20. Right hand side of unit Centre of unit Centre of component parts Centre of component parts Centre of unit Centre of unit Centre of unit Lifting points At four corners DO NOT lift from below From the sides and below N A By hand from top four corners otherwise from below Underneath at the four corners At the four corners and from below From below with transfer tube removed From below or using handles whilst Supporting transfer tube By hand from below By hand from below Front panel handles Version 2 4 Page 21 HANDLING INSTALLATION STORAGE AND TRANSIT INFORMATION 5 1 3 2 Boxed Weights Dimensions and Lifting Points on Delivery Width Height Weight kgs cm cm Goniometer Protection cabinet Electronics rack Helijet option KMW3000C Chiller Eos CCD detector Atlas CCD detector Titan CCD detector 160L LN2 dewar option 21 LCD TFT Monitor Cryojet option X ray generator X ray generator for Gemini The weights and dimension above are an estimate and should only act as an indication of the lifting requirements when the system is delivered All boxes are fitted with the facility to use forks to unload There is 15 cm clearance from floor to the base of each box It is recommended that a fork lift truck is available to unload the delivery vehicle with a pallet truck to move the packing cases into the systems final location 5 2 Installation and Setting to
21. Work 5 2 1 Preparation of Site and Services 5 2 1 1 Environmental Requirements It is the customer s responsibility to ensure that all local building and safety regulations are met Ensure that the environmental conditions of the installation site conform to the requirements stated in the SPECIFICATIONS section of this manual Xcalibur Gemini ama USER MANUAL Page 22 HANDLING INSTALLATION STORAGE AND TRANSIT INFORMATION 5 2 1 2 System Layout Adequate space is required around the system for servicing The minimum clearance from the walls and a suggested system layout are shown in drawing number OD 01 00 15 When the low temperature option is fitted an extra 100 cm space on the left hand side of the system is required Unpacked the largest subassembly will fit through a door aperture of 85 cm Check the door aperture to ensure the system can be assembled in its designated area 5 2 1 3 Electrical Services A 3 phase 63 A supply with one or two 32 A outlets for X ray generator one for Xcalibur or two for Gemini and one 16 A outlet is required Additionally four single phase outlets are required as described in drawing OD 01 00 015 C Use only the power cables supplied Do not connect the electrical power supply circuit to any other devices Limit the electrical noise in the system by attaching the earth cable exclusively to a system earth terminal with a resistance of less than 0 5 ohms Fit a line voltage regulator
22. ator and System X ray Generator System Power connection 1 N AC 230 V10 1 N AC 230 V 10 50 60 Hz 50 60 Hz Maximum mains current at 230V 19A 4A Power outlet fuse Xcalibur Gemini ana USER MANUAL Page 14 TECHNICAL DESCRIPTION 4 Technical Description 4 1 Overview of Xcalibur Gemini The Xcalibur Gemini system consists of 1 A kappa geometry 4 circle diffractometer 2 ACCD area detector 3 An instrument cabinet with electronics rack 4 A stand for optional equipment like high or low temperature attachments 5 System software installed on PC workstation 6 A water chiller for the X ray tube type KMW3000C Note The numbers on this diagram refer to the numbered list above Figure 4 1 1 Components of a typical Xcalibur Gemini system The diffractometer and CCD area detector are mounted inside a cabinet The cabinet experiment area is mounted on top of the electronics rack Water chillers for the CCD detector and the X ray generator are positioned to the side of the instrument The PC workstation is located close to the instrument to allow a clear view of the diffractometer and convenient access to it Xcalibur Gemini Version 2 4 USER MANUAL Page 15 TECHNICAL DESCRIPTION The diffractometer consists of an X ray tube a 4 axis Kappa goniometer omega kappa phi and theta axis for sample orientation with a detector arm which has a universal mount capable of supporting any Agilent Technologies CCD area detec
23. bled the Goniometer sample centre and the video microscope focal point should be close to each other however the video image only displays a field of view approximately 1 2mm x 0 8mm and its depth of field is similarly limited Adjustments need to be made so that the sample centre and microscope focal point coincide exactly Both the Goniometer head and the video microscope have adjustments to move their centres in three planes Agilent Technologies supply a pre mounted 0 3mm steel ball to aid this procedure The three adjustments for the microscope can be seen in the figure above Video Microscope Adjustments Xcalibur Gemini Version 2 4 USER MANUAL Page 39 MAINTENANCE INSTRUCTIONS To centre the video microscope and therefore the steel ball on the centre of the video image use the following procedure Procedure 1 Within the CrysAlis software press F12 on the computer keyboard to release control of the goniometer to the remote control pad Mount the 0 3mm steel ball plus goniomenter head onto the goniometer Press the Lower then 0 keys and wait for the goniometer to stop moving Adjust the goniometer head such that the steel ball is visible on the video image oN ge eer TS Press 180 and watch the steel ball as it is rotated it will probably move off image Use the adjustments on both the Head and Microscope equally to move the ball back to the centre press 0 The ball should end up close to the
24. by 9 5 then add 32 F 9 5C 32 To convert Celsius to Kelvin add 273 15 K C 273 15 To convert Fahrenheit to Kelvin first convert F to C then add 273 15 Xcalibur Gemini Version 24 USER MANUAL Page 59 ADDITIONAL INFORMATION Appendix 4 Maintenance Records The attached record sheets are provided as examples of the type of records of maintenance checks that should be completed for Xcalibur Gemini These records are to show only that maintenance has been completed as directed in this manual Other maintenance records should be kept as required by any local national or international regulations Weekly Maintenance Record Sheet Date of Name of person performing maintenance test Xcalibur Gemini Version 2 4 USER MANUAL Page 60 ADDITIONAL INFORMATION Weekly Maintenance Record Sheet Date of Name of person performing maintenance test el o o o S S Xcalibur Gemini Version 2 4 USER MANUAL Page 61 ADDITIONAL INFORMATION Weekly Maintenance Record Sheet Date of Name of person performing maintenance Date of Name of person Emergency X ray radiation maintenance performing test Stop Check check OK OK Y N Xcalibur Gemini Version 2 4 USER MANUAL Page 62 ADDITIONAL INFORMATION Date of Name of person maintenance performing test Yearly Maintenance Record Sheet Date of Name of person Machine CCD detector maintenance performing test parameter file vacuum refined pumped Xcalibur Gemini Version 2 4 USER MANUAL
25. cal guide to the system and Its operation This is intended to familiarise the user with how the system works and provide a better understanding of the system operation All personnel who are likely to operate the system or who are likely to come into contact with any of the system components should read the HEALTH AND SAFETY INFORMATION section of the manual This provides basic information aimed at highlighting the safety hazards associated with the equipment More detailed information and instructions for component parts of the system are given in the third party manuals supplied with the system which are listed in this manual These manuals should also be read and understood before operating the system The purpose of this manual is to e explain how to operate the equipment e explain how to interface to the equipment e list performance characteristics of the equipment e describe how the equipment operates e assist with simple fault finding and maintenance 2 3 System Overview The Xcalibur series are single crystal diffractometers that use the property of X ray diffraction to determine the crystal structure of materials They are intended for use with single crystals of chemical substances inorganic organic or organo metallic mineralogical and biological samples The Xcalibur may also be used in the analysis of powder samples Intended samples should have a maximum unit cell dimension of 100 Angstrom in any direction for small molec
26. ceecsesecsecessusecsesassesaesesseeessncesensassesasnsanes 42 9 Trouble Shooting cccsecessseeesseeesseeeessseeessseeeesseeeeaseeessseeesesseeseasseeesseeesneeeees 45 10 OUD AN SS was rss cece acae cers taseaciese acces cacertash ance eaananeasvakiececanee acted vanes auneseonvaneceanameaeastaevendeue 52 IC Fat Sy 2S en Pi ne RE le ee PR eee ee REE PER Cree POE Pee Pere et RrE Per Mer ree Beer 52 TOZ AI IID Sc se ce ceceeere eae pie dec case se castace cepa cetactapartada cls tattetartosatasectetetade ct atetectecatatactvetacectsetatecececaiectstetecectsuanetedeeatadeesenetans 52 11 Disposal INStructiOns cccccssessssssesessssseeesssseeeeeessseesesssseeeseesseseeneeneeseees 53 EAX tay Tube and CCD Detector etsitcieaitci esi ie telat edhe a eaiaieaaai ad 53 EA Thid Farny Equip mem ee 77 OBO Oo 53 12 Additional Information s sassuunnnnunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnns 54 494 pL 8 Pary Nirma 1919 9 Per mre meer Pm ne en aaa ea 54 122 DAWID S renee nE TenneT ENA ETUNA EENET OEO 55 Mechanical DANNOS e aed 55 Xcalibur Gemini Version 2 4 USER MANUAL Page vii 12 2 2 Electrical Drawings cccccceccsscssscesscsceecsececsucecsesacsesaesessasessucessusacsesaasesansesensassesaeeesaneetensaseneass 57 Table of Figures Figure 4 1 1 Components of a typical Xcalibur Gemini system ssseeseisisisisiriririrererrrrrrrersrsrssrsrsrnnnn 15 Figure 4 1 2 View of Xcalibur Ultra diffractometer
27. centre of the image adjust again to make it central repeat as necessary until the movement of the ball is minimised 6 Press 90 and move the ball to the centre using the head only 7 Press 270 and watch the ball as it rotates If the microscope is correctly centred left to right it will be possible to centre the ball using only the Head adjustments if not small adjustments of the microscope may be required repeat until the ball appears to spin on the spot for all four angle positions 8 Press 0 then Upper watching the ball as it moves Use the height adjustments on both the Head and the microscope equally to re centre the ball press Lower and repeat step 8 until there is no movement of the ball as the goniometer moves between the two positions 9 Repeat steps 5 to 7 at the Upper position 10 Adjust the focus on the microscope to bring the ball into sharp focus The video microscope Is now aligned The video microscope should not need to be adjusted again unless it is knocked or extra weight is added to or removed from the support arm for example a low temperature device is added or removed NOTES An indication that the video microscope is not properly centred is if the sample cannot be centred to the middle of the video image then small adjustments of the microscope may be needed during the sample centring process The focus may also need adjusting occasionally if the Crystal size varies wid
28. click on Shutter Open 3 Sweep the outside of the enclosure using the radiation meter paying particular attention to the plane of the X ray tube the area of the secondary beam stop mounted on the right hand side enclosure window and the door seals 4 Close the X ray shutter by clicking on the Shutter Close button in the Service Power Tool 5 Using the monthly maintenance schedule log record details of the test stipulating the date person testing outcome and signature 8 10 CCD Detector Pumping Out Vacuum Task Time 3 hours When Once a year Tools Special T tool carried by Agilent Technologies service engineer 1 set of Allen keys Rotary vacuum pump capable of obtaining a pressure of 1x10 mbar Vacuum tubing and adaptor Procedure 1 Switch off the cooling water for the CCD detector at the cooler chiller unit 2 Allow one hour for the detector to warm to room temperature 3 For the Eos detector unscrew front four corners of the collision sensor of the CCD detector This is spring loaded so be ready to catch it as you release the screws Remove the front of the CCD detector Xcalibur Gemini ama USER MANUAL Page 42 MAINTENANCE INSTRUCTIONS i i JA Pump out port with T tool Set screws E N attached Figure 8 7 1 View of the access plate and pump out port of the Eos CCD detector 4 For the Atlas or Titan detector unscrew the cap from the p
29. e performed without endangering any persons safety 6 5 1 Emergency Shutdown Procedure AN The emergency stop button will only shut down high voltage from the X ray generator Other equipment on the system will still be powered on 1 Press the red emergency stop button located on the front left of the system 2 Switch off all power at the mains electrical supply 3 Turn off mains water supply Xcalibur Gemini Bena USER MANUAL Page 30 MAINTENANCE SCHEDULES 7 Maintenance Schedules 7 1 Introduction Various maintenance tasks must be performed to ensure that the diffractometer system continues to operate safely and reliably These tasks are detailed in the maintenance schedules given below CAUTION 1 Maintenance tasks must only be carried out by authorised operators who have undergone specialist radiation training Refer to local rules for further details 2 Failure to perform scheduled maintenance tasks properly and at the correct intervals can affect the safety and performance of this system 3 Before performing any maintenance task ensure that you have read and understood the HEALTH AND SAFETY INFORMATION at the beginning of this manual and any local rules governing the use of the diffractometer system Planned maintenance that can be performed by the user is limited to replacing consumable items alignment procedures pump down procedures and checking radiation levels and safety features The users authori
30. e temperature is too high 6 X ray lamp on cabinet is defective 7 Additional X ray lamp is defective 1 RS232 communication cable not connected properly Problem reading kV and mA from generator 2 Check PC serial port is working Xcalibur Gemini USER MANUAL 1 Check KMW3000C water cooler is switched on 2 Check water cooler has no error state 3 Check all necessary water valves are open 4 Check external cooling water supply is flowing and has an acceptable temperature There is a temperature switch on the top of the X ray tube If it is hot then wait for it to cool down Investigate the reason for overheating of the X ray tube before proceeding Check light connections and LED light display some laboratory installations have an additional X ray lamp in the interlock circuit This might be wall mounted near to the system or outside the laboratory Check the lamp connections and the replace the bulb with the same type if necessary Check the RS232 cable is connected to back of PC serial COM port and to back of the generator CrysAlis e should search through all available serial ports Version 2 4 Page 47 TROUBLE SHOOTING Software cannot No communication with interface Check interface is switched control goniometer on For interface model MGC Check RS232 serial cable is connected between rear of PC and the interface For interface model DC08 Check Ethernet cable is connected be
31. ely from one experiment to another For a correctly centred sample and video microscope the variation in position of the sample Sphere of Confusion as it rotates to any of the positions on the remote control except home should be one small division on the image 10pm In the unlikely event that correct centring cannot be achieved contact Agilent Technologies for advice 11 When fully centred in the Upper and Lower positions the goniometer should be sent back to Home once this is complete the ball or Crystal will appear to be displaced towards the left of the video image This is an optical illusion caused by the angle of the microscope with respect to the Crystal at Home and can be ignored Xcalibur Gemini ana USER MANUAL Page 40 MAINTENANCE INSTRUCTIONS 8 7 Checking the Door Safety Interlocks Task Time 2 minutes When Once a week Tools None Procedure 1 With the diffractometer in normal operation and at normal X ray generator settings open the shutter using the shutter open button in the Service Power Tool of the CrysAlis software Open the front doors of the enclosure cabinet The X ray shutter should immediately close Close the enclosure doors Repeat step 1 and open the side panels of the cabinet The X ray shutter should immediately close Close the side panels Repeat step 1 and open the back panels of the cabinet X ray shutter should immediately close Close the back panels
32. ended Precautions cccccccccccscsscsscssesscsscesceseessesseseessesseseeseeseeseeseeseeseeseeseesensensensenees 2 EES 2 0 E eR ne en ee 3 1 3 Mechanical Handling Satety cccccessssssssssscsscscsscscsscsesessecscsececsscecsesacsesansesaesessecessusessesassesateesaneesenees 3 1 4 Safe Mechanical Practice sskctececedocactscedutecutadlecedssadcaceagcesedudasetadudadetedudes esaddadetacedasledadstadstacetatesedecadetadstadetededs 3 ES Moving Falls erasian a a aaia aaa a 4 LO Exireme VOT Clea OS asniensis S 4 1 7 X ray RACGATION ccccceccescsscsecsecsecsecsecsessessecsesensseceuconssuseusensenseusenseeseusensensenseusensensensenseeseuseuseusnsensensensenees 4 EON aC UUN r A A 5 1 9 High POSS UES dicsccsadacacsuanacteneddeondsaptnwcstandovndtandenadddndeupetundauactondiaartoctsandaapiasndtupiannetuatuanetiasnonmaadnundtantassdaundds 5 1 10 Hazardous or Toxic Materials won ccc ccsccsccsccsscsssesseescseseeseesceuseuseeseesseuseuseesceaseuseesseuseusensenseeusanses 6 1 17 Maintenance AE 6 2 introduction cioa a a aae eaae a aa a aa aaa Ta Raia 7 DMs GOP A PEREA ATEA AA IATER EEEE AA PEENE A PEE E PA EE P EE PE EEE a E EE E E EATE A A E E EE 1 2 2 How To Use This Mantl c ccc ccc cc ccccccsccsscsscsscsscsseeseeseesseseeseeseeseeseeseeseeseeseeseeseeseeseesenseesensnsensenseneenss 7 2 3 SVS temi OVE ere ee Re ne ee eee eee 7 3 Specifications a sseisiscesnacinecteniancuintsacausnsansesansnesacevsaneinandatesaevaansdacaseusaunwaestaa
33. ersonnel are not required to undertake mechanical work However servicing or repair may necessitate access to any part of the system Only personnel who have been trained by Agilent Technologies to carry out service work on this equipment should attempt to dismantle modify or repair the equipment Water connections should be made and tested in accordance with any local and national safety regulations Xcalibur Gemini Version 2 4 USER MANUAL Page 3 HEALTH AND SAFETY INFORMATION 1 5 Moving Parts There are a number of moving parts in the system which are powered by electric motors Injury could result if clothing or body parts become caught in moving mechanisms Keep clothing hands and body parts away from moving mechanisms es WARNING Between the moving parts of the goniometer there are a number of places at which a potential finger squeeze or shearing hazard exists The warning triangle shown to the left is visible on the goniometer close to these places Keep hands away from the goniometer when parts are moving 1 6 Extreme Temperatures A N WARNING 1 Systems fitted with the low temperature option use liquid nitrogen and or liquid helium as a coolant Liquid nitrogen and liquid helium are cryogenic liquids and can cause cold burns Wear gloves when handling cryogenic liquids and use eye protection Refer to the information supplied with the equipment for more information During operation both the X ray tube and the heat
34. esolution in 2 theta Maximum resolution tn d value Eos on Gemini Maximum resolution in 2 theta Maximum resolution tn d value Eos on Gemini Ultra Maximum resolution in 2 theta Maximum resolution tn d value Atlas on Xcalibur Maximum resolution in 2 theta Maximum resolution tn d value Atlas on Gemini Maximum resolution in 2 theta Maximum resolution tn d value Xcalibur Gemini cine USER MANUAL Page 12 Atlas on Gemini Ultra Maximum resolution in 2 theta Maximum resolution tn d value SPECIFICATIONS Titan on Xcalibur Maximum resolution in 2 theta Maximum resolution tn d value Titan on Gemini Maximum resolution in 2 theta Maximum resolution tn d value Titan on Gemini Ultra Maximum resolution in 2 theta Maximum resolution tn d value 3 3 2 CCD Detector Maximum Distance CCD detector to sample distance 42 to 150 mm Eos detector 52 to 150 mm Atlas detector 62 to 150 mm Titan detector Xcalibur Gemini USER MANUAL Version 2 4 Page 13 SPECIFICATIONS 3 3 3 Four circle Kappa Geometry X ray Goniometer Type Four circle Kappa geometry X ray goniometer Sphere of omega kappa phi axes 10 um coincidence Maximum load Phi axis 2 kg Reproducibility 0 00125 deg for Omega and Theta 0 0025 deg for Kappa 0 005 deg for Phi Scanning speed range 0 005 to 3 0 deg sec X ray shutter response time 3 ms 3 4 Electrical Data X ray Gener
35. etector head The data is then transferred via a gigabit Ethernet data link to the PC workstation The control program stores it for further analysis to the hard disk The four axis goniometer is driven by microprocessor controlled stepping motors with 12 800 microsteps per revolution The sample is aligned using a video microscope The sample picture is displayed on the control computer by using the built in frame grabber The cabinet halogen lighting provides brilliant high contrast illumination of the sample at all goniometer positions Optionally a fibre optic halogen flood light system can be ordered to provide additional lighting focussed onto the sample The X ray generator is located in the electronics rack in the instrument cabinet The generator power trips out if the X ray tube overheats and warning lights on the front panel indicate the operational status of the generator The generator is controlled remotely using Crysalis software Gemini systems contain two generators Xcalibur Gemini Version 2 4 USER MANUAL Page 17 TECHNICAL DESCRIPTION Figure 4 1 4 Goniometer phi kappa omega and theta axes The programs controlling the measurement procedures of the system are WIN32 applications which run under Windows XP or Windows 7 The data acquisition and reduction are run concurrently with the program Crysalis r 4 2 KMW200CCD Chiller and KMW3000C Chiller Information about the Chillers is in separate manuals suppl
36. express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a particular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or performance of this document or of any information contained herein Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the separate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcontract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer software as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or disclosure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in
37. he tube shield A N CAUTION Failure to fit these o rings will result in water leakage which could damage both the X ray tube and the instrument 10 Replace the X ray tube with an identical specification Cu X ray tube Holding by its metal base remove the new X ray tube from its protective box A wa Ensure that the X ray tube is correctly mounted Incorrect mounting may result in exposure of personnel to X ray radiation 11 From the front of the ULTRA insert the X ray tube into the tube shield in the same orientation as the previous one and secure with two screws 12 Re mount the thermocouple to the base of the X ray tube and re mount the ULTRA front face panel Secure in place using a 5mm Allen key and the single screw described above 13 Re connect the water supply to the back of the ULTRA X ray tube shield 14 Switch on power to the generator and KMW3000C chiller unit Xcalibur Gemini ET USER MANUAL Page 36 MAINTENANCE INSTRUCTIONS 8 3 Changing the X ray Tube of Enhance Vertical X ray Tubes Task Time 30 minutes When Sealed source X ray tubes have a limited useful lifetime Operation of a 3 kW Mo tube at typical output of 2 kW and a 2 2kW Cu tube at 1 5 kW will normally provide 10 000 hours of use actual values may vary see third party manual Note X ray tubes also have a limited shelf life Who Agilent authorised operator trained on radiation safety Tools Set of Allen keys Set of flat headed
38. hen returning components for service or repair it is essential that the item is shipped together with a signed declaration that the product has not been exposed to any hazardous contamination or that appropriate decontamination procedures have been carried out so that the product is safe to handle Care has been taken to ensure the information in this manual is accurate and at an appropriate level Please inform Agilent Technologies if you have any suggestions for corrections or improvements to this manual Xcalibur service and support is available for technical and operational issues as indicated below E mail XRDSupport agilent com e Phone 44 0 1865 291600 between 8 a m and 4 30 p m UK time Monday to Friday Fax 44 0 1865 291601 Agilent Technologies acknowledges all trademarks and registrations Copyright 2011 Agilent Technologies Limited All rights reserved No part of this document may be reproduced or distributed in any form or by any means or stored in a database or retrieval system without prior written permission of Agilent Technologies Xcalibur Gemini Version 2 4 USER MANUAL Page v Contents 1 Health and Safety Information ccccsssssssseeessseesesseeerssseeeesseeeesssseennees 1 Peds enea eese E 1 EZ Electical Sale N onenen te eet nC ree ee AE ee 2 1 2 1 Potential Electrical HaZards c cece cece ccccsscescsscsscesessessessesseseessessesseseeseeseeseesenseeseesensensenes 2 1 2 2 Recomm
39. ic materials Follow appropriate handling shipping use storage and disposal procedures and regulations Refer to BrushWellman Material Safety Data Sheet No M10 for further information AN 7 If Beryllium is exposed to fire it may oxidise to highly toxic beryllium oxide powder Do not attempt to clear up the remains of any fire but contact the relevant local agency stating that there is an incident involving possible beryllium or beryllium oxide contamination 1 11 Maintenance The manufacturer will not be held responsible for the safety reliability or performance of the equipment unless assembly operations extensions re adjustments modifications and repairs are carried out only by persons authorised by the manufacturer Interchangeable parts which are subject to deterioration during operation must be serviced or interchanged during the intervals given Xcalibur Gemini Version 2 4 USER MANUAL Page 6 INTRODUCTION 2 Introduction 2 1 Scope This manual applies to the Xcalibur system designed and manufactured by Agilent Technologies 2 2 How To Use This Manual This manual is aimed at operators and maintenance personnel of the Xcalibur system Operators of the system should be computer literate familiar with X ray diffraction techniques have had training in the use of the Xcalibur system by Agilent Technologies staff and have had training about radiation Safety This manual is intended to provide operators with a practi
40. ied with this equipment 4 3 Low Temperature Option If a cryogenic cooler is to be fitted to the diffractometer system then the correct adapter must be used to mount the cooler on the cryo support stand Further details can be obtained from Agilent Technologies 4 4 Safety Features In normal operation the X rays are generated and projected in a totally enclosed cabinet constructed of lead doped Perspex called Kyowaglas equivalent to 0 3mm of lead sheet Xcalibur has magnetic switches mounted at the base of the front doors and at the top of the side and rear panels of the protective enclosure During normal operation i e interlocks applied the X ray shutter will not open unless all the cabinet doors are closed If the doors are then opened whilst the X ray shutter is open the X ray shutter is immediately caused to close Access to the interior of the cabinet via the front doors is required when changing samples When the doors are opened during sample change and alignment the X ray generator remains on for optimum performance Indicator lights mounted on the outside of the enclosure show when the X ray generator power is on orange light and whether the X ray shutter is open red light or closed green If these lights are Xcalibur Gemini iene USER MANUAL Page 18 TECHNICAL DESCRIPTION defective then the X ray generator will not operate in the case of the orange light and the X ray shutter will not open in the case of the red
41. lent Technologies KMW3000C chiller manual Agilent Technologies Cryojet User Manual Oxford Instruments optional Cryostream User Manual Oxford Cryostreams optional Cobra User Manual Oxford Cryostreams optional Helijet User Manual Agilent Technologies optional Xcalibur Gemini and USER MANUAL Page 54 ADDITIONAL INFORMATION 12 2 Drawings 12 2 1 Mechanical Drawings hh hh heheheh hearkearkaankaka Lo iL LL LL Lf fff fff fff f f f f ie i N TE EEEE EEEE LLL LLL LLL LLL LLL LLL LLL LL 32A single phase all systems 32A single phase Gemini only Water Return Water Supply 16A single phase all systems 100 cm E S w N 44 cm 30 cm ke I Power Cables 2m ke e mm n cm 115 cm e a cm Figure 12 2 1 Xcalibur Gemini Suggested Layout Xcalibur Gemini Version 2 4 USER MANUAL Page 55 ADDITIONAL INFORMATION Xcalibur Gemini Dimensions 116 gt wd 100 gt A A 115 200 y 0000000000000 0000000000000000000 MMDQ000000 000000000 00000000 000000 QDNDODIO00 0000000000 00000000000000 QQQD000000 0000 0000000000 0000000000 QOND000000 0000000000 0000000000000 QOQO000000 0000 00000000000000000000 y 00000000000 00000000 000000000 00000 NOQQ0000000 000000000 00000000 000000 80 Me 80 gt KMW3000C Dimensions
42. ly CCD detector Cooling The CCD detector is water cooled by the KMW200CCD Cooler Ten metre long water pipes are supplied with the system to connect the cooler to an external water supply X ray Tube Cooling A cooling system is required to dissipate the heat produced by the X ray tube A closed circuit cooling system should be installed to minimise the effects of particles low pressure and water temperature fluctuation on the performance of the system from local tap water The KMW3000C Chiller is a closed circuit cooling system suitable for this purpose It is supplied with two hoses 10 metres long with 9 mm inner diameter and 15 mm outer diameter The maximum distance between the KMW3000C chiller and the system is 10 metres The distance between the water supply and the chiller is not limited but the supply must deliver 0 5 5 bar gauge pressure with a minimum 5 litres min flow and a gravity drain with an elevation that does not exceed 1metre The supply should have a wall mounted shut valve An additional chiller such as the ThermoNESLAB Is required when the location of the diffractometer does not have any running water or lab cooling system or if a continuous flow of water cannot be put down the drain The KMW3000C is a water to water heat exchanger and therefore the heat from the X ray tube is removed by the KMW3000C closed water circuit into the main water bath but this heat load has to be extracted by an additional cold water supply
43. mand from the software If you have the interface DC08 model then the front panel green LED Shutter Enable should light 6 3 X ray Tube Warm up Procedure When handling and using X ray tubes particular care should be taken to avoid injury caused by exposure to the X rays exposure to high voltages possible implosion of the vacuum tube and contact with Beryllium and Beryllium oxide If the X ray tube is stored for a lengthy period the vacuum may become impaired We recommend carrying out the following warm up procedure for new tubes and tubes that have not been used for more than 100 hours Use Crysalis e X ray device server software control to carry out the burn in procedure as detailed in the tube manufacturer s manual lf after completion of this procedure a flashover occurs in the next 30 minutes repeat the whole procedure 6 4 System Standby and Normal Shutdown Procedure Depending on the period of diffractometer inactivity follow one of the 3 procedures below 6 4 1 Shutdown Procedure Diffractometer not expected to be used for 2 3 days 1 Ramp down the X ray generator to 10 mA 30 kV improves lifetime of the X ray tube Park the goniometer in its home position simply by exiting the Crysalis e program Turn off the video microscope using the front panel mounted switch Turn off the cabinet amp sample illumination using the front panel mounted switches og FS Warm up turn off sample cooling device follo
44. meter File Task Time 4 5 hours When After adjustment of beam collimator CCD detector position etc Otherwise twice a year Tools Ylid test crystal C11H10802 Procedure See section Refining of Machine Parameter File located in the CrysAlis e software manual Xcalibur Gemini Bena USER MANUAL Page 34 MAINTENANCE INSTRUCTIONS 8 2 Changing the X ray Tube of Ultra Horizontal X ray tubes Task Time 30 mins When Sealed source X ray tubes have a limited useful lifetime Operation of a 2 2 kW tube at typical output of 1 5 kW will normally provide 10 000 hours of use actual values may vary see third party manual Note X ray tubes also have a limited shelf life Who Agilent authorised operator trained on radiation safety Tools Set of Allen keys Set of flat headed screwdrivers Water receptacle e g Bucket Do not touch the Beryllium windows in the X ray tube Beryllium is a potentially toxic material CAUTION The customer may change the X ray tube of Enhance Ultra but the focussing optic inside this X ray source must be precisely aligned to each new X ray tube and this may only be performed by a trained Agilent Technologies service engineer Missing this alignment could result in worse performance of this X ray source CAUTION Use only ceramic X ray tubes not glass X ray tubes Remove all packaging material and red plugs from water openings before fitting X ray tube must be inserted in the co
45. n Start This will move the detector away from the goniometer axis in 1 mm steps This should be repeated several times until there is a clear gap between the detector and the goniometer axis Turn on the KMW200CCD chiller Follow steps 2 9 from Power loss to goniometer below See above Version 2 4 Page 49 TROUBLE SHOOTING Xcalibur Gemini USER MANUAL 2 Power loss to goniometer 1 Restore power to system restart the PC and CrysAlis program 2 Switch off the interface wait 5 seconds and then switch on 3 In CrysAlis open the service power tool and select MGCUTIL and press start 4 Click on parameters and the two Edit deg buttons Set both to 1 0000 and click on slow Click enter 5 Select offending angle from the radio boxes Click on Set angles and Start Input actual position of each axis as read from the mechanical goniometer Pay special attention to A op 6 Select Rsync all and click Start Note that at the end of the Rsnync operation the Rsync flags should read 1 This is located on the text line below the parameter button 7 If the detector distance is not at home select Detector and drive relative Click on Start This will move the detector towards home in 1 mm steps Look at the HOME flag number for detector distance It might initially be 1 if the detector is far from home
46. ntateaisteanss 8 3 1 Environmental Requirements ccccccscccecescsscsccsceecsecssceceessuseecessessuseacesseseusencesseseuseaceseesenseasesensnsaseess 8 SO VC a ates cette cea tecetes te ect ct setetactsta tater dastatactstactetactstaaetect E tacutacssacedeceasaatecesacatecstacetecns 8 3 2 1 Electrical Supply oo cc cccceccscsscsccscsecssceececsessuseececseseuseasesseseeseasecseseuseusecseseusenseuseseesenseacesesensaneeses 8 32AN Atl GOO IMIG nn aa 9 3 2 3 Helium Gas Supply For Ultra ccc ceccscsscsccecssssecessessesseseesesseseuseuseseeseuseaceseeseuseasesensensanseses 9 3 3 Penormanc e D AU A cence ctstentacetecectects nade edacistastteceaes wtactstacteteclstadatactsac stacttadudedlstadetodusacstadstadeiadstadotadotanstacbiatete 10 3 3 1 X ray Tube Typical Operating Conditions 0 0 ccc csesceesssssecsscscsscseseceesecsesecsecessesessnsaseesaees 10 7 SOC Os CLC GION menona a aa 10 3 3 2 1 GOIMOV Al cecicicceeacica dts tandtstictaaciateicadtatciandtatdbanc tate scnsdatcdandtatdsanstatssanseadesauesaissaassatesanseadstacetatwcasssanniens 10 3 93 22 EOS COD DELO CO i adits coseciess dotacetialstacetacetadvtacistadedenlstadedtadosan staadaaawssaseaaetennsaastaadaaawshasoaetonnsaastaacsauettes 11 3 3 2 3 Atlas COD Detector oo ccc ccc ccccescescescescescescessessessesseseessesseseeseeseeseeseesesseseesensesensensensenss 11 3 39 24 Titan CCD Dele Ctr sssssssssssonssannns a a a 11 3 3 2 5 PC CCD Interface wee ccc cece ccccescescescescesse
47. oftware training 5 3 Storage Before installation commences or when the system is not being used for extended periods store the diffractometer in accordance with the environmental conditions for temperature and humidity stated in the SPECIFICATIONS section of this manual Always store Xcalibur in a secure room Xcalibur Gemini ae USER MANUAL Page 25 OPERATION 6 Operation Xcalibur is a computer controlled system All functions are controlled from the computer terminal except when control is released from the computer terminal to the remote control unit Power is switched on and off via manual switches located on the system The KMW200 and KMW3000C chillers must be connected to Xcalibur before operating the system AN Local rules and regulations may apply to the use of the diffractometer If these exist refer to these local rules before operating the system Do not operate the diffractometer unless ALL X ray tubes are fitted If the X ray tube is not present then a high voltage will appear on a bare connector and water will flow out of the tube shield When a tube reaches the end of its useful life it must be left fitted until a new tube is available for exchange 6 1 Controls and Indicators Control m om Jion a Emergency Stop Red button Front left corner of electronics Shutdown X ray generator rack power and stop goniometer movement Remote Control Key pad Inside protective enclosure Control and drive goniome
48. ower distribution Electronics rack left 10 A 250 V fast 5x20 mm F1 hand side rear panel Electronics rack rear 5x20 mm F3 panel Cabinet illumination Electronics rack rear 6 3 A 250 V fast panel Shutter driver Shutter driver PCB 0 8 A 250 V fast Interface MGC Interface front panel 2 A 250 V 5x20 mm model System control board System control board 800 mA left hand side of rack T800 mA 250 V 10 2 Bulbs a en Top panel of CCD camera MultiLED T5 5 RED 12 V 25 mA Swisstac MultiLED T5 5 GREEN 12 V 25 mA Swisstac Protective enclosure Inside top protective Halogen 12 V AC 35 W Osram type illumination enclosure 44865WEL x3 Fibre optic lights Inside light source box Halogen 12 V 75 W Osram type 64617 Xcalibur Gemini ana USER MANUAL Page 52 DISPOSAL INSTRUCTIONS 11 Disposal Instructions 11 1 X ray Tube and CCD Detector The X ray tube and CCD detectors have beryllium windows Dispose of Beryllium in accordance with local government regulations 11 2 Third Party Equipment Refer to third party manuals for information about disposing of third party equipment Xcalibur Gemini ie USER MANUAL Page 53 ADDITIONAL INFORMATION 12 Additional Information 12 1 Third Party Information Information marked optional is only supplied when that option is fitted to the system Title Supplier Material Safety Data Sheet M10 Beryllium Brushwellman KMW200CCD chiller manual Agi
49. ower supply when the KMW200CCD is operational To switch off the CCD detector use the KMW200CCD s front panel power switch Xcalibur Gemini Version 2 4 USER MANUAL Page 2 HEALTH AND SAFETY INFORMATION Do not touch any unshielded wires or connectors while mains power is supplied to the system Do not allow water or any other foreign objects to come into contact with the equipment s electrical components 1 2 3 First Aid A course in first aid to include methods of artificial respiration is recommended for those whose work involves equipment that may produce a high voltage A N WARNING Do not attempt to administer first aid to someone who may have suffered electric shock until the source of the shock has been isolated Mains voltages are present in the system High voltages are used by the X ray tube and power supply These can cause serious injury or death Only personnel qualified to work with high voltages and currents should perform service or maintenance work on such equipment 1 3 Mechanical Handling Safety AN Lifting points are provided for safe handling of components and safe handling practice must be observed to comply with local regulations Check that lifting points are used only for the job intended The system itself and some components are heavy and require careful handling Use safe lifting procedures for heavy items to prevent possible strain injury 1 4 Safe Mechanical Practice In normal use p
50. qualified to work with the voltages and currents used by this equipment should attempt to disconnect dismantle or modify the equipment 1 2 1 Potential Electrical Hazards The following list is not intended as a complete guide to all the electrical hazards on the system but serves to illustrate the range of potential hazards that exist e electric shock e electric burn fire of electrical origin e electric arcing 1 2 2 Recommended Precautions All of the electrical equipment supplied as part of the system should be provided with a protective ground Do not remove protective grounds as this may give rise to an electrical safety hazard It is vitally important that the system is properly grounded at all times Follow local and national electrical regulations and procedures Do not defeat interlocks remove connectors disconnect equipment open safety covers dismantle or modify equipment unless you are qualified and authorised to do so and you are fully conversant with its operation and potential hazards or have total assurance through your local electrical permit to work system that the equipment has been made safe Ensure that the mains supply is fused at an appropriate rating or fitted with a circuit breaker and that it can be isolated locally via a clearly labelled clearly visible and easily accessible isolating switch Isolate the supply before carrying out any maintenance work Never switch off the CCD detector s p
51. re in place 2 No sample should be mounted on the goniometer 3 Pull out the collimator from its housing pulling from the right hand side Be careful not to touch the beamstop or CCD detector 4 Select the required size of collimator and push into position on the diffractometer such that it is flush to the housing surface The collimator should be inserted such that the flat edge with the collimator size label is uppermost Ensure that the collimator is correctly mounted Incorrect mounting may result in exposure of personnel to X ray radiation Xcalibur Gemini Eea USER MANUAL Page 38 MAINTENANCE INSTRUCTIONS 8 5 Aligning the X ray Collimator of Enhance The X ray collimator is factory aligned via the collimator housing This means that re alignment is not needed when changing between the collimators supplied by Agilent Technologies If collimator re alignment is required please contact Agilent Technologies for assistance 8 6 Aligning the Video Microscope Task Time lt 30 minutes When When it becomes impossible to centre a sample correctly on the video microscope image Tools Pre mounted 0 3 mm steel ball mounted on a goniometer head f Left right Adjustment Height Adjuster r in a 4 b gt Z Left right Adjusters ve p Equivalent to Height Adjustment B ff owe iz i sf Figure 8 6 1 Goniometer Head Adjustments Figure 8 6 2 Video Microscope Adjustments When first assem
52. rrect orientation with the Agilent Technologies logo upside down Procedure 1 Switch off the power to the X ray tube to be changed 2 Turn off the KMW3000C chiller to stop water circulating 3 Leave for at least 20 minutes to ensure that the X ray tube is not hot test temperature before proceeding CAUTION Have a receptacle ready to receive water from the pipes and X ray tube shield Xcalibur Gemini TE USER MANUAL Page 35 MAINTENANCE INSTRUCTIONS 4 Disconnect the top water pipe from back of Ultra X ray tube shield This is attached with a quick release connector 5 Remove the Ultra front face panel To do this locate the metal block on the left side of the X ray tube housing which is behind the front face panel find the single screw at the rear of this block which is holding the front face panel and use a bmm Allen key to completely undo the screw Lift off the front face panel 6 Unscrew the temperature sensor from the front plate metal base with label of the X ray tube 7 Release the two screws holding the X ray tube in place and withdraw the X ray tube from the X ray shield Do this by holding the front plate metal base with label and pulling towards the front of the Ultra Ensure that the X ray tube is held level and withdraw parallel to the X ray shield 8 For disposal of used X ray tubes see the DISPOSAL chapter of this manual 9 Make sure the two o rings remain in their grooves at the front of t
53. screwdrivers Water receptacle e g Bucket Do not touch the Beryllium windows in the X ray tube Beryllium is a potentially toxic material CAUTION Use only ceramic X ray tubes not glass X ray tubes Remove all packaging material and red plugs from water openings before fitting X ray tube must be inserted in the correct orientation with the Agilent Technologies logo upside down Procedure 1 Switch off the power to the X ray tube to be changed 2 Turn off the KMW3000C chiller to stop water circulating 3 Leave for at least 20 minutes to ensure that the X ray tube is not hot test temperature before proceeding 4 Switch off and remove any cryogenic device mounted on the diffractometer 5 Remove the plate for mounting cryogenic devices 3x M8 screws to be removed from top of attachments tower 6 Unscrew one screw at the front and the back the end cap from the top of the Enhance and remove this may also need the loosening of the conical cover at the base end of the collimator for the Cu source and lay to one side along with the integrally mounted thermal sensor 7 Unscrew and slide out the X ray tube in an upwards direction A little water inside the end of the X ray tube plate will drip out and should be cleaned up but otherwise all water in the system will be retained inside the pipes 8 Make sure the two o rings remain in their grooves at the top of the tube shield Xcalibur Gemini T USER MANUAL Page 37
54. se note the following guidelines Only authorised personnel who have received appropriate instruction and are aware of the laboratory rules that govern the use of this type of system should operate the system Never dismount the beam stop when the system is operational Do not operate the system without the collimator unless performing the beam alignment procedure Use appropriate X ray detection equipment to perform regular radiation checks as per any laboratory rules Use only genuine hardware X ray tubes X ray generators monochromators goniometer heads and collimators as recommended by Agilent Technologies Use of other products may compromise the performance of the shielding and safety system and may invalidate your warranty 1 8 Vacuum N When handling and using X ray tubes and the CCD detector particular care should be taken to avoid injury caused by possible implosion of the vacuum tube Wear eye protection 1 9 High Pressures Know the law about high pressure gas cylinders and follow it High pressure cylinders are often used to store gases typically at pressures up to 200 bar Most countries have laws about using them e Chain cylinders to a fixed object or keep them in specially designed trolleys e Only use approved and tested high pressure fittings Xcalibur Gemini Version 2 4 USER MANUAL Page 5 HEALTH AND SAFETY INFORMATION 1 10 Hazardous or Toxic Materials Beryllium and beryllium oxide are tox
55. sed service representative should carry out other tasks If in any doubt about the performance of the diffractometer contact Agilent Technologies 7 2 Weekly Maintenance Schedule Tools and Materials None Action Personnel Estimated task Estimated duration elapsed time 1 Check door and cabinet window Authorised Operator 2 minutes 2 minutes safety interlocks 7 3 Monthly Maintenance Schedule Tools and Materials Radiation meter Action Personnel Estimated task Estimated duration elapsed time 1 Check Emergency Stop Authorised Operator 10 minutes 10 minutes 2 Check X ray radiation levels Authorised Operator 20 minutes 20 minutes Xcalibur Gemini Ban USER MANUAL Page 31 MAINTENANCE SCHEDULES 7 4 Six Monthly Maintenance Schedule This maintenance schedule should also be completed after adjustment of the X ray beam collimator and CCD detector position Tools Ylid test crystal C11H10802 Action Personnel Estimated task duration 1 Refining machine parameter file Authorised Operator 4 5 hours 2 Check alignment of video Authorised Operator 1 hour microscope and cryogenic cooling device if fitted 7 5 Yearly Maintenance Schedule Tools and Materials Ylid test crystal C11H10802 Special T tool Phillips screw driver Rotary vacuum pump capable of obtaining a pressure of lt 0 04 mbar Vacuum tubing and adaptor Personnel Estimated task duration 1 Refine machine parameter file
56. sessssssssecsessecsessesessesseseeseseesansessesensaesassesensaneates 32 8 Maintenance Instructions ccccccsssessssscsesssseesssseeeesseseeesssceesesssenessseeeseesoees 34 8 1 Refining the Machine Parameter File ccccssscsscscsscssescsssecsececsececsesessesacsesaesesaaeesensesensassesasensaees 34 8 2 Changing the X ray Tube of Ultra Horizontal X ray tub s ccccescessesesesesseseeeeseseeseeeeseseeeeees 35 8 3 Changing the X ray Tube of Enhance Vertical X ray TUDe S ccccccesesessesseseessssteessseseesseeeeeen 37 8 4 Changing the Collimator of Enhance ccccccccsssscsssscsssscescsesecsececsececsucessesassesaesessaeesensesensatsesasensanes 38 8 5 Aligning the X ray Collimator of Enhance cccccsscscssccessceessesecseceeseceesesecsesaesessasessucessnsassesasensanes 39 8 6 Aligning the Video MICrOSCOPE cccscescesssscsssscerssscsesscsessscacsecsessnsaesecsesensasseesesensansessesensatsassesensansaees 39 8 7 Checking the Door Safety Interlocks ceccsessssscsscscsscsesscsesecsececseceeseseesesassesaesessnsesenseseesassnsaseesanes 41 8 8 Checking the Emergency Stop ccccccccsscscssssssscsesscsscscscsesesacsessececsscessusessesacsesaesessasesensesensassesasensanes 41 8 9 Checking the X ray Radiation Level s ceccssscsssscsscscsscscsssseeecsesecsececseceesesacsesaesessaeessusessnsaseesasensanes 42 8 10 CCD Detector Pumping Out VACUUM cc ecceccssccsssssesss
57. sink of the CCD power supply become hot In normal use they are located inside a cabinet and hot parts are not accessible During maintenance periods however it may be necessary to open the cabinet so that adjustments can be made Therefore great care must be taken to avoid touching either the X ray tube or the heat sink of the CCD power supply when they are operating and for a period of 20 minutes after operation 1 7 X ray Radiation A N RNG This equipment contains an X ray tube Ensure that safe working practices relating to radiation are employed Follow any local national or international rules and guidelines Intentional or reckless misuse of the X ray generator or its safety devices including safety interlocks and cabinet shielding can result in serious injury or even death During operation there is an acceptable level of X ray radiation as based on the recommendations on risk published by the International Commission of Radiological Protection ICRP and endorsed by the Health Protection Agency HPA in the UK For use in the UK the lonising Radiations Regulations Xcalibur Gemini Version 2 4 USER MANUAL Page 4 HEALTH AND SAFETY INFORMATION 1999 should be adhered to For countries outside the UK the appropriate laws apply such as registration and inspection Customers should be aware of their duty of safety to their employees and visitors To prevent injury to personnel and possible damage to the equipment plea
58. ssessessesseseesseseesseseeseeseeseeseeseeseeseeseesensensenseneenss 11 3 3 2 6 CCD Detector Maximum Theta and Resolution ccc cece csecseeessssssceseesesseseseeseneenseeees 12 3 3 2 7 CCD Detector Maximum Distance u ccc ccc cece sceseeseesceseeseeseeseeseeseeseesesseseesensensensensenss 13 3 3 3 Four circle Kappa Geometry X ray GOMIOMEtED c cece ccccceecseceecesescesssceseesensenseseesensensenees 14 OA ElectriGal Date EEEE E E P Ee EE E E E E E EE E 14 4 Technical Description sssssssasssnununnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnne 15 A MOVER IOW 201 Celt Ge miN eroras ioa gs AAAA EAA 15 4 2 KMW200CCD Chiller and KMW30000 Chiller ccc csscescsseesseceeeessessusessesenseusesesensanenes 18 4 SLOW temperate OPO 9 Ree meme Pe re DB PO BP BR PTO BIO REPO A EEEN 18 4A Safety FeatUle S irciecaen eel a aisle 18 5 Handling Installation Storage and Transit Information cccee 20 Xcalibur Gemini Gea USER MANUAL Page vi 5 1 Reception and Handling c ccccccescsssssssssscssssscsesscessessesecsessscaesecsessesaesesseseesansessesensaasessesersansassesensaneates 20 OO Wella DEEN e ccc scstcacsaieeiaecaatcaccecaecacccatestacccatcaccscaecucecattatancaat dacseae dan aetetancat dccsea tan caetetaaees 20 eC UNPACKING E EE EAE AE AAA A A A A ee A a nten 20 Oe lise IEC Mal Gall tel ACMI G cainii iiaii i 21 02 INStall ation and Setting TO VOLK 5 isiatiosisistvactietsavetsiica
59. ter Control must be released from computer Cabinet Switch Front of electronics rack Illuminate inside of enclosure Illumination Sample Switch Front of electronics rack Illuminate crystal sample illumination optional extra Video Microscope Switch Front of electronics rack Switch on off video microscope Flow gauge Turn knob Inside front right of electronics Control of Helium flow rate rack through Ultra optic housing only on systems hould be 30 40 cm mi fitted with Ultra SHOR He Sys amet Xcalibur Gemini Bua USER MANUAL Page 26 OPERATION Power wrt tw ieee Diffractometer Red switch Interface front panel left Power on off to goniometer goniometer Inside front door of electronics interface interface rack CCD power supply Switch Inside enclosure underneath Power on off to CCD power supply box detector Water Cooler for Red Switch Cooler front panel left Inside Power on off to Water CCD front door of electronics rack Cooler also to CCD detector Mains power Switch Inside left panel electronics Power on off to system supply rack Safety Override Key for Agilent service use only Cabinet Illumination Switch Video Microscope Switch Sample Illumination Switch optional SS Flow Gauge only on systems fitted with Ultra Figure 6 1 1 Location of switches Xcalibur Gemini Version 2 4 USER MANUAL Page 27 OPERATION Indicator Location Meaning Orange light
60. to maintain the instrument in safe condition General This product is a Safety Class 1 instrument provided with a protective earth terminal The protective features of this product may be impaired if it is used in a manner not specified in the operation instructions Environment Conditions This instrument is intended for indoor use in an installation category II pollution degree 2 environment Refer to the specifications tables for the ac mains voltage requirements and ambient operating temperature range Before Applying Power Verify that all safety precautions are taken The power cable inlet of the instrument serves as a device to disconnect from the mains in case of hazard The instrument must be positioned so that the operator can easily access the power cable inlet When the instrument is rack mounted the rack must be provided with an easily accessible mains switch Ground the Instrument To minimize shock hazard the instrument chassis and cover must be connected to an electrical protective earth ground The instrument must be connected to the ac power mains through a grounded power cable with the ground wire firmly connected to an electrical ground safety ground at the power outlet Any interruption of the protective grounding conductor or disconnection of the protective earth terminal will cause a potential shock hazard that could result in personal injury Do Not Operate in an Explosive Atmosphere
61. tor Xcalibur Gemini ney USER MANUAL Page 8 SPECIFICATIONS Voltage fluctuation lt 10 with line voltage regulator fitted if necessary Location of outlets On wall behind system except computer monitor supply which should be near intended computer table location Protection Circuit breaker to be fitted to all electrical outlets 3 2 2 Water Cooling Maximum flow rate 1 8 I min Pressure 0 5 3 bar gauge Temperature stability Her G Temperature range 5 18 C Composition Refer to third party manual provided by X ray tube manufacturer 3 2 3 Helium Gas Supply For Ultra Purity 99 99 Regulator low pressure regulator Minimum pressure 0 5 bar gauge Flow rate 30 40 cm3 min ATP Xcalibur Gemini jose USER MANUAL Page 9 SPECIFICATIONS 3 3 Performance Data 3 3 1 X ray Tube Typical Operating Conditions Tube Voltage kV setting Current mA setting Resulting power kW Cu 2 2kW tube 50 40 2 0 Mo 3kW tube 55 40 2 2 Maximum radiation dose due to scattering lt 0 5 uSv h with Mo 3 kW tube operating at 2 2 kW at outside surface of the enclosure door closed shutter open Maximum radiation dose due to scattering lt 0 5 uSv h with Mo 3 kW tube operating at 2 2 kW door open with shutter closed 3 3 2 CCD Detector 3 3 2 1 General CCD chip Kodak KAF4320 E Scintillator material Gadox Peltier cooling 40 C two stage cooler Temperature stability 0 05 C micro processor P
62. tor or scintillation point detector The CCD area detector and the point detector are used to measure the X quanta diffracted from the sample Y fs Key 1 X ray tube 4 Collimator 2 4 circle Kappa goniometer 5 Beamstop 3 X ray Shutter 6 Beryllium Window 7 Video microscope Figure 4 1 2 View of Xcalibur Ultra diffractometer The X rays are generated by a sealed tube which is mounted on the goniometer and powered by the high voltage X ray generator The X ray optics consist of a high speed shutter located next to the tube shield a monochromator for selecting a specified bandwidth from tube spectrum and a collimator for limiting beam divergence The sample can be viewed with the video microscope which is attached to the stand doming the instrument The video image is made available through CrysAlis software on the PC monitor just outside the cabinet Xcalibur Gemini Version 2 4 USER MANUAL Page 16 TECHNICAL DESCRIPTION Figure 4 1 3 View of Gemini diffractometer The CCD area detector works according to the following principle The X rays enter the detector through a Beryllium window to the vacuum sealed detector unit A scintillation screen absorbs the X rays and emits visible light which is conducted via a fibre optic reduction taper towards the scientific grade CCD chip The CCD signal is digitised to 18 bit resolution by a correlated double sampling circuit with analog to digital converter located in the d
63. tween PC and system and to rear panel of interface For interface model MGC check emergency stop on the front of the interface has not been pressed If yes twist it to release turn off power on front panel wait 5s and then restart Goniometer axis will not move Check the goniometer is connected to the interface with two cables Always turn off the interface before plugging unplugging these cables Check yellow green grounding cable is connected to the goniometer Contact Agilent Technologies for further Support Xcalibur Gemini cine USER MANUAL Page 48 TROUBLE SHOOTING Goniometer Detector 1 Collision of the goniometer with collision the collision sensor on the front of Eos CCD detector interface front panel will show a red LED for the collision error state Other detector types do not have a collision sensor Goniometer lost angle 1 Collision of the goniometer positions Xcalibur Gemini USER MANUAL Turn off the KMW200CCD using the switch in the front of the electrical rack this will disable the collision sensors great care should be taken while the machine is in this state as considerable damage could be caused In CrysAlis re CCD open the service power tool and select MGCUTIL and press start Click on parameters and the two Edit deg buttons Set both to 1 0000 and click on slow Click enter Select Detector and drive relative Click o
64. ule diffractometers and 500 Angstrom for macromolecular systems The Xcalibur may be used with crystal conditioning devices Specifically low and high temperature attachments and high pressure cells Some minor modifications may be required by Agilent Technologies to enable use of these devices Xcalibur Gemini Version 2 4 USER MANUAL Page 7 SPECIFICATIONS 3 Specifications 3 1 Environmental Requirements Ambient temperature during operation 18 28 C Stability of ambient temperature during ae te operation Storage temperature gt 10 C lt 40 C Relative humidity 20 80 non condensing Location Clean dust free environment gt 2m from air conditioning or heating units Floor covering Conductive or if carpeted covered with electrostatic mats Floor strength Able to bear system weight of 500 kg over an area of 0 64 m2 3 2 Services 3 2 1 Electrical Supply Total power requirements 230 V 10 or 208V for USA for X ray generators and diffractometer 240 220 or 110V depending on region for temperature attachments and computer monitor 63 A All single phase supplies should be connected to the Same phase Number of outlets required 1 single phase outlet 16 A for diffractometer system comprising goniometer interface water chillers and computer etc 1 single phase outlet 32 A for each X ray generator 4 single phase outlets 15 A total for temperature attachments and computer moni
65. ump out port Pump out port with cover unscrewed Figure 8 7 2 View of the pump out port of the Atlas Titan CCD detector 5 Screw the T tool into place on the pump out port 6 Attach vacuum pump to the side arm of T tool using a suitable adaptor and vacuum tubing CAUTION Only use new clean tubing Apply vacuum before removing the CCD detector vacuum seal to prevent oil etc diffusing into the detector and causing damage 7 Switch on vacuum pump and evacuate tubing pumping line to 1x10 bar pressure 8 Depress T tool plunger and screw into place This screws into the o ring sealed metal stopper that secures the detector vacuum 9 Slowly withdraw plunger to remove stopper Secure plunger in extended position 10 Leave under vacuum for 20 minutes 11 Slowly depress T tool plunger to replace stopper and unscrew plunger CAUTION Do not turn off the vacuum pump until the CCD detector has been sealed using the relevant stopper Xcalibur Gemini T USER MANUAL Page 43 MAINTENANCE INSTRUCTIONS 12 Switch off vacuum pump and disconnect pipes 13 Unscrew T tool and replace the cap on the port of Atlas or Titan For Eos replace the front access plate of CCD detector leaving 1mm gap equally all around the edge of the collision sensor 14 Switch on the cooling water for the CCD detector at the cooler chiller unit and monitor the cool down using the CCD device server
66. ure that the shutter cable Fischer connection is secured to the optics shutter housing Version 2 4 Page 45 TROUBLE SHOOTING Generator will not generate X rays Xcalibur Gemini USER MANUAL 7 He flow is out of normal range ULTRA 8 Beam stop is in the up position ULTRA 9 Emergency stop has been pressed 1 No power reaching the generator 2 Computer RS232 communication is not connected 3 Emergency stop has been pressed and not released Adjust He flow rate to normal range so that lamp behind flow gauge shows green colour not red Move beam stop to the down position Ensure emergency stop has not been pressed generator will also not function If yes twist to release and turn off on the interface 1 Ensure fuse or circuit breaker of mains supply is OK 2 Ensure switch on the unit rear panel is in the correct 1 position Check COM cable from generator is connected at the rear of the computer Check COM port number has been detected by CrysAlis ro 1 Twist emergency stop button clockwise to release 2 Restart high voltage on generator 3 Switch off system interface at the front panel wait 3 s and then restart Type gon reinit on Crysalis e command line 4 If Mo X rays are required then change over radiation type Gemini models only using software button Version 2 4 Page 46 TROUBLE SHOOTING 4 No cooling water ts flowing 5 X ray tub
67. utsiudaastutsaiadiatnanesistuinadtetutuassehdeaeiatsiuautaiteadunantiat 22 5 2 1 Preparation of Site aNd SCTVICES wic sccacscicccsccdacedscccicdiaccdee deagcdadeachicseig hicdatdeiidcigdhaadead hiadaad hieeds 22 EPAPER e CHING 00 0 OF AA E EAE EA AS EA A AE AE A E A AA AAEE 25 Eo OOE ainai i aa 25 0 Operan O E deans apne vauiel cane cundevenauseeeravaccuiaut sieaetes 26 OA CONTOIS and Mda O S nea EEE isa liad 26 OVS eU i A 28 CSA tay lube Warmup Proce dU Geanina 29 6 4 System Standby and Normal Shutdown Procedure ccccecccscssescescescccseeecsecsecseeessusesseseesensanseees 29 O29 EMERGE ICY O NUTONE ENNS AES 30 6 5 1 Emergency Shutdown Procedure cccccsscscsssscesssseessesecsecseseceesesaesessesecseceesnsassesassesaasesenees 30 7 Maintenance SCHEGUICS scciiicesecrcirsattainesAinivecescitiacwddinedlwaiiabeudcursncwssastbuisdcunddutacee 31 FA MMUOOUCHON e222 tance saeauen ea ena ent ea eet eae eee 31 1 2 Weekly Maintenance SCNEGUICs ccicicdcciccddeddecdadestestadsdbestadsddesdadeidcadadeadeuiadetdeciadsacdidschacdadvihcstadsddccdades 31 7 3 Monthly Maintenance Schedule u ccccccccsccscccscsscsccscsessscsscssessuseececseseuseucessesenseacessesensauseseesensanseses 31 7 4 Six Monthly Maintenance Schedule cccccccecsscsscscessssssccscsecseseecessesseseacesseseeseucessesensauseseesensaneeses 32 Jo Veal Maintenance oCheGUiG s 13c 22 e tiated 32 7 6 10 000 Hours Maintenance Schedule ccccecsssscs
68. ways of avoiding possible injury and equipment damage which may result from inappropriate ways of working A description of such potential hazards and how to avoid them Is given in this section This manual adopts the following convention N Indicates a potential hazard which may result in injury or death CAUTION Indicates a potential hazard which may result in damage to equipment Warning symbols on the equipment are Protective conductor terminal Earth ground terminal AN CAUTION Risk of electric shock CAUTION Refer to accompanying documents WARNING Radiation Hazard A CAUTION Risk of finger squeeze between moving parts See original manufacturers manuals for further safety data on third party equipment supplied with the system A list of these is given in this manual CAUTION Do not take risks You have a responsibility to ensure the safe condition and safe operation of equipment Xcalibur Gemini Version 2 4 USER MANUAL Page 1 HEALTH AND SAFETY INFORMATION The equipment should only be operated and maintained by authorised operators of the system An authorised operator is a person who has undergone specialist radiation training and has been trained in the use of Xcalibur by Agilent Technologies personnel 1 2 Electrical Safety In normal use the user is protected from the dangers associated with the voltage current and power levels used by the equipment Only personnel
69. wing manufacturers guidelines where applicable 6 Logoff the computer and shut down 7 Turn off the computer Monitor O on the screen Xcalibur Gemini Eea USER MANUAL Page 29 OPERATION 6 4 2 Shutdown Procedure Diffractometer not expected to be used for 1 week or more 1 Turn off X ray generator using the X ray device server in the Crysalis re GUI Allow water to flow for 15 minutes to cool tube 2 After 15 minutes turn off the KMW3000C X ray tube chiller using the key provided You may wish to turn off the external water supplying circuit although this is not necessary since a thermostatic valve will cease flow when the bath reaches a pre determined temperature Park the goniometer in its home position simply by exiting the Crysalis program Turn off the video microscope using the front panel mounted switch Turn off the cabinet amp sample illumination using the front panel mounted switches Gao Sk a p Warm up turn off sample cooling device following manufacturers guidelines where applicable 7 Logoff the computer and shut down 8 Turn off the computer Monitor 0 on the screen 9 Turn off the diffractometer interface red illuminated switch located on the left side of the front face 6 5 Emergency Shutdown The emergency shutdown procedure should be used e lf there is a fire or any other emergency requiring the evacuation of personnel from the area AND e The procedure can b

Download Pdf Manuals

Related Search

Related Contents

BoConcept Nago Assembly Instruction  Workflow Manager Manual Version 5.4  GE DBSR453GBWW Gas Dryer  021 - Oventrop  全ページpdf （8.77MB）  BULLETIN COMMUNAL Printemps 2013 n°50  

Copyright © All rights reserved. Failed to retrieve file