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User Manual - Agilent Technologies

1. 9 1 2 Electrical Safety RH Ert nic ice miae hi emis 10 1 2 1 Potential Electrical 10 1 2 2 Recommended Precautions 0 111 1 10 1 3 Mechanical Handling 5 11 1 4 Safe Mechanical Pr ctice m ete ee ei dum etie RR edens 11 Tob Mechanical Strass i i Eee desertae ser Dun n cde 11 EGIT ETE REED TEUER 11 NP Ornare 12 1 8 Extr me 13 1 9 gt 13 ra edes iere 13 1 11 Hazardous or Toxic 14 1 12 14 2 MACHO UC TON Secr IE 21 5 ER 15 2 2 How To Use This 15 2 9 System DVervIeW 15 3 Specifica O S FO DOES D AU
2. 1 26 Figure 8 IO Device Control 27 Fig re 9 Location of SWIEChes Sane ee tea 36 Figure 10 Status LEDs of SuperNova X ray 38 Figure 11 Microfocus X ray source mounted on SuperNova diffractometer 2 38 Figure 12 Rotating the beamstop position 40 Figure 13 CrysalisPre interface to X ray enne nennen nnne nennen 42 Figure 14 Goniometer Head Adjustments sssssssssssssssseeeeeeenenen enne nennen nn ennt nennen nennen 48 Figure 15 Video Microscope Adjustments 48 Figure 16 View of the pump out port of the Titan CCD detector sees 52 Figure 17 View of the pump out port of the Eos CCD detector eese 52 Figure 18 View of the pump out port cover on the AtlasS2 detector sess 52 Figure 19 Helijet adapter plate screws 01 54 Figure 20 Starting position for Helijet alignment
3. Status Device connected Lights Figure 8 10 Device Control window 4 5 3 Vacuum sensor and pump The vacuum sensor and electronics are mounted inside the high voltage generator One sensor port bottom side is open to atmospheric pressure and the other is connected through a fitting on the rear panel of the Generator to a Y piece in the hose between the vacuum pump and the microfocus X ray source The pump is mounted inside the electrical rack near the top 4 5 4 Ethernet switch An Ethernet hub is mounted in the system electrical enclosure for connections between an external network and the system PC and SuperNova X ray generator and Water Cooler This allows the PC to remotely control and communicate with the generator and cooler via Ethernet even when isolated from an external network 4 5 5 Piezo motor driver Inside the electronics rack is mounted a driver box for the piezo motors for aligning the microfocus sources The driver box contains four outputs for driving two motors on each of two x ray sources 4 6 Software 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 CrysAlisPre 4 7 Low Temperature Option If a cryogenic cooler is fitted to the diffractometer system then the correct adapter must be used to mount the coole
4. 3 1 Environmental 5 1 dada dada daga dadas 16 REASCNUIBMPM IEEE 17 3 2 4 Blectrical Supply 3 eines eddie Deer ter ar eene 17 32 2 W ter Coolingsiu droit p E i eed 17 3 3 Performance eae heen ety 17 93 USD CITIES 17 2 92 66 18 3 19 3 3 4 Four circle Kappa Geometry 19 344 Electrical IIS 20 4 Technical Desceriptigita evi paa c cua ko aei n d a kx uas Len ODER ri eus 4 1 Overview Of SuperNOVa rede de d res end eri hee 21 42 Micr focus X ray SOUrTCe as eh eee de ee cue eese poe Ae et 23 4 3 SuperNova X ray Generator c0sccseseseseseseseseseseseseseseseseseseseseseseeeseseseseseseseseseseeeeeseseseseeesees 23 44 Water o OE 24 AH EleCtromies Back teet
5. 56 9 Ele UE I CC Su perN ova Version 1 9 USER MANUAL Page 7 TOT 65 Bulbs cine e eate ed ete iret Lee LS LER f iL 65 11 Disposal Instructions ee sees eere eere eene O0 11 1 X ray Tube and CCD 66 11 2 Third Party Equipirient z iiie oL e RENE nale evi ATP 66 12 Additional Information 67 12 1 Third 1 67 12 2 DrawiniS e ivo 68 Table of Figures Figure 1 Components of a typical SuperNova system sess 21 Figure 2 Computer and nnne nnne netr tnit enin aiai ae ideia 21 Figure 3 View of a typical diffractometer 0sssseseseseseseseseseseseseeeseseseseseseseseseseseseseseeeseseseseeeeeeees 22 Figure 4 Goniometer phi kappa omega and theta axes shown on a typical diffractometer 23 Figure 5 Inside SuperNova X ray 4400 24 Figure 6 Air Cooler 25 Figure 7 Water distribution panel and
6. 0 ccccccceseeeececeeeeeeeeeeeaeeeeeeeeesesaaeeeeeeeeeeeeenneeeeeeeess 54 Figure 21 Helijet alignment tip nennen eren 54 Fig re 22 Water 56 Figure 23 SuperNova Suggested 68 Figure 24 SuperNova System Dimensions extended 69 SuperNova Version 18 USER MANUAL Page 8 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 SuperNova should be aware of potential hazards which exist in and around equipment of this type and the 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 Indicates warning or caution If you see this symbol on a product you must refer to the manuals for specific Warning or Caution information to avoid personal injury or damage to the product Warning symbols on the equipment are Protective conductor terminal Earth ground terminal CAUTION Risk of electric shock CAUTION Refer to accompanying documents WARNING Radiation Hazard This instrument produces X rays when energised CANADA WARNING Radiation Hazard This instrument pr
7. 26 4 5 1 Water distribution 26 4 5 2 10 Device for safety interlocks ueeeeeeeeeeeeseeeseeee eene nn 26 4 5 3 Vacuum sensor and pump 100 1111 nn nnne nn nn nhan sh 27 15 4 Ethernet SWIECTI TIR Te S PORE SNR 27 4 5 5 Plezo motor UFlVer E dee sts ten exti aede a ads 27 ALG SoftWate E tapete lesu tees 27 427 c EE 27 48 Safety Features 28 SuperNova Version 18 USER MANUAL Page 6 5 Handling Installation Storage and Transit Information 29 5 1 Reception and 29 HAITI EE 29 packing 29 5 1 3 Mechanical Handling i etie tenete 30 5 2 Installation and Setting to 31 5 2 1 Preparation of Site and 31 52 2 Setting o eret ER edid pe pte bete dile c eru 33 5 2 3 Installation Procedure Sii nui 33 SEIEN MELLE TE 34 6 peratiolicoss 6 1 Cont
8. 200 240V option 100 120V 32A 1 single phase outlet 16A 200 240V 32A 100 120V for diffractometer system comprising goniometer interface water cooler generator etc 4 6 single phase outlets for temperature attachments and computer and monitor 10 with line voltage regulator fitted if necessary On wall behind system Circuit breakers to be fitted to all outlets 3 2 2 Water Cooling This is required only if the SuperNova is not to be used with an air to water chiller Min flow rate Pressure Return line pressure Temperature stability Temperature range 1 l min 1 3 bar gauge At least 1 bar less than supply line pressure Take care to check this on closed loop water systems tb C 10 20 C 3 3 Performance Data 3 3 1 X ray Tube Maximum radiation dose due to scattering or leakage at 10cm distance from any outside surface lt 1pSv hr Typical Operating Conditions Tube Voltage kV setting Current mA setting Resulting power W Mo Cu 50W tube 50 0 8 40 Ag 44W tube 65 0 62 40 Su perN ova Version 1 9 USER MANUAL Page 17 Maximum Operating Conditions SPECIFICATIONS Tube Voltage kV setting Mo Cu 50W tube 50 Ag 44W tube 65 Current mA setting Resulting power W 50 44 3 3 2 CCD Detector 3 3 2 1 General CCD chip Scintillator material Peltier cooling Temperature stability Analogue to digital resolution
9. 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 SuperNova USER MANUAL Version 1 9 Page 3 APPENDICES Weekly Maintenance Record Sheet Week Date of Name of person performing Signature Comments No maintenance test 47 48 49 50 51 52 Monthly Maintenance Record Sheet Month Date of Name of person Signature Emergency X ray radiation Comments maintenance performing test Stop Check check OK OK Y N Y N Su perN ova Version 1 9 USER MANUAL Page 4 APPENDICES Six Monthly Maintenance Record Sheet Date of Name of person Signature Comments maintenance performing test Yearly Maintenance Record Sheet Date of Name of person Signature Machine CCD detector Comments maintenance performing test parameter file vacuum refined pumped Y N Y N Su perN ova Version 1 9 USER MANUAL Page 5 Agilent Technologies Inc Printed in Poland September 2014 E Agilent Technologies
10. Su perN ova Version 1 9 USER MANUAL Page 29 5 1 3 Mechanical Handling 5 1 3 1 Weights Dimensions and Lifting Points HANDLING INSTALLATION ETC Description NET Dimensions Centre of gravity Lifting points Weight width x height x depth kg cm Kappa 106 43x 64 x 47 Offset from centre of At four corners goniometer unit towards side of X DO NOT lift from ray tube mount below X ray generator 12 48 x 13 x 43 Centre of unit From the sides and below Protection 120 100 x 72x 84 Centre of unit By hand from bottom Cabinet four corners Electronics rack 140 60 x 104 x 77 Centre of unit By hand from top or bottom four corners Water cooler 35 48 x 13 x 48 Centre of unit At the four corners and from below AirCooler 25 70x93x32 Centre of unit From the sides and below Helijet 10 30 x 25 x 10 head only Centre of component From below with parts transfer tube removed Cryojetb 15 15 x 35 x 15 head only Centre of component From below or using parts handles whilst supporting transfer tube MercurylTC 5 44 x 10 x 30 Centre of unit By hand from below GFC1 12 45 x 26 x 38 Centre of unit Front panel handles Su perN ova Version 1 9 USER MANUAL Page 30 HANDLING INSTALLATION ETC 5 1 3 2 Boxed Weights and Dimensions Weight Length Width Height Box No Item 1 Goniometer 160 95 60 90 2 Electronics rack 185 92 7i 134 3 Protection cabinet 220 115 100 100 4 Chiller A
11. Switch off the Water Cooler using the front panel mounted red switch this will also stop the HV Generator and prevent X rays from being generated 4 CCD detector will be turned off automatically by the previous step 5 Open the left side of the electrical rack and locate the two water filters as shown in the figure below SuperNova Version 18 USER MANUAL Page 55 6 7 8 9 10 11 12 13 14 15 MAINTENANCE INSTRUCTIONS Using an appropriately sized spanner unscrew the brass nuts one at a time as indicated by arrows in the figure below Be ready to catch water spillage From the inside remove the metal sieve and clean under running water or with a brush as necessary Figure 22 Water filters Replace the metal sieve in the correct orientation Replace the brass nut and o ring seal and tighten with correct torque to seal against water leakage Start the Water Cooler and wait for a minute to observe that there are no water leaks Repair if necessary Observe the front panel of the Water Cooler to check that there are no error indications In the case of a level warning refill the reservoir according to the procedure below Close the left side of the electronics rack Wait about 60 minutes for the CCD detector to cool down Close and re open the CrysAlisPro software to ensure re connection to the CCD detector 8 9 Refilling water reservoir The system includes a small water reservoir mount
12. stipulating the date person testing outcome and signature 8 6 Pumping Out Vacuum of CCD detector Task Time 16 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 Water Cooler this will also stop the HV Generator and prevent X rays from being generated 2 Wait for 12 hours for the detector to warm up 3 Unscrew cover from pump out port see Figure 12 below For the Eos detector this is underneath the collision protection cover which is removed by loosening four screws as shown in Figure 17 below On the S2 detector range the pump out port is accessed from the rear end of the detector by removing a circular cover as shown in Figure 18 below by inserting the appropriate hexagon key and rotating anticlockwise until the cover becomes loose and drops out Su perN ova Version 1 9 USER MANUAL Page 51 MAINTENANCE INSTRUCTIONS Set screws Figure 17 View of the pump out port of the Eos CCD detector Figure 18 View of the pump out port cover on the AtlasS2 detector 4 Screw into place the T tool the S2 detector range requires a longer version of this tool which is inserted into the opening on the rear side 5 Attach vacuum pump to the side arm of T tool using a suitable adaptor and vacuum tubing A N CAUTION
13. 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 Su perN ova Version 1 9 USER MANUAL Page 52 MAINTENANCE INSTRUCTIONS 6 Switch on vacuum pump and leave for 5 minutes 7 Depress T tool plunger and screw into place This screws into the o ring sealed metal stopper that secures the detector vacuum 8 Withdraw plunger to remove stopper Secure plunger in place 9 Leave under vacuum for 16 hours 10 Depress T tool plunger to replace stopper and unscrew plunger A N CAUTION Do not turn off the vacuum pump until the CCD detector has been sealed using the relevant stopper 11 Switch off vacuum pump and disconnect pipes 12 Unscrew tool and replace cover pump out port or collision cover the case of Eos leaving 1mm gap to allow the cover to move On the S2 detector range replace the circular cover on the rear side and lock it into place by inserting the appropriate hexagon key and rotating clockwise until tight 13 Switch on the Water Cooler 8 7 Aligning Low Temperature Attachment Task Time 30 mins When When the low temperature device s cold stream is observed to be misaligned from the crystal sample which is mounted and centred on the goniometer Tools 1 set of Allen keys Procedure The following instructions show how to align Helijet on the Xcalibur or SuperNova diffractomet
14. System noise so called read noise Dark current Communication Readout time EosS2 552 TitanS2 Readout time Eos Atlas Titan Truesense Imaging KAF4320 E Gadox 40 three stage cooler 0 05 C micro processor PID True 18 bit lt 12 e RMS lt 0 05 e pix s Gigabit Ethernet 0 225 4 x 4 binning 0 38s 2 x 2 binning 0 75s 1 x 1 binning 0 28s 4 x 4 binning 0 46s 2 x 2 binning 1 59s 1 x 1 binning 3 3 2 2 Eos EosS2 detectors Active area Weight Pixel size on scintillator Fibre optic reduction 95mm diagonal 10kg 31pm 1 3 low distortion reduction taper SuperNova USER MANUAL Version 1 9 Page 18 3 3 2 3 Atlas AtlasS2 detectors SPECIFICATIONS Active area Weight Pixel size on scintillator Fibre optic reduction 135mm diameter 16kg 48 2 0 1 low distortion reduction taper 3 3 2 4 Titan TitanS2 detectors Active area Weight Pixel size on scintillator Fibre optic reduction 165 mm diameter 20kg 60 um 2 5 1 low distortion reduction taper 3 3 3 PC CCD Interface Communication Drivers Typical host computer Gigabit Ethernet Win XP Win 7 Pentium IV class 22 8 GHz 21 0 Gb RAM 20 colour display 3 3 4 Four circle Kappa Geometry Goniometer Type Sphere of omega kappa phi coincidence Maximum load Phi axis Resolution Scanning speed range CCD detector angular ran
15. be performed by the user is limited to replacing consumable items alignment procedures pump down procedures and checking radiation levels and safety features The user s authorised 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 elapsed duration time 1 Check door safety interlocks Authorised Operator 2 minutes 2 minutes 7 3 Monthly Maintenance Schedule Tools and Materials Radiation meter Action Personnel Estimated task Estimated elapsed duration time 1 Check Emergency Stop Authorised Operator 10 minutes 10 minutes 2 Check X ray radiation levels Authorised Operator 20 minutes 20 minutes Su perN ova Version 1 9 USER MANUAL Page 44 MAINTENANCE SCHEDULES 7 4 Six Monthly Maintenance Schedule This maintenance schedule should also be completed after adjustment of beam collimator CCD detector position etc Tools Ylid test crystal 10 11502 Action Personnel Estimated task duration 1 Refining machine parameter file Authorised Operator 30 mins 2 Check alignment of video Authorised Operator 30 mins microscope 3 Check alignment of low Authorised Operator 30 mins temperature attachment if fitted 4 Cleaning water filters Authorised Operator 30 mins 5 Refilling water reservoir
16. below the SuperNova system Check that the transparent hoses are securely fitted between the y piece and the SuperNova and the vacuum sensor in the enclosure below the SuperNova system Check that the collimator is fitted to the SuperNova Check that the pipe is connected to the sensor port on the back panel of the X ray Generator Generator will not generate X rays 1 No power to generator 1 Switch on at rear panel 2 Press POWER ON button on front panel SuperNova USER MANUAL Version 1 9 Page 58 TROUBLE SHOOTING Symptom Fault Solution 2 Emergency stop has been pressed and not released 1 Twist emergency stop button clockwise to release 2 Reset generator using POWER ON button on front panel 3 No cooling water through X ray source 1 Turn on the Water Cooler 2 Confirm all water hoses are connected properly 3 Confirm no error states on Water Cooler front panel 4 Confirm cable connected between rear panel of Water Cooler and X ray generator 4 Cabinet X ray warning lamp is disconnected or not functioning Confirm cable is connected to warning lamp inside protection cabinet on top frame of front right door then contact Agilent XRD Service 5 X ray tube is over the maximum temperature Error will be shown on generator front panel Reset generator using POWER ON button on front panel Contact Agilent XRD Service for advice Problem
17. 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 SuperNova systems 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 SuperNova systems may also be used in the analysis of powder samples Intended samples should have a maximum unit cell dimension of 500 Angstrom for macromolecular PX systems SuperNova systems 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 Su perN ova Version 1 9 USER MANUAL Page 15 SPECIFICATIONS J Specifications 3 1 Environmental Requirements It is essential that the climate of the laboratory is controlled t
18. leave the goniometer in its home position ready for operation 2 Emergency stop button pressed Release the emergency stop button by twisting clockwise and follow the instructions on PC screen Power off interface wait 5 seconds and then power on Type gon reinit in CrysAlis e and press enter This will reinitialise all drives and return the goniometer to the position it was at when the emergency stop button was pressed SuperNova USER MANUAL Version 1 9 Page 60 TROUBLE SHOOTING Symptom Fault Solution Goniometer movement error Goniometer stopped after collision or blockage prevents movement Remove the blockage from the goniometer and follow the instruction on the PC screen Power off interface wait 5 seconds and then power on Type gon reinit in CrysAlis e and press enter This will reinitialise all drives and return the goniometer to the position it was at when the movement error occurred If the error persists then close and reopen the CrysAlisPro software When the software initialises it will test the goniometer slits definitions and if a fault is found it will ask the user to re run the slit definition Follow the instructions on the PC screen Strange artefacts on CCD images lines blocks chequer board 1 Errors occurring on Ethernet communication between detector and PC 1 Reset the CCD detector by switching off the Water Cooler power o
19. levelled and firmly set on the feet not resting on the wheels 3 The wheels can only be used by Agilent authorised service personnel Su perN ova Version 1 9 USER MANUAL Page 33 HANDLING INSTALLATION ETC 4 During transporting the system on the wheels care should be taken not to tilt the system It is possible to use the wheels to move the system only in the following cases the floor is a smooth and even surface the movement speed is not faster than 1 km h the movement is confined within the room where the system is installed 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 SuperNova in a secure room Su perN ova Version 1 9 USER MANUAL Page 34 6 Operation SuperNova is a computer controlled system All functions are controlled from the computer terminal Power is switched on and off via manual switches located on the SuperNova OPERATION WARNING Local rules and regulations may apply to the use of the diffractometer If these exist refer to these local rules before operating the system 6 1 Controls and Indicators 6 1 1 List of controls Control Type Location Effect Emergency Stop Red button Top right corner of front door of Shutdown X ray generator power electronics
20. 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 personnel 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 are permitted to service the equipment Water connections should be made and tested in accordance with any local and national safety regulations 1 5 Mechanical stress The protection cabinet housing protects personnel from exposure to various risks including electrical mechanical thermal and electro magnetic radiation Care should be taken to avoid mechanical damage of the cabinet housing The metal panels of the housing shield the device against an impact energy of up to 5J whereas the transparent window in the front door is resistant to an impact energy up to 1J IK06 rating If damage is found on the enclosure panels or window then stop using the instrument immediately and inform Agilent Technologies WARNING Protect the window against mechanical damage Do not use the instrument if the 06 window is broken 1 6 Moving parts There are a number of moving parts in the system which are powered by electric mo
21. shutter housing 5 Beamstop Ensure beamstop is rotated into data collection position i e vertical 6 Emergency stop has been pressed Ensure main emergency stop has not been pressed generator will also not function If yes twist to release and turn off on the interface Goniometer will not move Goniometer will not move when the cabinet is open Press and hold the two Motion Enable buttons simultaneously to allow the goniometer to move Water Cooler Symptom Fault Solution Unit cannot be turned on from the front panel Mains power is not connected Connect mains power at the rear panel Level error LED lights after switching on module Air Cooler Reservoir water level is too low Fill the Air Cooler Reservoir with coolant solution of 90 distilled water and 1096 of glycol SuperNova USER MANUAL Version 1 9 Page 62 TROUBLE SHOOTING Flow error LED lights after switching on module Some air bubbles remain in the water circuit Turn off and on the device If needed repeat the procedure a few times to get rid of the air in hoses and pipes Flow error LED flashes during operation Liquid cannot flow through the internal circuit through CCD detector or X ray source Check if the hoses are properly connected and valves are open Check if the filter is not blocked and clean it if necessary Air Cooler Reservoir error
22. 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 FAR 52 227 19 1 2 June 1987 U S Go
23. water cooling mode Open the front door of the electrical rack and switch on the top red switch 4 Turn the Water Cooler red switch on front panel 5 Both modules are started simultaneously by pressing that power switch on the front panel During the start up phase all error status LEDs will be illuminated When they are turned off that module of the unit is operating normally 6 Only when start up has completed successfully the CCD detector will be supplied with power from the CCD module and the flow acknowledge signal from the X ray module will appear 7 Allow 60 minutes for the CCD detector to cool the Peltier and chip to 40 C CAUTION AN The CCD detector requires 60 minutes cool down time Allow another 12 hours cool down time for all internal parts to equalise in temperature and give optimum detector performance 8 Turn on the interface using the red switch located on the left side of the interface front panel and wait 10 seconds Ensure 2 green LEDs are illuminated on the right of the interface 9 Turnon the PC and computer monitor 10 Launch the CrysAlisPr program from a desktop shortcut The goniometer should auto initialise providing a system ready dialogue in the CrysAlis history window if command prompt window is opened 11 Turn on the x ray generator key switch on front panel 6 3 1 Microfocus X ray Tube Warm up Procedure Normal operation of the microfocus X ray source is at 40W pow
24. 1 Refining the Machine Parameter File Task Time 4 5 hours When After adjustment of beam collimator CCD detector position etc Otherwise twice a year Tools Ylid test crystal 10 11502 Procedure See operating section Refining of Machine Parameter File in software manual Su perN ova Version 1 9 USER MANUAL Page 47 MAINTENANCE INSTRUCTIONS 8 2 Aligning the Video Microscope Including Sample Centring and Sphere of Confusion Check Task Time 30 minutes When When it becomes impossible to centre a sample correctly on the video microscope screen although this can also indicate the much more serious and unlikely problem of the Goniometer being out of alignment Tools Pre mounted 0 3 mm steel ball Height Adj Equivalent to Lateral Adj Height Adj Figure 14 Goniometer Head Adjustments Figure 15 Video Microscope Adjustments When first assembled the Goniometer sample centre and the video microscope focal point should be close to each other however the field of view is 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 Ltd supply a pre mounted 0 3mm steel ball to aid this procedure The three adjustments for the microscope can be seen in the picture ab
25. AL Page 25 TECHNICAL DESCRIPTION 4 5 Electronics Rack 4 5 1 Water distribution panel Figure 7 Water distribution panel and reservoir The water distribution panel is mounted in the left side of the rack This panel contains flow sensors and in line water filters for the internal water circuits through CCD detector and microfocus X ray source s If the KMW70 water chiller is installed in water to water mode then a reservoir is also mounted on this panel which fills the internal circuits separated from external cooling water 4 5 2 10 Device for safety interlocks Safety interlock wiring is organised through a PCB named IO Device in the system electrical enclosure After an error state the IO Device has to be reset to clear the error This must be done in order to close the interlock circuit to allow the X ray generator to operate The IO Device window shown in the figure below is opened by clicking on the IO icon near the top right of the Crysalis software main window The user must click on the Reset button to clear the error The cabinet lights can also be remotely controlled from this window Su perN ova Version 1 9 USER MANUAL Page 26 TECHNICAL DESCRIPTION EE Warnings and Errors Emergency stop Off Cooler error Detected Beam stop In Place Cabinet door Front door is open 7 r Firmware version Cabinet light Sample light 2 3 3 123 Final 517 PCB2v2 logic 5
26. Authorised Operator 30 mins Estimated elapsed time 4 5 hours 30 mins 30 mins 30 mins 30 mins 7 5 Yearly Maintenance Schedule Tools and Materials Special T tool Phillips screw driver Rotary vacuum pump capable of obtaining a pressure of 1x10 mbar Vacuum tubing and adaptor Action Personnel Estimated task Estimated elapsed duration time 1 CCD detector pump out vacuum Agilent Engineer 1 hour 16 hours 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 Su perN ova Version 1 9 USER MANUAL Page 45 MAINTENANCE SCHEDULES Action Personnel Estimated task Estimated elapsed duration time 1 Changing the X ray tube Agilent Engineer 1 2 hours 1 2 hours 2 Alignment of X ray optics Agilent Engineer 2 3 hours 2 3 hours Su perN ova Version 1 9 USER MANUAL Page 46 MAINTENANCE INSTRUCTIONS 8 Maintenance Instructions WARNINGS 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 8
27. LEDs lights Air Cooler Reservoir power or signal cable is not connected Turn off the KMW70 Water Cooler power supply at the front panel Connect Air Cooler Reservoir signal cable to the unit and the power supply cable to the back panel of the system Turn on the unit Int Ext Temp Error LED lights Liquid in the circuit is too hot a In water to air mode reduce the air temperature in the room below 25 deg C Provide good air flow space around the Air Cooler b In water to water mode reduce the temperature of water in the external circuit or increase flow rate X ray generator Problem Cause Action Unit cannot be turned on from the front panel Mains power is not connected Connect mains power and switch on at the front panel Unit sounds the intermittent alarm when switched on Beamstop is up Lower the beamstop Vacuum pump does not start Power is not connected to the vacuum pump Connect cable between CON 10 on rear panel and the vacuum pump Vacuum pump is noisy Sufficient vacuum cannot be created in the x ray optics Check the vacuum pipe is securely fitted between the pump and the y piece in the enclosure below the protection cabinet Check that the transparent hoses are securely fitted between the y piece and SuperNova USER MANUAL Version 1 9 Page 63 TROUBLE SHOOTING the microfocus source and the vacuum sensor conn
28. NUAL Page 28 HANDLING INSTALLATION ETC 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 SuperNova system 1 When the system arrives check that there is no visible damage with the delivery driver present If damage has occurred contact the carrier and Agilent Technologies immediately 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 A N 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 2 Always lift packing cases from the bottom using suitable lifting equipment refer to list of component weights in the following section 3 Move packing cases into the designated installation site 4 Contact Agilent Technologies to notify them that the equipment is awaiting installation by an Agilent authorised service provider 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
29. T Rd 44 7 2 Weekly Maintenance Schedule uueeeeeeeeeeseeeeeeee enses nenne 44 7 3 Monthly Maintenance Schedule c ccccscceseecscceseeeeeaeaeeeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaes 44 7 4 Six Monthly Maintenance Schedule ccccscscscsececcseeeeaeeeeeaeaeaeaeaeseaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaeaes 45 7 5 Yearly Maintenance icc ee FL e ee EAE Ee 45 7 6 10 000 Hours Maintenance Schedule uueeeeeeeeeeeseseeeeee eene nn nnn ann rn rara ranas 45 8 Maintenance 5 47 8 1 Refining the Machine Parameter 47 8 2 Aligning the Video 48 8 3 Checking the Door Safety 50 8 4 Checking the Emergency stop 50 8 5 Checking the X ray Radiation 51 8 6 Pumping Out Vacuum of CCD 51 8 7 Aligning Low Temperature Attachment 53 8 8 RU EIS EET INIRE M S 55 8 9 Refilling water nnnm nn
30. Version 1 9 Sept 2014 Agilent Technologies XRD Products 10 Mead Road Yarnton Oxfordshire 0 5 1QU UK Tel 44 0 1865 291600 Fax 44 0 1865 291601 http www agilent com chem SuperNova X ray Diffractometer System User Manual RES Agilent Technologies 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 express or implied with regard
31. ains an interlock switch which will result in a beeping noise sounding when the beamstop is in the up position and will also prevent the X ray shutter from opening The software collision model of the instrument assumes the beamstop is in the down position Therefore do not move the goniometer axes while the beamstop is in the up position since a collision might occur When moving the beamstop between positions take care not to strike the CCD detector beryllium window with the end of the beamstop If this happens then the beamstop may become misaligned and in the worst case the beryllium window may be damaged The beamstop handle is rotated by hand gripping it in the position shown in the figure below Pulling the beamstop handle forwards and downwards will rotate the beamstop from the down to the up position The opposite movement will return it to the down position The beamstop will be felt to click into position at both the up and down positions Figure 12 Rotating the beamstop position Su perN ova Version 1 9 USER MANUAL Page 40 OPERATION 6 3 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 Plugin all mains power cords to their wall mounted sockets system accessories 2 Ensure that the external circuit water cooling is turned on only for water to
32. ally Do not switch off the water supply while the microfocus X ray tube is operational since this will cause it to shutdown quickly and this will shorten the lifetime of the tube The tube should first be ramped down slowly to zero power before stopping the water flow 6 2 3 Temperature Sensor The microfocus X ray source contains a temperature sensor in contact with the microfocus X ray tube This sensor is connected to the X ray generator unit through the cable which includes the safety shutter connection If the temperature of the tube exceeds a set limit then the X ray generator will shut down the high voltage in order to allow the tube to cool down Such overheating may be caused by failure of cooling water supply or by a fault inside the X ray tube Do not turn on the tube again until the fault has been discovered and corrected 6 2 4 Vacuum pump The X ray focussing optics must be operated in a vacuum environment Without vacuum the X rays will degrade the quality of the optics and worsen the performance of the source Vacuum is produced using a diaphragm pump connected to the microfocus X ray source The pump must be connected with a vacuum pipe to the source before starting to generate X rays The X ray generator unit automatically starts the pump when high voltage is turned on The pin hole on the end of the collimator can be exchanged even when the vacuum pump is operational since part does not form part of the pumped volume Su perN o
33. beryllium or beryllium oxide contamination 1 12 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 Su perN ova Version 1 9 USER MANUAL Page 14 INTRODUCTION 2 Introduction 2 1 Scope This manual applies to the SuperNova 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 SuperNova system Operators of the system should be computer literate familiar with X ray diffraction techniques have had training in the use of the SuperNova system by Agilent Technologies staff and have had training about radiation safety This manual is intended to provide operators with a practical 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
34. ccessories 195 122 80 95 5 X ray source s Generator 195 122 80 95 6 CCD detector 145 120 95 117 7 LN2 Dewar 120 70 70 155 8 Cryojetb 145 70 80 190 9 Helijet 90 60 95 55 The weights and dimension above an estimate and should only act as 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 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 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 a figure below When the low temperature option is fitted an extra 100 cm space on the left hand side of the system is required Su perN ova Version 1 9 USER MANUAL Page 31 HANDLING INSTALLATION ETC Unpacked the largest subassembly will fit through a door aperture of 85 cm Check the door ap
35. d requested After completing the ramping the error LED should go off SuperNova USER MANUAL Version 1 9 Page 64 SPARES 10 Spares 10 1 Fuses bee flocon he peritos Power distribution Electronics rack right 10 A 250 V fast side Chiller Back of the chiller 3 15 A 250 V fast 10 2 Bulbs Device Location Description Protection cabinet X ray On cabinet front door M LIGHT LED modules yellow green red and shutter indicators Shutter open indicator On beamstop base MultiLED T5 5 RED 12 V 25 mA Swisstac Protection cabinet Inside top protection MEGA X1R WHITE LED illumination cabinet Sample illumination On beamstop arm LED WHITE 10MM 6DEG Su perN ova Version 1 9 USER MANUAL Page 65 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 Su perN ova Version 1 9 USER MANUAL Page 66 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 Cryojet User Manual Oxford Instruments optional Cry
36. dition SuperNova USER MANUAL 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 Page 3 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 D
37. doming the instrument The image is displayed on the computer monitor 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 transforms the X ray photons to 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 SuperNova Version 19 USER MANUAL Page 22 TECHNICAL DESCRIPTION the detector head The data transfer is via a gigabit Ethernet link to the PC workstation The control program stores the data for further data analysis to the hard disk The four goniometer axis is driven by microprocessor controlled stepping motors with 12 800 microsteps per revolution Figure 4 Goniometer phi kappa omega and theta axes shown a typical diffractometer The sample is aligned using a CCD video microscope The sample picture is displayed on the control computer A high brightness LED lighting system provides brilliant high contrast illumination of the sample at all goniometer positions 4 2 Microfocus X ray Source In the standard configuration this source unit contains a sealed tube microfocus Mo or Cu X ray tube dual shutter X ray focussing optics collimator and X ray beamstop The name Mova refers to the Mo sou
38. ecking the Emergency stop Task Time 10 minutes When Once a month Tools None Procedure 1 With the diffractometer running at minimum settings for example 10 kV 0 05 mA press red Emergency Stop button 2 generator should switch off immediately release the emergency stop button restart the x ray generator Return to required settings 3 Crysalis software will indicate that the emergency stop was activated switch off the interface restart the interface and then type command gon reinit in order to restart the system 4 Record details of the test in the local radiation log stipulating the date person testing outcome and signature Su perN ova Version 1 9 USER MANUAL Page 50 MAINTENANCE INSTRUCTIONS 8 5 Checking the X ray Radiation Levels Task Time 20 minutes When Once a month Tools Radiation meter Procedure 1 With the X ray generator on at normal settings and the shutter closed use the radiation meter to sweep the area around the X ray tube housing fast shutter and collimator for any radiation leak inside the enclosure Close the protective enclosure doors and open the X ray shutter command sh o in CrysAlisP o 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 enclosure window and the door seals Record details of the test in the local radiation log
39. ection on the rear panel of the generator Check that the collimator is fitted to the microfocus source HV On is not possible The x ray tube may be too hot cooling water may not be flowing through the microfocus source or the emergency stop may have been pressed Check that the emergency stop button is released Check that the water cooler generator module is switched on and showing no error states Check that the generator temperature error LED is not on Then switch off the generator on the front panel and switch on again to reset the status Switch on HV Temperature error LED is lit X ray tube has overheated and HV has been switched off Switch off the generator on the front panel and switch on again to reset the status Contact Agilent XRD Support for advice before proceeding Safety shutter does not open and intermittent alarm is sounding Beamstop is up Lower the beamstop Safety shutter does not open but without alarm sounding Protection cabinet panel or door is open Close protection cabinet panels and doors HV is on but cannot set mA above zero kV setting is too small Set kV to at least 10 and then raise mA setting kV setting is correct but no emission is possible X ray tube filament may be broken Contact Agilent Technologies to change the tube kV or mA error LED lights when changing settings Setting is ramping quickly so that actual value lags behin
40. ed either in the AirCooler or inside the left side of the electronics rack for water to water cooling option The software may report to the user a water level warning and if no action is taken later a water level error which will shut down the water cooler for the CCD detector The front panel of the water chiller in the electrical rack will also show this warning with a flashing LED In case of this warning or error the user is required to refill the reservoir The procedure is as follows 1 bes npo Water to water version Open the left side panel of the electronics rack by turning the locks at the top and bottom using the same key used to open the protection cabinet doors Locate the reservoir tank which is towards the front side of the rack Open the filling port on the top of the reservoir or on the top of the AirCooler Pre mix a solution of 10 ethylene glycol 90 distilled water If fitted locate the viewing window on the side of the reservoir Pour the solution into the filling port until the level is visible in the viewing window SuperNova Version 1 3 USER MANUAL Page 56 MAINTENANCE INSTRUCTIONS 7 If no viewing window is fitted then fill until just below the filling port 8 Close the filling port 9 Close the left side panel of the electronics rack 10 If the water chiller of the CCD detector had shut down due to the level error then open the front door of the electronics rack switch off the wate
41. er settings 50kV and 0 8mA for Mo Cu or 65kV and 0 62mA for Ag Use Crysalis software to choose the power settings The graphical interface is shown in Figure 13 below The SuperNova X ray generator will automatically ramp up the settings at the proper rate After reaching the operating values it is recommended to wait for 20 minutes to attain optimal x ray intensity Su perN ova Version 1 9 USER MANUAL Page 41 OPERATION SuperNova Device Control 4 Read values Voltage kV Current m4 Power w Temperature Set values Volage kV 50000 C Xray off Current m4 0 990 Xray o CITED Status Device connected X RAY Faults Status Status ERR g RIO Xray Indicator VC WERE mi ERROR Interlock closed i e water ok ENS 751 kP Temperature ERRORI Pump ON 9 indi S Safety shutter ERRORI Safety shutter open Lamp status Safety shutter lamp ERROR Fast shutter open Usage time 23h Atay lamp ERRORI O Calibration run Number of cycles 32 Yacuum ERRGR O X ray stop Log Figure 13 Crysalis interface to X ray generator 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 zer
42. erforming the beam alignment procedure Su perN ova Version 1 9 USER MANUAL Page 12 HEALTH AND SAFETY INFORMATION 4 Use appropriate X ray detection equipment to perform regular radiation checks as per any laboratory rules 5 Useonly genuine firmware X ray tubes X ray generators 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 Extreme Temperatures WARNING 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 1 9 Vacuum WARNING A 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 The CCD detector front panel is made from beryllium and can be easily damaged by a strong force by hand or a gentle force by a sharp instrument Such damage can result in vacuum implosion of the CCD detector There is danger of exposure to potentially toxic beryllium material In case of such an event take action to close the protection cabinet doors and panels and obtain specia
43. ers A similar procedure will be used for aligning other low temperature attachments Each of them will require a different compatible support ring to be attached to the support arm which is universal for all attachments The support rings for low temperature attachments from most major producers can be purchased from Agilent Technologies For low temperature attachments such as Oxford Instrument s Cryojet and Oxford Cryosystem s Cryostream the compatible support ring also allows the attachment to be translated up and down towards or away from the crystal and held in place with a side mounted locking screw Before proceeding with the alignment procedure ensure that the attachment has been translated to the bottom position closest to the crystal Su perN ova Version 1 9 USER MANUAL Page 53 MAINTENANCE INSTRUCTIONS Adjustment screws Figure 19 Helijet adapter plate screws 1 Retract the adjustment screws the support arm so that the support ring is clamped against the underside of the support arm The attachment screws might require tightening to provide sufficient clamping force through the springs Clamp this ring up against the plate Figure 21 Helijet alignment tip SuperNova Version 19 USER MANUAL Page 54 MAINTENANCE INSTRUCTIONS Place the alignment tip in the end of the Helijet nozzle Fit a metal pointer to the XYZ head as shown in the photo above and place on the goniometer Align optically the end of
44. erture to ensure the system can be assembled in its designated area 5 2 1 3 Electrical Services One single phase outlet 16A 200 240V 32A 100 120V is required Additionally four single phase outlets are required as described in a figure below 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 an external earth terminal The instrument is equipped with a terminal to attach an external protective grounding cable which should have a cross section of not less than 4mm The resistance between the ground connection and the instrument terminal should be not greater than 0 1 ohm This grounding connection should be made in a secure manner to avoid accidental disconnection Fit a line voltage regulator 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 2200VA with single phase output and one or two battery packs for example the following solution from APC would run SuperNova for about 200 minutes APC Sma
45. f required 6 5 Emergency Shutdown The emergency shutdown procedure should be used e If there is a fire or any other emergency requiring the evacuation of personnel from the area 6 5 1 Emergency Shutdown Procedure 1 Press red emergency stop button located on the front right of the SuperNova WARNING The emergency stop button will only shut down HV from the X ray generator Other equipment on the SuperNova system will still be powered on 2 Switch off all power at the mains electrical supply 3 Turn off mains water supply for water to water mode Su perN ova Version 1 9 USER MANUAL Page 43 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 WARNINGS 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
46. f 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 note that if the cabinet is open the Motion Enable buttons will need to be simultaneously pressed 9 Use the height adjustments on both the Head and the microscope equally to re centre the ball send back to Lower and repeat until there is no movement of the ball as the Goniometer moves between the two positions 10 Confirm that the left right position is ok for Upper as well as Lower 11 Adjust the focus on the microscope to bring the ball into sharp focus Once this process is complete the microscope should not need adjusting again unless it is knocked or extra weight is added to or removed from the support arm for example a low temperature environment is added or removed All sample centring should involve only the adjustments on the Head Ey us An indication that the microscope is not properly centred is if the sample cannot be centred to the middle of the video screen 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 widely 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 re
47. for X electronics rack ray source or CCD detector has an error as indicated Su perN ova Version 1 9 USER MANUAL Page 37 OPERATION High Voltage On High Voltage On INTLK Closed INTLK Closed INTLK Open Open kV RGLT Error kV RGLT Error mA RGLT Error mARGLT Error X Ray Tube Temp Error X Ray Tube Temp Error Safety Shutter Open Safety Shutter Open Safety Shutter Closed Safety Shutter Closed Figure 10 Status LEDs of SuperNova X ray generator 6 2 Microfocus X ray Source f Figure 11 Microfocus X ray source mounted on SuperNova diffractometer 6 2 1 X ray generation This unit generates a focussed beam of X rays during normal operation The microfocus X ray tube generates X rays when supplied with high voltage and filament current from the X ray generator unit The dual shutter blocks X ray emission from the source when either one of the two shutters is closed The shutters are positioned between the X ray tube and the focussing optics X rays shine onto the optics only when both shutters are opened N WARNING The X ray tube is contained within a shielded housing The shielding should NEVER be removed whilst the high voltage generator is active as this would cause human exposure to damaging X rays The tube shield housing should only be removed by fully trained operatives Su perN ova Version 1 9 USER MANUAL Page 38 OPERATION The alignment and performance of the X ray
48. ge CCD detector to sample distance Response time Four circle Kappa geometry goniometer 10 2 kg 0 00125 deg for Omega and Theta 0 0025 deg for Kappa 0 005 deg for Phi 0 005 to 3 0 deg sec 115 to 157 deg 40 to 150 mm depending on the detector 3 ms SuperNova USER MANUAL Version 1 9 Page 19 3 4 Electrical Data SPECIFICATIONS Power connection Maximum power consumption Maximum mains current Main fuse Ground terminal X ray Generator 1 N AC 200 240V optionally 100 120V 50 60 Hz 100W 1 2A 6 3A None Goniometer Interface CCD Detector 1 N AC 200 240V optionally 100 120V 1 N AC 200 240V optionally 100 120V 50 60 Hz 50 60 Hz 250 W 125 W 12 12 6 3 A 3 15 A 2 5 mm Cu 2 5 mm Cu Power connection Maximum power consumption Maximum mains current Main fuse Ground terminal Water Cooler 1 N AC 100 230V 50 60 Hz 500W 2 4A 230V T 3 15A 230V T6 3A 110V 2 5 mm Cu AirCooler radiator 1 N AC 100 230V 50 60 Hz 80 W 0 3A T 1A 230V T2A 110V 2 5 mm Cu SuperNova USER MANUAL Version 1 9 Page 20 4 Technical Description 4 1 Overview of SuperNova The SuperNova system consists of 1 An instrument cabinet with electronics rack 2 Aircooler only if water to air option is chosen 3 A stand optional component for the computer monitor keyboard and mouse 4 System software installed on PC worksta
49. he 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 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 Su perN ova Version 1 9 USER MANUAL Page 10 HEALTH AND SAFETY INFORMATION WARNING Mains voltages are present in the system High voltages are used by the X ray tube and power supply Only personnel qualified to work with high voltages and currents are permited to perform service or maintenance work on such equipment 1 3 Mechanical Handling Safety WARNING Lifting points are provided for safe handling of components and safe handling A practice must be observed to comply with local
50. list assistance to clean up the beryllium The microfocus X ray source uses a diaphragm pump to evacuate internal parts of the unit Due to the limited degree of vacuum pumping there is little risk of implosion Nevertheless care should be taken and the unit must not be disassembled while still under vacuum 1 10 High Pressures WARNING A 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 Su perN ova Version 1 9 USER MANUAL Page 13 HEALTH AND SAFETY INFORMATION 1 11 Hazardous or Toxic Materials Beryllium and beryllium oxide are toxic materials Follow appropriate handling shipping use storage and disposal procedures and regulations Refer to BrushWellman Material Safety Data Sheet No M10 for further information Beryllium is contained in the front panel of the CCD detector and in the X ray tubes Care should be taken not to touch the beryllium panels windows on the detector and tubes WARNING A 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
51. me 70 is located in the electronics rack in the instrument cabinet The KMW70 Water Cooler device can work with water to air or water to water heat exchangers To transfer the unit from one mode to another some extra parts are required They can be purchased from Agilent Technologies and will require assembly by an Agilent Technologies engineer Su perN ova Version 1 9 USER MANUAL Page 24 TECHNICAL DESCRIPTION KMW70 Water Cooler in water to air operation requires an external Air Cooler see Figure 6 This device transfers the heat to the environment and does not require an external ie tap water supply While operating in water to water mode the device contains a water reservoir see Figure 7 on the left hand side of the electronic rack This reservoir is used to fill internal circuits It also needs an external water supply tap water integrated building water circuit or additional water chiller such as Thermoflex 900 to cool the device The heat from the internal circuits is delivered to the external water circuit To fill the reservoirs in the rack or AirCooler use 1 10 solution of distilled water with ethylene glycol to prevent the liquid and circuits from algae growth 3L of liquid should be used to fill the reservoir and an additional 3L of liquid should be needed to fill the pipes The filling ports is on the top of the AirCooler reservoir in the rack Figure 6 Air Cooler module Su perN ova Version 1 9 USER MANU
52. mote control except home should be one small division on the display 10pm In the unlikely event that correct centring cannot be achieved contact Agilent Technologies for advice 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 screen This is an optical illusion caused by the angle of the microscope with respect to the Crystal at Home and can be ignored Su perN ova Version 1 9 USER MANUAL Page 49 MAINTENANCE INSTRUCTIONS 8 3 Checking the Door Safety Interlocks Task Time 2 minutes When Once a week Tools None Procedure WARNING Ensure the interlocks are not defeated No warning buzzer to be heard If interlock defeated there is the risk of exposure to X ray radiation 1 With the diffractometer in normal operation and at normal X ray generator settings with the shutter open open the front doors of enclosure cabinet The X ray shutter should immediately close 2 Close the enclosure doors From the software open the shutter again 3 Open the side panels of the cabinet The X ray shutter should immediately close 4 Close the side panels From the software open the shutter again 5 Open the back panel of the cabinet X ray shutter should immediately close 6 Close the back panel 7 Record the date persons testing and sign off the outcome 8 4 Ch
53. n 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 CrysalisPro Blank images due to X ray shutter not opening 1 Protection cabinet doors are not closed properly Ensure all doors panels are closed and secured If the safety circuit is closed a green lamp is illuminated within the control electronics Access is via the top panel of the electronics cabinet behind the front door SuperNova USER MANUAL Version 1 9 Page 61 TROUBLE SHOOTING Symptom Fault Solution 2 Shutter open closed lamps are defective To check if LED arrays are working turn off the interface wait 5b seconds and turn back on the interface For a short period all shutter indicators should be illuminated e g open closed on the exterior of the cabinet and the Shutter Open red lamp inside the cabinet on the beamstop mounting If the LED arrays do not function as indicated contact Agilent XRD Service 3 X ray generator is not turned on or is not generating X rays 1 Ensure generator is turned on and that the software indicates that X ray power settings are normal 2 Ensure that the orange X ray LED array is illuminated see section above for fault finding the X ray generator system 4 Shutter signal cable Ensure that the shutter cable Fischer connection is secured to the optics
54. ntrolling one or two high voltage X ray tubes shutter operation and safety interlocks It also supplies power to a pump to create vacuum in the X ray optics and contains the vacuum measurement gauge It has been designed to operate with the microfocus X ray source from Agilent Technologies which is described in a separate manual The figure below shows two high voltage supplies mounted side by side inside the generator enclosure 245542222 Figure 5 Inside SuperNova X ray generator The range of voltage is 10 50kV The supplied high voltage cable should be connected between the X ray tube and the module at the back of the SuperNova X ray Generator The generator power trips out if the X ray tube overheats Warning lights on the front panel indicate the operational status of the generator The SuperNova generator also contains the sensor to monitor the vacuum maintained inside the microfocus X ray source This unit may be specially ordered to operate the Agilent Technologies microfocus X ray source containing the Ag X ray tube In this case there are some differences from the standard build of the unit Only one X ray source can be connected in this case dual source is not available The range of voltage is 10 65kV The Ag X ray tube should be connected the side of the unit which is referred to as Cu in the standard build The Mo side of the unit is unused in this special configuration 4 4 Water Cooler The Water Cooler model na
55. o ensure that the CCD detector is not damaged Typically air conditioning should be installed to maintain the temperature and humidity within the ranges listed below The Relative Humidity is particularly important as the CCD and its cooling pipes can reach 15 C condensation should not be allowed to collect on the CCD at any time SuperNova may be cooled using either ambient air or an external water supply but this decision must be made when ordering the instrument and Agilent Technologies should be informed so that the hardware can be pre configured before shipment The configuration may also be changed at the installation by Agilent Technologies engineers but extra cost will be incurred The environmental requirements for both configurations are shown below Air temperature in the room during operation 18 25 C SuperNova dissipates 4000 BTU hr heat not including any optional cryogenic devices Stability of ambient temperature during 1 C 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 strength Able to bear system weight of 450 kg on a footprint 80x60 cm Su perN ova Version 1 9 USER MANUAL Page 16 3 2 Services 3 2 1 Electrical Supply SPECIFICATIONS Total power requirements Number of outlets required Voltage fluctuation Location of outlets Protection
56. o 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 Version 1 9 Environmental Information SuperNova USER MANUAL 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 Page 4 Version 1 9 Important Information This user manual applies to the SuperNova system manufactured in Poland by Agilent Technologies Singapore International ATSI Product SuperNova single or dual source Model Type CCD Eos EosS2 Atlas AtlasS2 Titan or TitanS2 Electrical Ratings 1 N AC 200 240V 50 60Hz 900W optionally 100 120V 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 Man
57. o settings and then turn off HV using CrysalisPre software improves lifetime of the x ray tube 2 Park the goniometer in its home position simply by exiting the CrysAlisP e program 3 Turn off the cabinet amp sample illumination using the front panel mounted switches 4 Warm up turn off sample cooling device following manufacturers guidelines where applicable 5 Shutdown the PC and turn off computer Monitor 6 4 2 Shutdown Procedure Diffractometer not expected to be used for 1 3 weeks 1 Follow the Shutdown Procedure Diffractometer not expected to be used for 2 3 days 2 Turn off x ray generator by using the key switch on the front panel 3 Turn off the diffractometer interface red illuminated switch located on the left side of the front face 6 4 3 Shutdown Procedure Diffractometer not expected to be used for more than 3 weeks 1 Follow the Shutdown Procedure diffractometer not expected to be used for 1 3 weeks 2 off the Water Cooler which in turn shuts down the CCD detector It is advisable to leave this item running unless absolutely necessary Cooling the CCD detector from room temperature will be the time limiting factor when re starting the diffractometer Su perN ova Version 1 9 USER MANUAL Page 42 OPERATION 3 Turn off system power using red switch on top panel inside front door of electronics rack 4 Turn off mains water supply for water to water mode 5 Unplug system power cords i
58. oduces X rays when energised CAUTION Risk of finger squeeze between moving parts gt gt gt 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 WARNING Do not take risks You have a responsibility to ensure the safe condition and safe operation of equipment Su perN ova Version 1 8 USER MANUAL Page 9 HEALTH AND SAFETY INFORMATION WARNING 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 SuperNova 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 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 electric shock electric burn fire of electrical origin electric arcing 1 2 2 Recommended Precautions N WARNINGS 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 t
59. on Meaning Orange light X ray Red light Shutter open Green Light Shutter closed Outside top right of the protective enclosure Outside top right of the protective enclosure Outside top right of the protective enclosure X ray power is on X ray shutter open X ray shutter closed Red light Inside enclosure on top of microfocus source X ray shutter open Green light Inside enclosure on top of microfocus source X ray shutter closed Green LEDs Generator front panel right Inside front door of High voltage module s fitted Orange LEDs electronics rack Generator front panel right Inside front door of electronics rack inside and enabled for operation High voltage is ON Interlock is closed thus enabling shutter operation Safety shutter open closed indicators Red LEDs Generator front panel right Inside front door of Interlock is open thus disabling electronics rack shutter operation Error indicators as indicated Green LEDs Water cooler front panel right Inside front door of Water cooler circuit either for X Orange LEDs electronics rack Water cooler front panel right Inside front door of electronics rack ray source or CCD detector is operational Water cooler circuit either for X ray source or CCD detector has closed interlock for source or CCD operation to be activated Red LEDs Water cooler front panel right Inside front door of Water cooler circuit either
60. ostream User Manual Oxford Cryosystems optional Helijet User Manual Agilent Technologies optional SuperNova Version 18 USER MANUAL Page 67 ADDITIONAL INFORMATION 12 2 Drawings REX marem i Only required if no I Water 1 T 1 water to air cooler is to alves Filter and pressure regulator I i setto 3 bar supply B M l PEES I2 21 271 2 21 AE EEE ELE EEE ER EEE BEER ERE CER E EEG 16A single phase all systems 230 240V 20A single phase all systems 115 120V 16A single phase Electrical supply 105 cm 16A single phase 70 cm E y AIT PIAA IIA II ADT optional Min Ceiling height 2 2M Figure 23 SuperNova Suggested Layout SuperNova Version 1 3 USER MANUAL Page 68 ADDITIONAL INFORMATION SuperNova Dimensions in cm Figure 24 SuperNova System Dimensions extended cabinet Su perN ova Version 1 9 USER MANUAL Page 69 APPENDICES Appendices Appendix 1 X ray Tubes Wavelengths Anode Kao Kao Kf Kao Cr 2 28976 2 2 293663 6 2 08492 2 1 00170 Co 1 78901 1 1 79290 1 1 62083 2 1 00217 Cu 1 540598 2 1 544426 2 1 39225 1 1 00248 Mo 0 7093187 4 0 713609 6 0 632305 9 1 00605 Ag 0 5594214 6 0 563812 4 0 497081 4 1 00785 W 0 180199 2 0 185080 2 0 158986 3 1 02709 Appendix 2 Standard Crystal Pa
61. ove The first is to adjust the focal length of the unit the next has the equivalent adjustment to the height of the sample on the Goniometer when sample is in Lower or Upper position Finally there is the left right adjustment To centre both the video screen and check the Sphere of confusion use the following procedure Procedure 1 Press F12 on the computer keyboard to start the alignment procedure a new window opens Su perN ova Version 1 9 USER MANUAL Page 48 MAINTENANCE INSTRUCTIONS 2 Mount the 0 3mm steel ball onto the Goniometer 3 Press the Lower then 0 buttons and wait for the Goniometer to stop moving note that if the cabinet is open the Motion Enable buttons will need to be simultaneously pressed 4 Find the steel ball on the video screen using the Goniometer Head adjustments 5 Press 180 and watch the steel ball as it is rotated it will probably move off screen 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 centre of the screen 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 o
62. r chiller using the front panel illuminated switch wait 55 and switch on again 11 The system should then restart automatically Observe that the level error LED is not illuminated on the front of the water chiller 12 Close the front door of the electronics rack Su perN ova Version 1 9 USER MANUAL Page 57 9 Trouble Shooting TROUBLE SHOOTING Symptom Fault Solution X ray shutter will not open 1 Protective cabinet doors or side panels are not closed properly Close doors and side panels properly 2 X ray generator signal light defective Check light connections and bulb Replace bulb 3 Beamstop is in up position Move beamstop to down position to block x ray beam 4 Shutter open and or shutter closed lights defective Check light connections and bulbs Replace bulbs 5 Protective cabinet doors were opened whilst the shutter was open and safety circuit was activated In CrysAlis e re start experiment Intermittent beeping sound from the system Beamstop is in up position Move beamstop to down position to block x ray beam Vacuum pump does not start Power is not connected to the vacuum pump Connect cable between power output on X ray generator rear panel and the vacuum pump Vacuum pump is noisy Sufficient vacuum cannot be created in the x ray optics Check the vacuum pipe is securely fitted between the pump and the y piece in the enclosure
63. r on the stand for optional equipment Further details can be obtained from Agilent Technologies Su perN ova Version 1 9 USER MANUAL Page 27 TECHNICAL DESCRIPTION 4 8 Safety Features During operation X rays are generated and projected in a totally enclosed cabinet constructed of steel and lead equivalent glass SuperNova has magnetic switches interlocked to safety system mounted on the front door and rear left and right side panels of the protective enclosure During operation the X ray shutter will not open unless the door and panels are closed If the door or panels 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 door is required when changing samples When the door is opened during sample change and alignment the X ray generator remains on for optimum performance but the safety shutter is automatically closed 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 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 and green shutter lights The door of the cabinet should remain locked when the system is unattended to prevent unauthorised access to the system Su perN ova Version 1 9 USER MA
64. rack and stop goniometer Motion Enable Two metallic Inside the protection cabinet in Pushing and holding both push buttons front of the goniometer buttons simultaneously enables goniometer movement while the protection cabinet is open Cabinet Illumination Small black Front of protection cabinet Illuminate inside of enclosure button Sample illumination Small black Front of protection cabinet Illuminate crystal sample button 6 1 2 Power Control Type Location Effect Diffractometer Red switch Interface front panel left Inside Power on off to goniometer goniometer front door of electronics rack interface X ray Generator Key lock Generator front panel left Inside Power on off to X ray switch front door of electronics rack generator Water cooler Red switch Water cooler front panel left Power on off to cooling modules Inside front door of electronics rack DC power supply Switch Inside rear door of electronics Power on off to CCD detector rack underneath power supply SuperNova USER MANUAL Version 1 9 Page 35 OPERATION Cabinet Illumination Switch Sample Illumination Main power switch to whole rack System interface power switch HV generator power switch key locked Water cooler power switch Figure 9 Location of switches SuperNova Version 19 USER MANUAL Page 36 6 1 3 List of indicators OPERATION Indicator Locati
65. rameters Compound name Compound formula Cell constants Appendix 3 Ylid 2 Dimethylsulfuranylidene 1 3 indandione C10H1002S a 5 947 b 9 026 18 399 a y 90 Temperature Scales Conversion To convert Fahrenheit to Celsius To convert Celsius to Fahrenheit To convert Celsius to Kelvin To convert Fahrenheit to Kelvin Appendix 4 Maintenance Records subtract 32 from F then multiply by 5 9 multiply by 9 5 then add 32 add 273 15 first convert F to C then add 273 15 C 5 9 F 32 9 5 32 K C 273 15 The attached record sheets are provided as examples of the type of records of maintenance checks that should be completed for SuperNova These records are to show only that maintenance has been completed as directed Version1 4 Page 1 SuperNova USER MANUAL APPENDICES in this manual Other maintenance records should be kept as required by any local national or international regulations Weekly Maintenance Record Sheet Week Date of Name of person performing Signature Comments No maintenance test 20 21 22 Su perN ova Version 1 9 USER MANUAL Page 2 APPENDICES Weekly Maintenance Record Sheet Week No Date of maintenance Name of person performing test Signature Comments 23 24 25 26 27 28 29
66. rce and Nova the Cu source The optics are positioned with a combination of piezoelectric motors and manual adjustment screws It has been designed to operate with the SuperNova X ray generator and Water Cooler from Agilent Technologies which are described in separate manuals The microfocus X ray tube is connected to a module to produce high voltage and filament current which is located inside the SuperNova X ray generator unit The range of voltage is 10 50kV The supplied high voltage cable should be connected between the X ray tube and the module inside the SuperNova X ray Generator The microfocus X ray source contains both a fast shutter and a safety shutter The safety shutter is for safety purposes only and cannot react fast enough to make time controlled exposures of a CCD detector Fast exposures are created using the fast shutter The safety shutter is controlled from the SuperNova X ray generator unit and the fast shutter from the System Interface As a special configuration SuperNova may be ordered with a single Ag microfocus source and modified X ray generator with a range of voltage 10 65kV 4 3 SuperNova X ray Generator SuperNova systems are supplied with the Agilent Technologies SuperNova X ray generator Su perN ova Version 1 9 USER MANUAL Page 23 TECHNICAL DESCRIPTION The X ray generator is located in the electronics rack in the instrument cabinet This unit contains power supplies and electronics associated with co
67. reading kV and mA from generator Ethernet cable s not connected properly Check Ethernet connections between PC and hub right side of electrical enclosure and between generator and hub SuperNova USER MANUAL Version 1 9 Page 59 TROUBLE SHOOTING Symptom Fault Solution Goniometer lost angle positions from memory 1 Power loss to goniometer 1 Restore power to SuperNova restart the and CrysAlis program 2 Switch off the SuperNova interface wait 5 seconds and then switch on 3 In CrysAlis e open command prompt and type KM4 MGCUTIL and press enter 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 F or 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 Select Hsync all and click Start Note that at the end of the Hsnync operation the Hsync flags should read 1 This is located on the text line below the parameter button Click on OK 8 Type gon reinit in the command bar and press enter This will reinitialise all drives and
68. rols and 35 controls re Hc t n 35 6 1 2 POWOIZ S s ai et en ec tasa entia ea ebbe mE t bsp se deve e RENE Pape 35 6 1 3 Eist of indicators Pp 37 6 2 Microfocus X ray Source a 38 6 2 1 X ray generation 5 2 1 ot caedi ead en Ede danse aay 38 62 2 Water Cooling dere deut td rut 39 6 2 3 Temperature SernsQr e n aet RN RR NER e NR REA 39 6 2 4 Vacuum puimp eene edet entere ee de deta 39 6 2 5 5 40 6 2 6 Beamstop rotation 40 6 3 System Startlp ie Tate e etri M re vede Gi disses daw cer adt Mage ove 41 6 3 1 Microfocus X ray Tube Warm up Procedure 41 6 4 System Standby and Normal Shutdown Procedure ueeeeeeeeeeseeeeee esent nnn nnne 42 6 5 Emergency SHUtdOWN a i e ten hend e e Sg 43 6 5 1 Emergency Shutdown Procedure 43 7 Maintenance Schedules 44 T Introductionis oie o cinia type errat d apa e P EET E
69. rt UPS XL 2200VA 230V Tower Rack Convertible 2 SUA48XLBP Battery Units Description Voltage Frequency Maximum nominal V Hz mains current A X ray generator 100 240 50 60 1 2 Water cooler 100 240 50 60 2 5 CCD detector 90 130 180 260 50 60 2 5 Goniometer Interface video 90 130 180 260 50 60 2 5 monitor halogen lamp sample illumination Computer and peripherals 100 240 50 60 2 5 Cryojet controller option 100 240 50 60 2 Autofill controller option 100 230 50 60 0 6 Su perN ova Version 1 9 USER MANUAL Page 32 HANDLING INSTALLATION ETC 5 2 1 4 Water Supply if water to air chiller is not used A cooling system is required to dissipate the heat produced by the X ray tube A closed circuit cooling system is supplied to minimise the effects of particles low pressure and water temperature fluctuation on the performance of the system from local tap water supply The Chiller is a closed circuit cooling system suitable for this purpose It is supplied with hoses that have a 10mm inside diameter The distance between the water supply and the chiller is not limited but the supply must deliver 1 3 bar gauge pressure with a minimum 1 8 litres min flow The water supply should have a wall mounted shut off valve 5 2 1 5 Low Temperature Option A suitable high vacuum pump ideally 70 Litres sec turbo is required to periodically evacuate the vacuum legs of the cooling device To demonstrate the opera
70. the metal pointer using the XYZ screws on goniometer head with the centre of the goniometer using the F12 command from the CrysalisPre software Adjust the Helijet alignment screws until the alignment tip nearly comes in contact with the end of the metal pointer By screwing in all of the alignment screws equally the Helijet will move down towards the pointer and vice versa By screwing in only one of the alignment screws the Helijet will move sideways relative to the pointer Ensure all four of the adjustment screws are touching the support ring and are not loose in space above the ring Ensure all four attachments screws are tight so that the Helijet remains clamped in the aligned position Remove the goniometer head Remove the alignment tip 8 8 Cleaning Water Filters Task Time 2 hours When Once a year or as required Tools Large size spanner Container to catch water spillage Cleaning brush In order to clean the CCD coolant filter the CCD detector will need to be turned off for a period of time while the filter is opened This will cause the CCD to warm up and therefore this procedure should not be carried out frequently but only on a regular preventive maintenance visit or in the case of a coolant flow error on the CCD detector circuit Procedure 1 UseCrysAlisPro software to turn off the X ray source power Wait for the active source power to ramp down to zero 2 Open the front door of the electronics rack 3
71. tion Figure 2 Computer and monitor SuperNova USER MANUAL TECHNICAL DESCRIPTION Note The numbers on this figure refer to the numbered list above Version 1 9 Page 21 TECHNICAL DESCRIPTION The diffractometer and CCD area detector are mounted inside a cabinet The cabinet experiment area is mounted on top of the electronics rack The water cooler for the CCD detector and the X ray source is positioned in the electronics rack A stand to the side of the system supports the control PC monitor keyboard and mouse The diffractometer consists of one or two X ray tubes 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 detector or scintillation point detector The CCD area detector and the point detector are used to measure the X quanta diffracted from the sample Key 1 X ray tube 4 Collimator 2 4 circle Kappa goniometer 5 Beamstop 3 X ray Shutter 6 Beryllium Window Figure 3 View of a typical diffractometer The X rays are generated by a micro focus 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 X ray focussing optics and a collimator for refining the X ray beam The sample can be viewed with the video microscope which is attached to the stand
72. tion of a cooling device such as Cryojet or Cryostream 100 litres of liquid nitrogen are required The customer should supply a suitable rack or table for the cooling device controller 5 2 1 6 CCD Camera Pumping A suitable high vacuum pump ideally 70 Litres sec turbo molecular 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 Table shelving for cooling device controller and a table pedestal stand for the computer monitor keyboard and mouse 5 2 2 2 Personnel Required for Installation 5 persons for lifting of heavy components 5 2 3 Installation Procedures Agilent Technologies personnel perform the installation The duration of the installation is typically 3 working days with an additional 1 day for the low temperature option This is followed by 2 days training from an Agilent Technologies applications engineer 5 2 3 1 Movement of system on wheels The SuperNova system is equipped with feet which include integrated wheels Note the following 1 foot is moved vertically using the red adjusting wheel such that the weight of the system is applied either through the wheel or the foot 2 During operation the system must be
73. tors WARNING A Injury could result if clothing or body parts become caught in moving mechanisms Keep clothing hands and body parts away from moving mechanisms Su perN ova Version 1 9 USER MANUAL Page 11 HEALTH AND SAFETY INFORMATION 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 When the protection cabinet is open the goniometer moving parts are disabled The SuperNova system contains two MOTION ENABLE switches in front of the goniometer inside the protection cabinet During some operations such as mounting a sample the goniometer must be moved between defined positions while the protection cabinet is open In order to do this BOTH Motion Enable switches must be pressed and held simultaneously and this ensures that both hands of the operator are kept away from the potential finger squeeze or shear locations In the event that the goniometer moving parts become blocked by an obstruction the movement will be automatically stopped and a small reverse movement made so that the blockage can be safely released The control software will report a movement error and will wait for user intervention The procedure to follow to restart the instrument is shown in the tro
74. tube depends on the correct setting within the generator unit When initially provided by Agilent Technologies the X ray generator will be correctly set for the associated microfocus X ray source The microfocus X ray tube is a consumable item which in time will need to be replaced This should only be carried out by an Agilent authorized service provider The voltage should be increased before the current in order to ensure proper X ray tube operation Thus current cannot be increased above zero until a minimum of 10kV has been set on the voltage parameter The maximum parameters are 50kV and 1 in the standard configuration and 65kV 1mA in the special build for Ag X ray source The Ag source contains a filter mounted between the tube and focussing optic which is not removable by the user Only Agilent Technologies service engineers may make modifications to the filter 6 2 2 Water cooling Generation of X rays causes the production of heat and thus the microfocus X ray source requires water cooling for removal of heat and high stability of the temperature On the underside of the source unit there are two quick connectors for the input and output of cooling water The direction of water flow is not important The Water Cooler unit should be used to supply cooling water to the microfocus X ray source The X ray generator unit is interlocked to the cooling unit and thus high voltage cannot be applied until cooling water is flowing norm
75. ual the protection provided by the equipment may be impaired Important Health and Safety Notice When 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 SuperNova service and support is available for technical and operational issues as indicated below e Web www agilent com chem contactus E mail XRDSupport agilent com 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 registrations Copyright 2014 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 Original instructions in English language Su perN ova Version 1 9 USER MANUAL Page 5 Contents 1 Health and Safety Information 9 VV GONG Val oss gt
76. ubleshooting section of this user manual 1 7 X ray Radiation WARNING This equipment contains X ray tube Ensure that safe working practices relating to radiation are employed WV Owners and operators of the equipment are responsible to follow any local national or international rules and guidelines related to X ray equipment 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 National Radiological Protection Board NRPB in the UK For use in the UK the lonising Radiations Regulations 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 WARNINGS To prevent injury to personnel and possible damage to the equipment please note the following guidelines 1 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 2 Never dismount the beam stop when the system is operational 3 Do not operate the system without the collimator unless p
77. va Version 1 9 USER MANUAL Page 39 OPERATION 6 2 5 Safety shutter operation The safety shutter will only open if the safety interlocks are closed This shutter is automatically controlled and will open and close depending on the interlock status The front panel of the X ray generator indicates whether the interlock circuit is open or closed If the beam stop is open then an intermittent alarm will sound The fast shutter also cannot be opened if the interlock is open If the protection cabinet is opened while the two shutters are opened then the interlock circuit is opened and causes the two shutters to close When the cabinet is closed again the safety shutter will automatically open but the fast shutter will remain closed until the user again commands it to open by the use of the software 6 2 6 Beamstop rotation operation The beamstop may be rotated between down and up positions The down position is for normal operation and covers the primary beam or two beams in the case of a dual source SuperNova to prevent them from reaching the CCD detector The up position moves the beamstop 90 degrees towards the rear of the instrument and thus opens access around the crystal position to aid crystal mounting especially when mounting in liquid nitrogen underneath a low temperature device such as Cryojet or Cryostream is required The beamstop must be moved back to the down position before making an X ray exposure The beamstop cont
78. vernment users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 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 to maintain the instrument in safe con

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