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MAINTENANCE INSTRUCTIONS
WARNING
Ensure that the X-ray tube is correctly mounted. Incorrect mounting may result in exposure of personnel to X-ray radiation. Red plastic spacers may need to be removed to ensure perfect fit of X-ray tube.
9. From the front of the Xcalibur insert the X-ray tube into the tube shield and secure.
NOTE
X-ray tube must be inserted the correct way up. See figure 9.3.1
Water in
TOP
Water out
Water in
TOP
Water out
RT FE
Mo
SEIF
AE
G
BOTTOM
Mount Seiffert and Philips X-ray tubes so that the tube label is upside down, as shown above, with the cooling water flowing in through the top and out at the bottom.
BOTTOM
Mount older tubes manufactured by AEG as shown in the diagram above
Figure 9.3.1 Position of the X-ray source
10. Secure temperature sensor to base of X-ray tube
11. Replace the front plate of the Enhance by tightening the two grub screws holding it to the optic housing
12. Reconnect water supply to back of X-ray tube shield
13. Switch on water and power to Xcalibur and chiller units.
14. Align X-ray optics as described below.
9.4 Changing the X-ray Tube of Enhance ULTRA
Task Time:
When:
30 mins
Sealed source X-ray tubes have a limited useful lifetime. Operation of a 3 kW tube at typical output of 2 kW will normally provide 10,000 hours of use (actual values may vary, see third party manual).
Note: X-ray tubes also have a limited shelf life.
Version 1.4 Xcalibur_Manual_v1.4
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Xcalibur
USER MANUAL
MAINTENANCE INSTRUCTIONS
Tools:
Set of Allen keys
Set of flat-headed screwdrivers
Water receptacle (e.g. Bucket)
Procedure
1. Turn off all power and water to the Xcalibur system, KMW200CCD and KMW3000C chiller units
2. Leave for at least 20 minutes to ensure that the X-ray tube is not hot (test temperature before proceeding).
CAUTION
Have a receptacle ready to receive water from the pipes and X-ray tube shield.
3. Disconnect water pipes from back of Enhance Ultra X-ray tube shield (These are attached with quick release connectors).
4. Remove the Enhance ULTRA front face panel. Using a 3mm Allen key completely undo the screw 1 (see Figure 9.4.1) and lift off the front face panel.
5. Unscrew the temperature sensor from the front plate (metal base, with label) of the X-ray tube.
WARNING
Do not touch the Beryllium windows in the X-ray tube. Beryllium is a potentially toxic material.
6. Release the two screws holding the X-ray tube in place and withdraw the X-ray tube from the Xray shield. Do this by holding the front plate (metal base, with label) and pulling towards the front of the Enhance ULTRA. Ensure that the X-ray tube is held level and withdraw parallel to the X-ray shield.
7. For disposal of used X-ray tubes see the DISPOSAL chapter of this manual.
WARNING
Do not touch the Beryllium windows in the X-ray tube. Beryllium is a potentially toxic material.
8. Replace the x-ray tube with an identical specification Cu X-ray tube. Holding by its metal base, remove the new X-ray tube from its protective box.
WARNING
Ensure that the X-ray tube is correctly mounted. Incorrect mounting may result in exposure of personnel to X-ray radiation. Red plastic spacers may need to be removed to ensure perfect fit of X-ray tube.
9. From the front of the Enhance ULTRA insert the X-ray tube into the tube shield and secure with two screws.
NOTE
X-ray tube must be inserted the correct way up. See figure 9.3.1
10. Secure temperature sensor to base of X-ray tube
11. Remount the thermocouple and the Enhance ULTRA front face panel and secure in place using a 3mm Allen key and the screw 1 (see Figure 9.10.1).
Version 1.4 Xcalibur_Manual_v1.4
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USER MANUAL
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Table of contents
- 10 1. Health and Safety Information
- 10 1.1 General
- 11 1.2 Electrical Safety
- 11 1.2.1 Potential Electrical Hazards
- 11 1.2.2 Recommended Precautions
- 11 1.2.3 First Aid
- 12 1.3 Mechanical Handling Safety
- 12 1.4 Safe Mechanical Practice
- 12 1.5 Moving Parts
- 12 1.6 X-ray Radiation
- 13 1.7 Extreme Temperatures
- 14 1.8 Vacuum
- 14 1.9 High Pressures
- 14 1.10 Hazardous or Toxic Materials
- 14 1.11 Modifications and Service
- 15 2. Introduction
- 15 2.1 Scope
- 15 2.2 How To Use This Manual
- 15 2.3 System Overview
- 16 3. Specifications
- 16 3.1 Environmental Requirements
- 16 3.2 Services
- 16 3.2.1 Electrical Supply
- 16 3.2.2 Water Cooling
- 17 3.2.3 Helium Gas Supply (where applicable)
- 17 3.3 Performance Data
- 17 3.3.1 X-ray Tube (Typical Operating Conditions)
- 18 3.3.2 Sapphire 2 CCD Detector
- 19 3.3.3 Sapphire 3 CCD Detector
- 20 3.3.4 Onyx CCD Detector
- 20 Onyx CCD Detector Theta and Resolution Ranges
- 21 3.3.5 PC CCD Interface
- 21 3.3.6 Four-circle Kappa Geometry X-ray Goniometer
- 22 4.4 Electrical Data
- 23 4. Technical Description
- 23 4.1 Overview
- 24 4.2 CCD Detector Technology
- 25 4.2.1 Beryllium Window
- 26 4.2.2 Phosphor
- 26 4.2.3 Taper
- 26 4.2.4 CCD
- 26 4.2.5 Readout Speed
- 26 4.2.6 Binning
- 27 4.2.7 Dark Current and MPP Mode
- 27 4.2.8 Radiation Damage
- 27 4.2.9 Full Well Depth and 18-bit Digitisation
- 27 4.2.10 Anti-blooming
- 27 4.2.11 Vacuum
- 27 4.2.12 Fast Shutter
- 28 4.2.13 Zingers and Cosmic Ray Events
- 28 4.3 Four-Circle Kappa Geometry Goniometer
- 29 4.4 X-ray Generator
- 30 4.5 Software
- 30 4.5.1 Directory Structure
- 31 4.5.2 Basic Menu Philosophy
- 31 4.6 KMW200CCD Chiller
- 31 4.7 KMW3000C Chiller
- 31 4.8 Low Temperature Option
- 31 4.9 Safety Features
- 32 5. Handling, Installation, Storage and Transit Information
- 32 5.1 Reception and Handling
- 32 5.1.1 Delivery
- 32 5.1.2 Unpacking
- 33 5.1.3 Mechanical Handling
- 33 5.1.3.1 Weights, Dimensions and Lifting Points
- 34 Delivery
- 34 5.2 Installation and Setting to Work
- 34 5.2.1 Preparation of Site and Services
- 34 5.2.1.1 Environmental Requirements
- 34 5.2.1.2 System Layout
- 35 5.2.1.3 Electrical Services
- 36 5.2.1.4 Water Supply
- 36 5.2.1.5 Low Temperature Option
- 36 5.2.1.6 CCD Camera Pumping
- 36 5.2.1.7 Helijet Option
- 37 5.2.2 Setting to Work
- 37 5.2.2.1 Equipment Required
- 37 5.2.2.2 Personnel Required for Installation
- 37 5.2.2.3 Setting up Procedures
- 39 Storage
- 40 6. Operation
- 40 6.1 Controls and Indicators
- 41 6.2 Initial Switch on Procedure
- 42 6.3 X-ray Tube Warm-up Procedure
- 43 6.4 Software
- 43 6.4.1 Software Updates
- 44 6.4.2 Software Installation
- 44 6.4.2.1 MGC interface software
- 45 6.4.2.2 CrysAlis Software
- 45 6.4.3 Changing Machine Correction and Set-up Files
- 46 6.5 Normal Operation
- 46 6.5.1 General Commands
- 48 6.5.2 Changing Xcalibur Settings
- 52 6.5.3 Standard Diffraction Experiment
- 52 6.5.3.1 Crystal Mounting and Alignment
- 54 6.5.3.2 Diffraction Photographs to Determine Crystal Quality
- 55 6.5.3.3 Unit Cell Determination
- 57 6.5.3.4 Data Collection
- 58 6.5.3.5 Data Processing and Reduction
- 59 6.5.3.5.1 Orientation Matrix
- 60 6.5.3.5.2 Run List
- 61 6.5.3.5.3 Scan Width
- 61 6.5.3.5.4 Background Evaluation
- 62 6.5.3.5.5 Special Corrections
- 63 6.5.3.5.6 Outlier Rejection
- 64 6.5.3.5.7 Output Format
- 65 6.5.3.6 Changing the Output Format from Data Reduction
- 66 6.5.3.7 Absorption Correction
- 74 6.5.3.8 GRAL - Space Group Determination
- 80 6.5.3.9 Structure Solution and Refinement
- 80 6.5.4 Ewald explorer
- 86 6.5.5 Dc Movie - Replay of Data Collection Movie
- 87 6.5.6 Reconstruction of Precession Photographs
- 91 6.5.7 Dc opti - Optimisation of Data Collection Strategy
- 96 6.5.8 Indexing and Data Reduction of Incommensurate Samples
- 97 6.5.9 Indexing and Data Reduction of Twinned Samples
- 99 6.5.10 Extracting Data from Powder Samples
- 100 6.5.11 Refining of Machine Parameter File
- 103 6.5.12 Glossary of CrysAlis Commands
- 110 6.6 Normal Shutdown
- 110 6.7 Emergency Shutdown
- 111 6.7.1 Emergency Shutdown Procedure
- 112 7. Mechanical Changeover of Detectors and X-ray Sources
- 112 7.1 Interchange of CCD Detectors
- 112 7.1.1 Installation of a Sapphire 2 and Sapphire 3 CCD detectors
- 113 7.1.2 Removal of a Sapphire 2 and Sapphire 3 CCD detectors
- 113 7.1.3 Installation of the Onyx CCD camera
- 116 7.1.4 Removal of the Onyx CCD camera
- 117 7.2 Procedure for Interchange of the Molybednum and Copper Enhance X-ray Source
- 121 8. Maintenance Schedules
- 121 8.1 Introduction
- 121 8.2 Weekly Maintenance Schedule
- 121 8.3 Monthly Maintenance Schedule
- 122 8.4 Six Monthly Maintenance Schedule
- 122 8.5 Yearly Maintenance Schedule
- 123 8.6 10,000 Hours Maintenance Schedule
- 124 9. Maintenance Instructions
- 124 9.1 Special Tools
- 124 9.2 Refining the Machine Parameter File
- 125 9.3 Changing the X-ray Tube of Enhance
- 126 9.4 Changing the X-ray Tube of Enhance ULTRA
- 128 9.5 X-ray Beam Stop Alignment
- 129 9.6 Changing the Collimator of Enhance
- 130 9.7 Changing the Collimator of Enhance Ultra
- 130 9.8 Aligning the X-ray Collimator of Enhance
- 130 9.9 Aligning the Enhance X-ray Source
- 133 9.10 Aligning the Enhance Ultra X-ray Source
- 133 9.10.1 X-ray Beam Alignment of Enhance Ultra
- 135 9.10.2 Optic Alignment of Enhance Ultra
- 136 9.10.3 Collimator Alignment of Enhance Ultra
- 136 9.10.4 Aligning the beam to the centre of the goniometer – Enhance Ultra
- 137 9.11 Checking the Door Safety Interlocks
- 137 9.12 Checking the Emergency stop
- 138 9.13 Checking the X-ray Radiation Levels
- 138 9.14 CCD Detector – Pumping Out Vacuum
- 140 9.15 Dismantling Xcalibur
- 143 10. Trouble Shooting
- 146 11. Spares
- 148 12. Disposal Instructions
- 148 12.1 X-ray Tube and CCD Detector
- 148 12.2 Third Party Equipment
- 149 13. Additional Information
- 149 13.1 Third Party Information
- 150 13.2 Drawings
- 150 13.2.1 Mechanical Drawings
- 150 Xcalibur Suggested Layout
- 150 System and Component Dimensions
- 152 13.2.2 Electrical Drawings
- 154 14. CE Conformity notice
- 155 Appendices
- 155 Appendix 1 X-ray Tubes Wave Lengths
- 155 Appendix 2 Standard Crystal Parameters
- 155 Appendix 3 Temperature Scales Conversion
- 155 Appendix 4 Maintenance Records
- 160 Appendix 5 Example of Local Rules for the Xcalibur System Set Up at Oxford Diffraction