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OPERATION
9. Mount CCD detector
Slide detector onto graduated mount from right hand side of Xcalibur (from front) and secure at
60 mm.
WARNING
Do not touch the Beryllium window at the front of the detector.
Beryllium is potentially toxic material.
10. Mount beam stop and collimator (where applicable).
Screw into position the beam stop.
WARNINGS
1. Do not touch the Beryllium window at the front of the detector.
Beryllium is potentially toxic material.
2. Ensure that the collimator is correctly fitted as incorrect mounting
may result in exposure of X-ray radiation.
Select the required size of collimator and push into position on the Xcalibur such that it is flush to the housing surface.
11. Mount video tower.
Screw into position.
12. Mount DC power supply.
Attach to support arm or back of goniometer table (Xcalibur PX).
13. Mount fibre-optic power supply.
Attach to support arm.
14. Mount video monitor.
Lift monitor into position and secure from below.
15. Mount video telescope camera.
Slide video camera into video camera support arm.
16. Connect halogen cabinet lights. Attach fibre-optic lights, cabinet vents and Xcalibur remote control.
17. Using 5 persons lift chiller units into position (see layout drawing OD-01-00-15).
18. Connect cables (Do not connect to mains power) and water pipes as per wiring instructions
(refer to electrical drawings and third party manuals listed in chapter 12).
19. Fill chiller water reservoirs (see the third party manuals).
20. Connect mains power. Turn on power as described in initial switch on procedure (chapter 6).
21. With the X-ray generator settings at 0 kV and 0 mA. Turn on water to chillers, very slowly at first and check for leaks around the X-ray tube shield and all water connections (including chiller units and the back of X-ray generator).
5.3 Storage
Before installation commences, or when the system is not being used for extended periods, store
Xcalibur in accordance with the environmental conditions for temperature and humidity stated in the
SPECIFICATIONS section of this manual.
Always store Xcalibur in a secure room
Version 1.4 Xcalibur_Manual_v1.4
Page 30
Xcalibur
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