oxford diffraction Gemini Series Pre-Installation Manual

Pre-installation Guide
Xcalibur and
Gemini
Diffractometer
January 6, 2006
Version 1.6
Oxford Diffraction Limited
68 Milton Park, Abingdon,
Oxfordshire. OX14 4RX. UK
Tel: +44 (0)1235 443630
Fax: +44 (0)1235 443631
http://www.oxford-diffraction.com
Contents
1. Pre-installation Check List.............................................................iii
2. Health and Safety Information ........................................................1
2.1 General.................................................................................................................................... 1
2.2 Electrical Safety....................................................................................................................... 2
2.2.1 Potential Electrical Hazards ........................................................................................... 2
2.2.2 Recommended Precautions........................................................................................... 2
2.2.3 First Aid .......................................................................................................................... 3
2.3 Mechanical Handling Safety.................................................................................................... 3
2.4 Safe Mechanical Practice........................................................................................................ 3
2.5 Moving Parts ........................................................................................................................... 3
2.6 X-ray Radiation........................................................................................................................ 4
2.7 Extreme Temperatures............................................................................................................ 5
2.8 Vacuum ................................................................................................................................... 5
2.9 High Pressures........................................................................................................................ 5
2.10 Hazardous or Toxic Materials ............................................................................................... 6
2.11 Modifications and Service ..................................................................................................... 6
3. Introduction ......................................................................................7
3.1 Scope ...................................................................................................................................... 7
3.2 How To Use This Guide .......................................................................................................... 7
3.3 System Overview .................................................................................................................... 7
4. Specifications...................................................................................8
4.1 Environmental Requirements.................................................................................................. 8
4.2 Services................................................................................................................................... 8
4.2.1 Electrical Supply............................................................................................................. 8
4.2.2 Mains Supply Water Cooling.......................................................................................... 9
4.2.3 X-ray Tube Cooling Water.............................................................................................. 9
4.2.4 Helium Gas Supply (where applicable).......................................................................... 9
4.3 Performance Data ................................................................................................................. 10
4.3.1 X-ray Tube (Typical Operating Conditions).................................................................. 10
5. Handling, Installation, Storage and Transit Information ............11
5.1 Reception and Handling........................................................................................................ 11
5.1.1 Delivery........................................................................................................................ 11
5.1.2 Unpacking .................................................................................................................... 11
5.1.3 Mechanical Handling.................................................................................................... 12
5.2 Installation and Setting to Work ............................................................................................ 14
5.2.1 Preparation of Site and Services ................................................................................. 14
5.2.2 Setting to Work............................................................................................................. 18
5.3 Storage.................................................................................................................................. 21
6. Drawings.........................................................................................22
6.1.1 Mechanical Drawings ................................................................................................... 22
6.1.2 Electrical Drawings....................................................................................................... 23
Appendix Example of Local Rules for the Xcalibur or Gemini
System Set-up at Oxford Diffraction ................................................25
PRE-INSTALLATION CHECK LIST
1. Pre-installation Check List
It is vital that your laboratory is fully ready when the Installation Engineer arrives to start work as there
is only a short time allocated. Please complete and return the following check list as soon as possible
confirming that you have read and understood our requirements and that your Laboratory will be
prepared in time. Failure to meet these requirements could result in the Installation not being completed
in the time allowed. Oxford Diffraction would expect the customer to contribute towards any extra costs
involved in completing an installation in these circumstances.
Full name
E-mail
_______________________________
_________________________________
Address _______________________________ Tel
_________________________________
_______________________________ Fax
_________________________________
YES
1.
I have looked at the suggested system layout drawing (OD-01-00-15-C) and have
allowed adequate space for the system and service access
1.1
The floor of the laboratory is capable of supporting a load of 500kg over an area of
0.64m2. If this is not the case it may be necessary to place a metal sheet on the floor to
spread the load.
2.
I have allowed an additional space on the left-hand side of the system for the low
temperature attachments
2.1
Liquid nitrogen and/or helium will be available at the beginning of the installation so that
the low temperature attachments may be demonstrated.
2.2
Helium Gas, (Purity 99.99%), will be available at the beginning of the installation (Helijet
only)
2.2.1
A turbo molecular pump, (capacity ≥70 l/min) is available for use in demonstrating the
Helijet
3.
Doorways to the room for installation are at least 85 cm wide
4.
A 3-phase 63A mains power supply with three single phase outlets (see drawing OD-0100-15-C) has been installed on the wall behind the system. For Gemini systems a further
32A single phase supply will be needed making a total of four outlets.
4.1
Connectors suitable for the mains outlets will be available when the Oxford Diffraction
service engineer arrives to carry out the installation. (If local rules require it an Electrician
may have to be arranged by the customer to make the connections)
5.
The mains supply is fitted with a circuit breaker as per drawing (see drawing OD-01-0014-C)
5.1
The power supply voltage fluctuates more than +/- 10%
5.1.1
If answered yes to 5.1 a line voltage regulator has been fitted
5.2
Four, ordinary single phase power outlets have been installed or are available, Ideally
using the third single phase 16A outlet from 4 above.
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Pre-installation Guide
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Page iii
NO
PRE-INSTALLATION CHECK LIST
YES
6.
A water supply (min flow 1.8 L/min) has been installed with a wall mounted shut off valve
6.1
60 L of filtered water will be available at the beginning of the installation (see chapter
4.2.3 for specifications)
7.
If providing own water cooling for the X-ray tube and generator, a flow sensor and
thermal switch are present to monitor cooling.
8.
An engine hoist / persons will be available to help with assembly
9.
Tables will be provided for computers and temperature controllers
10.
I have read and understood the pre-installation guide and all pre-installation work has
been completed
11.
Bottled Helium gas of grade 99.95% is available and fitted with a helium low pressure
regulator (for systems including Ultra Optics only).
12.
An Uncompensated Geiger Muller tube radiation monitor will be available to carry out a
critical examination of the equipment.
13.
24hr climate control is available in the laboratory where Xcalibur or Gemini will be
installed, and the Relative Humidity can be controlled to a non-condensing level.
See 4.1 below for details
NO
Available date for start of installation_____________________________________________________________ (dd/mm/yr)
Signature_______________________________________________ Date_______________________________
(dd/mm/yr)
PLEASE COMPLETE AND FAX TO OXFORD DIFFRACTION ON +44 (0)1235 443631
FOR THE ATTENTION OF DAVID WARNER
Xcalibur or Gemini
Pre-installation Guide
Version 1.6
Page iv
HEALTH AND SAFETY INFORMATION
2. Health and Safety Information
2.1 General
In normal operation the system is designed to operate safely. All users of Xcalibur and Gemini
systems 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
methods of working. A description of such potential hazards and how to avoid them is given in this
section.
This manual adopts the following convention:
WARNING
Indicates a potential hazard which may result in injury or death
CAUTION
Indicates a potential hazard which may result in damage to equipment
Warning symbols on the equipment are:
Protective conductor terminal
Earth (ground) terminal
CAUTION
Risk of electric shock
CAUTION
Refer to accompanying documents
WARNING
Radiation Hazard
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.
WARNING
Xcalibur and Gemini systems should only be operated and
maintained by authorised operators of the system. An authorised
operator is a person who has undergone specialist radiation training
and has been trained in the use of Xcalibur or Gemini systems by
Oxford Diffraction personnel.
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HEALTH AND SAFETY INFORMATION
2.2 Electrical Safety
In normal use the user is protected from the dangers associated with the voltage, current and power
levels used by the equipment. Only personnel qualified to work with the voltages and currents used
by this equipment should attempt to disconnect, dismantle or modify the equipment.
2.2.1 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
2.2.2 Recommended Precautions
WARNINGS
All of the electrical equipment supplied as part of the system should
be provided with a protective ground. Do not remove protective
grounds as this may give rise to an electrical safety hazard. It is
vitally important that the system is properly grounded at all times.
Follow local and national electrical regulations and procedures.
Do not defeat interlocks, remove connectors, disconnect equipment,
open safety covers, dismantle or modify equipment unless you are
qualified and authorised to do so and you are fully conversant with its
operation and potential hazards, or have total assurance through your
local electrical permit to work system that the equipment has been
made safe.
Ensure that the mains supply is fused at an appropriate rating, or
fitted with a circuit breaker, and that it can be isolated locally via a
clearly labelled, clearly visible and easily accessible isolating switch.
Isolate the supply before carrying out any maintenance work.
Never switch off the CCD detector’s power supply when the
KMW200CCD is operational. To switch off the CCD detector use the
KMW200CCD’s switch.
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 Xcalibur or Gemini systems’ electrical components.
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HEALTH AND SAFETY INFORMATION
2.2.3 First Aid
A course in first aid to include methods of artificial respiration is recommended for those whose
work involves equipment that may produce a high voltage.
WARNING
Do not attempt to administer first aid to someone who may have
suffered electric shock until the source of the shock has been
isolated.
Mains voltages are present in the system. High voltages are used by
the X-ray tube and power supply. These can cause serious injury or
death.
Only personnel qualified to work with high voltages and currents
should perform service or maintenance work on such equipment.
2.3 Mechanical Handling Safety
WARNING
Lifting points are provided for safe handling of components and safe
handling practice must be observed to comply with local regulations.
Check that lifting points are used only for the job intended.
The system itself and some components are heavy and require
careful handling. Use safe lifting procedures for heavy items to
prevent possible strain injury.
2.4 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
Oxford Diffraction to carry out service work on this equipment should attempt to dismantle, modify
or repair the equipment.
Water connections should be made and tested in accordance with any local and national safety
regulations.
2.5 Moving Parts
There are a number of moving parts in the system which are powered by electric motors.
WARNING
Injury could result if clothing or body parts become caught in moving
mechanisms.
Keep clothing, hands and body parts away from moving mechanisms.
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Version 1.6
Page 3
HEALTH AND SAFETY INFORMATION
2.6 X-ray Radiation
WARNING
This equipment contains an X-ray tube. Ensure that safe working
practices relating to radiation are employed. Follow any local,
national or international rules and guidelines.
Intentional or reckless misuse of the X-ray generator or its safety
devices including safety interlocks and cabinet shielding can result in
serious injury or even death.
During operation, there is an acceptable level of X-ray radiation as based on the recommendations
on risk published by the International Commission of Radiological Protection (ICRP) and endorsed
by the National Radiological Protection Board (NRPB) in the UK. For use in the UK, the Ionising
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
performing the beam alignment procedure.
4. Use appropriate X-ray detection equipment to perform regular
radiation checks as per any laboratory rules
Use only genuine firmware, X-ray tubes, X-ray generators,
monochromators, goniometer heads and collimators, as
recommended by your Xcalibur or Gemini supplier. Use of other
products may compromise the performance of the shielding and
safety system, and may invalidate your warranty.
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Version 1.6
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HEALTH AND SAFETY INFORMATION
2.7 Extreme Temperatures
WARNINGS
1. Systems fitted with the low temperature option use liquid nitrogen
and/or liquid helium as a coolant. Liquid nitrogen and liquid
helium are cryogenic liquids and can cause cold burns. Wear
gloves when handling cryogenic liquids and use eye protection.
Refer to the information supplied with the equipment for more
information.
2. During operation both the X-ray tube and the heat sink of the CCD
power supply become hot. In normal use they are located inside a
cabinet and hot parts are not accessible. During maintenance
periods, however, it may be necessary to override the interlock so
that adjustments can be made. Therefore great care must be taken
to avoid touching either the X-ray tube or the heat sink of the CCD
power supply when they are operating and for a period of 20
minutes after operation.
2.8 Vacuum
WARNING
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.
2.9 High Pressures
WARNING
Know the law about high pressure gas cylinders and follow it. Highpressure cylinders are often used to store gases (typically at
pressures up to 200 bar). Most countries have laws about using them.
•
Chain cylinders to a fixed object or keep them in specially
designed trolleys
•
Only use approved and tested high pressure fittings
Gas cylinders become dangerous projectiles if they are ruptured or the valve is knocked off. They
can break through thick walls or travel hundreds of metres (by rocket propulsion).
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HEALTH AND SAFETY INFORMATION
2.10 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. http://www.brushwellman.com/EHS/MSDS/M10.pdf
WARNING
If Beryllium is exposed to fire, it may oxidise to highly toxic beryllium
oxide powder. Do not attempt to clear up the remains of any fire, but
contact the relevant local agency stating that there is an incident
involving possible beryllium or beryllium oxide contamination.
2.11 Modifications and Service
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. It should be stressed that those parts of
the equipment which are interchangeable, and which are subject to deterioration during operation,
may significantly affect the safety of the equipment.
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Pre-installation Guide
Version 1.6
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INTRODUCTION
3. Introduction
3.1 Scope
This manual applies to the Xcalibur and Gemini systems designed and manufactured by Oxford
Diffraction.
3.2 How to Use This Guide
This manual describes the pre-installation requirements to enable the Xcalibur or Gemini system to
be installed efficiently and in the minimum time. Account is taken of the environmental
specifications, power and water requirements, system configuration, handling of the components,
health and safety issues regarding unpacking, installation and operation of the system.
All personnel who are likely to operate the system or who are likely to come into contact with any of
the system components should read the HEALTH AND SAFETY INFORMATION section of the
manual. This provides basic information aimed at highlighting the safety hazards associated with
the equipment.
More detailed information and instructions for Xcalibur or Gemini diffractometers and the
component parts of the system are given in the third party manuals supplied with the system. These
manuals should be read and understood before operating the system.
3.3 System Overview
Xcalibur and Gemini 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. Xcalibur and Gemini systems may also be used in the analysis of powder samples.
Intended samples should have a maximum unit cell dimension of 100 Angstrom in any direction for
small molecule Xcalibur or Gemini diffractometers and 500 Angstrom for macromolecular Xcalibur
or Gemini PX systems.
Xcalibur or Gemini 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 Oxford Diffraction to enable use of these devices.
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SPECIFICATIONS
4. Specifications
4.1 Environmental Requirements
It is essential that the climate of the laboratory is controlled to ensure that the Sapphire CCD
detector is not damaged. Typically air-conditioning would 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 ~12°C, condensation should not be allowed to collect on the
CCD at any time.
Ambient temperature during operation
18 – 28 °C
Stability of ambient temperature during operation
± 1 °C
Storage temperature
>10°C
<40°C
Relative humidity
<80 % non – condensing
Location
Clean, dust free environment
>2m from air conditioning or heating units
Floor covering
Conductive or, if carpeted, covered with
electrostatic mats
Floor strength
Able to bear the system weight of about 500kg
over an area of 0.64m2.
4.2 Services
4.2.1 Electrical Supply
Number of outlets required.
1 x single-phase outlet (16A) for Xcalibur system (computer,
goniometer, interface, water chillers etc.)
1 x single-phase outlet (32A) per X-ray generator (i.e 2 for
Gemini).
4 x single-phase outlets (for temperature attachments, and
computer monitor) these can be supplied from a second 16A
outlet.
Voltage fluctuation
< ± 10 % ( with line voltage regulator fitted if necessary)
Location of outlets
On wall behind system, (except Computer Monitor supply which
should be near intended computer location).
Protection
Circuit breaker to be fitted to all outlets
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Version 1.6
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SPECIFICATIONS
4.2.2 Mains Supply Water Cooling
Min flow rate
1.8 l/min
Pressure
0.5 - 5 bar gauge
Temperature stability
± 5 °C
Temperature range
10 – 20 °C
Composition
Filtered, without deposits, chemically neutral and
optically clear
4.2.3 X-ray Tube Cooling Water
In addition to the mains supply water outlined above, the Customer will also need to supply suitable
water for the closed circuit water cooling of the X-Ray tube(s). This water should meet the following
criteria:60L filtered (<10µm)
10 µS/cm < specific conductivity < 250 µS/cm
1 D < hardness in German Degrees < 4 D
7.5 <acidity (pH) < 9.5
In practise this can usually be achieved by using a mixture of demineralised water and tap water.
The pH can be modified by adding NaOH to the water whenever required. Whenever possible use
old or boiled water rather than fresh tap water. This volume of water is enough to fill the CCD
cooling circuit as well.
This water will need to be replaced periodically throughout the life of the Diffractometer as part of
the normal maintenance schedule.
4.2.4 Helium Gas Supply (where applicable)
Purity
99.99%
Regulator
low pressure regulator
Minimum pressure
0.5 bar gauge
Flow rate
30 - 40 cm3/min @ ATP
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Pre-installation Guide
Version 1.6
Page 9
SPECIFICATIONS
4.3 Performance Data
4.3.1 X-ray Tube (Typical Operating Conditions)
Tube
Voltage (kV) setting
Current (mA) setting
Resulting power (kW)
Cu 2kW tube
40
35
1.4
Mo 2kW tube
50
30
1.5
Mo 3kW tube
55
40
2.2
Maximum radiation dose due to scattering
radiation at outside surface of the
enclosure (door closed)
0.6 µSv/h (with Mo 3 kW tube operating at 2.2 kW)
Maximum radiation dose due to scattering
(door open, with shutter closed)
0.18 µSv/h (with Mo 3 kW tube operating at 2.2 kW)
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Version 1.6
Pre-installation Guide
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
5. Handling, Installation, Storage and
Transit Information
5.1 Reception and Handling
5.1.1 Delivery
Carry out the following steps on delivery of the system and before unpacking Xcalibur or Gemini:
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 Oxford Diffraction immediately.
2. Check that shock-watch and tilt indicators fitted to the outside of the packing cases have not
been activated. If the indicators have been activated notify Oxford Diffraction immediately.
3. Check the number of delivered items against the packing list. If any items are missing contact
Oxford Diffraction within 3 days.
WARNING
The packing crates are heavy and could cause serious injury and
damage to the equipment if not handled correctly. Use suitable lifting
equipment and procedures. Only lift the packing cases from the
bottom.
CAUTION
Do not remove the equipment from the packing crates until they have been moved
to their designated installation site. The equipment has been carefully packed to
protect the equipment from damage in transit. Removal of the packing equipment
could make the equipment vulnerable to damage during transit.
4. Always lift packing cases from the bottom using suitable lifting equipment (refer to list of
component weights in the following section).
5. Move packing cases into the designated installation site.
6. Contact Oxford Diffraction to notify them that the equipment is awaiting installation by a factory
trained service representative.
5.1.2 Unpacking
Unpacking of the system should only be carried out under Oxford Diffraction supervision. If
unpacking is unavoidable, all packing materials should be kept until the end of the installation, and
contents stored in a secure location. Once installation is complete, the Installation Engineer will
advise you on which boxes/ packing materials should be kept and which may be disposed of.
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Version 1.6
Pre-installation Guide
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
5.1.3 Mechanical Handling
5.1.3.1 Weights, Dimensions and Lifting Points
Description
NET
Weight
kg
Dimensions
(width x height x depth)
cm
Centre of gravity
Lifting points
Kappa
goniometer
106
43 x 64 x 47
Offset from centre of
unit towards side of
X-ray tube mount
At four corners
(DO NOT lift from
below)
X-ray
generator
40
48 x 22 x 69
Centre of unit
From the sides and
below
Enclosure
50
115 x 100 x 100
N/A
N/A
Electronics
rack
80
80 x 85 x 80
Centre of unit
By hand from top
four corners,
otherwise from
below
KMW200CCD
55
38 x 54 x 75
Centre of unit
At the four corners
and from below
KMW3000C
56
38 x 54 x 96
Centre of unit
At the four corners
and from below
Helijet
10
30 x 25 x 10 (head only)
Centre of component
parts
From below with
transfer tube
removed
Cryojet
15
15 x 35 x 15 (head only)
Centre of component
parts
From below or
using handles
whilst supporting
transfer tube.
ILM210
5
44 x 10 x 30
Centre of unit
By hand from below
ITC502
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
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Version 1.6
Pre-installation Guide
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
5.1.3.2 Approximate Boxed Weights, Dimensions and Lifting Points on Delivery
Box
Item
Length
(cm)
Width
(cm)
Height
(cm)
Weight
(kgs)
1
Goniometer
102
67
80
148
2
Protection cabinet
140
120
60
200
3
Electronics rack
98
96
106
170
4
PC, Optics, Accessories
102
67
80
118
5
CCD camera
1121
99
113
140
6
KMW200CCD
112
54
80
96
7
KMW3000C Chiller
112
54
80
98
8
Generator, Monitor, X-ray tube
83
67
80
70
9
Cryojet
70
79
189
143
10
160L LN2 dewar
73
73
176
119
11
Helijet
92
60
96
55
(No.)
The weights and dimension above are an estimate and should only act as an indication of the lifting
requirements when the system is delivered. All boxes are fitted with the facility to use forks to
unload. There is 15cm 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.
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Pre-installation Guide
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
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 drawing number OD-01-00-15.
When the low temperature option is fitted an extra 100 cm space on the left-hand side of the system
is required.
Unpacked, the largest subassembly will fit through a door aperture of 85 cm. Check the door
aperture to ensure the system can be assembled in its designated area.
5.2.1.3 Electrical Services
A 3-phase 63 A supply with one 32A and two 16A single-phase outlets. One of the 16A outlets can
be used to supply the additional four single-phase outlets that are required as described in drawing
OD-01-00-015-C. For Gemini systems which have 2 High Voltage Generators, two 32A single
phase outlets will be required.
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 with a
resistance of less than 0.5 ohms.
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 10 kVA with 3-phase input and single phase
output.
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Version 1.6
Pre-installation Guide
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
Description
Voltage
V
Frequency
Hz
Maximum
mains
current
A
Main
fuse
A
Maximum
power
W
X-ray generator
1/N AC 230 ±10%
50/60
19
32
4300
CCD detector &
KMW200CCD cooler
1/N AC 230 ±10%
50/60
2
2.5
700
Kappa geometry, X-ray
goniometer, video
monitor, halogen lamp,
fibre optics
1/N AC 230 ±10%
50/60
3.6
6.3
400
KMW30000C Cooler
1/N AC 230 ±10%
50/60
1.2
6.3
300
Computer and
peripherals
1/N AC 230 ±10%
50/60
10
10
Cryojet controller
100 - 240
50/60
2
2.5 – 5
ILM201 – Liquid
Nitrogen Level meter
100 - 230
50/60
0.6
0.8 –
1.6
Merlin 100/150
(Optional) Auxilliary
water chiller for
KMW3000
220-240
50/60
15.4
24-32
?
5.2.1.4 Water Supply
CCD detector cooling
The CCD detector is water cooled by the KMW200CCD Chiller. Ten metre long water pipes are
supplied with the system.
The minimum required distance between the KMW200CCD and the KMW3000 or the electronics
rack is 30 cm.
X-ray Tube and Generator Cooling
A cooling system is required to dissipate the heat produced by the X-ray tube. A closed circuit
cooling system should be installed to minimise the effects of particles, low pressure and water
temperature fluctuation on the performance of the system from local tap water supply.
The KMW3000C is a closed circuit cooling system suitable for this purpose. It is supplied with two
10 metre long hoses and 8mm inside diameter. The maximum distance between the KMW3000C
chiller and the system is 10 metres. The distance between the water supply and the chiller is not
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limited but the supply must deliver 0.5 – 5 bar gauge pressure with a minimum 1.8 litres/min flow
and a gravity drain with an elevation that does not exceed 1metre.
The water supply should have a wall mounted shut off valve.
If the X-ray tube and generator are not to be cooled by the KMW3000C Chiller, the cooling system
selected must have a flow sensor and thermal switch to monitor the cooling and act as safety
devices for the X-ray tube and generator. It must also meet the following requirements.
Min flow rate
Pressure
Temperature stability
Temperature range
1.8 Litres/min
0.5 - 5 bar gauge
+/- 5ºC
10-20 ºC
CAUTION
There is no flow sensor or thermal switch inside the system to protect internal
components against improper cooling. These are provided inside the KMW3000C.
The X-ray tube warranty does not cover damage due to improper cooling water.
5.2.1.5 Low Temperature Option
Occasional access to a suitable high vacuum pump, ideally 70 Litres/sec turbo molecular pump is
required to periodically evacuate the Cryojet head and the heater leg.
To demonstrate the operation of the Cryojet, a minimum 100 litres of liquid nitrogen are
required during the installation. This should be delivered no later than the morning after
installation commences. If the autofill option has been purchased this will need to be a
minimum of 120 litres.
The customer should supply a suitable rack/ table for both the ILM and the Cryojet controller.
5.2.1.6 CCD Camera Pumping
Occasional access to a suitable high vacuum pump, ideally 70 Litres/sec turbo molecular pump, is
required to periodically evacuate the CCD camera. (Only one pump is required between the Cryojet
and CCD)
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.
A turbo molecular pump, capacity 70 litres/sec is REQUIRED before each use of the Helijet, and
must be supplied if not purchased as part of the system.
5.2.1.8 PX Ultra systems
The customer should provide 1 full helium gas cylinder of at least 99.95% grade helium gas in order
that the Ultra Optics can be demonstrated. The cylinder should be supplied with a suitable
Regulator capable of supplying gas at pressures <0.5bar.
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
5.2.2 Setting to Work
5.2.2.1 Equipment to be supplied by customer;In addition to equipment mentioned elsewhere, the following equipment is needed permanently;
1. Table (and Chairs) for computer that controls the system.
2. Table/ shelving for Cryojet controller.
Equipment needed during Installation only.
3. Engine hoist/portable lifting device with soft slings capable of lifting 100 kg, (or several people,
see below).
4. Electric screwdriver / Drill with screwdriver attachments (Pozidrive)
5. Flat headed screwdrivers (assorted sizes).
6. Ethanol.
7. Paper Towels.
5.2.2.2 Personnel Required for Installation
5 people for lifting of heavy components.
The main user of the equipment should make themselves available throughout the installation for
training in the use and maintenance of the equipment. Any other users should be available for
training in the final two to three days of the installation. If the user group is very large it may be
useful to supply a seminar room with network access.
If there is a Technician that will be responsible for routine maintenance, they should be available for
at least the first 3 days of the installation.
5.2.2.3 Setting up Procedures
Oxford Diffraction personnel normally perform the installation. The duration of the installation is
typically 2-3 working days, with an additional day for the low temperature option. This is followed by
2-3 days training from an Oxford Diffraction crystallographer.
The numbers on Figure 5.2.1 refer to the step numbers in this section. These notes provide
installation guidance only.
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
6
15
4
14
5
11
12
9
8
10
13
3
2
7
1
Figure 5.2.1 Xcalibur or Gemini installation procedure
1. Install electronics rack.
Use 2 persons to lift electronics rack into position on a level floor (see environmental
requirements).
2. Mount table top.
Remove vented front, back and side panels at the top of the electronics rack.
Screw table top into position (from below and at the four corners).
Check that the table top is level.
3. Mount goniometer.
Use 5 persons to lift the goniometer to the centre of the table top.
Position goniometer on feet provided.
4. Mount protective cabinet frame and top.
Use 4 persons. Each person supports one of the four side struts of the cabinet frame.
Attach and secure the frame uprights (Remember to secure corner screws).
Once base is securely positioned around the tabletop, attach cabinet top (Remember to secure
corner screws).
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5. Connect halogen cabinet lights. Attach fibre-optic lights, cabinet vents and System remote
control.
6. Mount support arm.
Mount in position shown and secure fixing screws.
7. Attach cable guide and video camera arm.
Use appropriate screws to attach in positions shown.
8. Insert X-ray generator.
Use 3 persons to insert the X-ray generator. Insert from front of electronics rack. 2 persons
lifting, third person guiding cables through to back of rack. (This requires removal of back and
side panels of electronics rack).
9. Mount Enhance or Enhance ULTRA X-ray source assembly(s), X-ray tube and temperature
sensor.
Mount Enhance or Enhance ULTRA and secure with fixing screws.
From back of system, insert the power cable from the X-ray generator into X-ray tube shield and
secure.
WARNING
Ensure tube shield is properly aligned with the fast shutter. Incorrect
mounting may result in exposure of personnel to X-ray radiation.
Holding by its metal base, remove the X-ray tube from its protective box.
WARNING
Do not touch the Beryllium windows in the X-ray tube. Beryllium is a
potentially toxic material.
From the front (Top) of the housing(s) insert the X-ray tube(s) into the tube shield and secure.
WARNING
Ensure a perfect fit of the X-ray tube. Remove red plastic spacers if
necessary. Incorrect mounting may result in exposure of personnel to
X-ray radiation.
Secure temperature sensor(s) to cover plate of X-ray tube.
Mount cover plate(s) to X-ray source and secure in position using fixing screws.
10. Mount CCD detector
Slide detector onto graduated mount from right hand side of Xcalibur or Gemini (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.
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
11. 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 Optics such that it is flush to
the housing surface.
12. Mount video tower.
Screw into position.
13. Mount DC power supply.
Attach to support arm on back or side of goniometer table.
14. Mount fibre-optic power supply.
Attach to support arm.
15. Mount video monitor.
Lift monitor into position and secure from below.
16. Mount video telescope camera.
Slide video camera into video camera support arm.
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).
5.3 Storage
Before installation commences, or when the system is not being used for extended periods, store
Xcalibur or Gemini in accordance with the environmental conditions for temperature and humidity
stated in the SPECIFICATIONS section of this manual.
Always store Xcalibur or Gemini in a secure room.
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HANDLING, INSTALLATION, STORAGE AND TRANSIT INFORMATION
6. Drawings
6.1.1 Mechanical Drawings
Drawing no
Title
Number
of pages
OD-01-00-15-C
Xcalibur or Gemini Suggested Layout
1
OD-01-00-15-C Xcalibur and Gemini Suggested Layout
Xcalibur and Gemini
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DRAWINGS
6.1.2 Electrical Drawings
Drawing no
Title
Number
of pages
OD-01-00-01
System and Component Dimensions
1
OD-1-00-14
Mains Distribution Diagram
1
(Circuit Breaker 3-Phase 63A 4Outlets)
OD-01-00-01
System and Component Dimensions
Xcalibur and Gemini Dimensions
116
100
80
80
115
200
KMW3000C Dimensions
96
37
75
54
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DRAWINGS
KMW200CCD Dimensions
78
75
37
54
OD-1-00-14-C Mains Distribution Diagram (Circuit Breaker 3-Phase 63A 3 Outlets)
L1
Mains distribution box
(3-phase 63A circuit breaker
with 3 single phase outlets)
L2
L3
N
X-RAY
GENERATOR
16A
16A
32A
32A
PE
Xcalibur
system
Other devices
Single phase sockets
OXFORD DIFFRACTION
XCALIBUR SYSTEM
TITLE
MAINS DISTRIBUTION DIAGRAM
A. No.
Appr
C
Date
01.2003
DRG. NO.
OD-01-00-014-C
DRAWN BY:
APPROWED BY:
FILE
DATE
Radoslaw Smaga
SIZE
SCALE
Jan 2003
REV.
C
SHEET 1 OF 1
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DRAWINGS
Appendix Example of Local Rules for the
Xcalibur or Gemini System Set-up at Oxford
Diffraction
An example of the Local Rules for the Xcalibur and Gemini system set up at Oxford Diffraction is
provided for information. As part of our Installation procedure a ‘Critical Examination’ of the
equipment should be carried out during the Installation. For this purpose please arrange for a
Radiation Monitor to be available so that this work can be carried out. Ideally the monitor should be
an Uncompensated Geiger Muller Tube. Local rules may require you to arrange for an independent
examination of the equipment, if this is the case please make suitable arrangements for the
inspection to be done towards the end of the Installation or in the following week.
Xcalibur and Gemini
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Local Rules
For the operation of X-ray Crystallography Equipment
Issue 1.4
July 2005
File reference: Xcalibur and Gemini Local Rules.doc
Oxford Diffraction Ltd
68 Milton Park, Abingdon
Oxfordshire OX14 4RX U.K.
Tel: +44 (0)1235 443630
Fax: +44 (0)1235 443631
E-mail:[email protected]
www.oxford-diffraction.com
LOCAL RADIATION RULES – EXAMPLE COPY
Contents
1. Introduction ....................................................................................................................................................3
1.1 Description ........................................................................................................................................................3
1.2 Risk Assessment ...............................................................................................................................................3
2. Contingency Plans .........................................................................................................................................4
2.1 Exposure ...........................................................................................................................................................4
2.2 Fire ....................................................................................................................................................................4
3. Names and Duties of Persons.......................................................................................................................5
3.1 Radiation Protection Supervisor (RPS) .............................................................................................................5
3.1.1
Duties of the Radiation Protection Supervisor ...................................................................................5
3.2 Radiation Protection Adviser (RPA)...................................................................................................................6
3.3 Authorised Operators ........................................................................................................................................6
3.3.1
Duties of an Authorised Operator ......................................................................................................7
4. Designated Areas ...........................................................................................................................................8
5. Monitoring Routines ......................................................................................................................................9
5.1 New or replacement equipment.........................................................................................................................9
5.2 Normal conditions..............................................................................................................................................9
5.3 Interlock over ridden ..........................................................................................................................................9
6. Maintenance .................................................................................................................................................10
6.1 Alignment of source...................................................................................................................................10
6.2 Exchange of X-ray source ...............................................................................................................................10
Appendix 1. Systems of Work.........................................................................................................................11
a) System commissioning (Critical Examination) ............................................................................................11
b) Start-up procedure......................................................................................................................................11
c) Sample change and alignment ...................................................................................................................12
d) Normal running conditions ..........................................................................................................................12
e) Unattended operation of system.................................................................................................................12
f) Alignment of X-ray tube without collimator ..................................................................................................12
g) Shutdown ...................................................................................................................................................12
Appendix 2 Critical Examination test sheets.................................................................................................13
Appendix 3 Example of Operator Log Book ..................................................................................................15
Appendix 4 Acknowledgement of Local Rules..............................................................................................17
Warnings
Before you attempt to install or operate this equipment for the first time, you must have read and understood these rules
and confirm this to the RPS by using the form attached in Appendix.
 Oxford Diffraction Limited, July 2005. All rights strictly reserved.
S. Clarke
Page 2
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
1. Introduction
These rules are the general principles and description of the means of complying with The Ionising Radiations
Regulations 1999 (IRR99) based on the recommendations on risk published by the International Commission on
Radiological Protection (ICRP) and endorsed by the National Radiological Protection Board (NRPB). All employees and
visitors have a legal obligation to comply with these rules, to co-operate in their implementation and not to intentionally or
recklessly interfere with or misuse the equipment.
1.1 Description
These local rules apply to the operation of the ‘Xcalibur’ X-ray diffractometer installed in the Applications
Laboratory of Oxford Diffraction Ltd., 68 Milton Park, Abingdon Oxfordshire
1.2 Risk Assessment
The radiological hazard results from the use of an X-ray source while its generator is switched on. The maximum
operating parameters of the generator are 60kV and 50mA (3KW) although normally the tube is run at no more than 70%
of its maximum power. The target material is Molybdenum. In normal operation the X-rays are generated and projected
in a totally enclosed cabinet constructed of suitable shielding material. The resulting maximum dose rate due to
scattering radiation is calculated to be no more than 0.4 µSv/h from a count rate of 5 c.p.s. at the outside surface of the
enclosure, which is well within acceptable levels. A background of 1c.p.s. at other points on the surface of the enclosure
would be acceptable. Access to the interior of the cabinet via the front doors is required in order to change the sample
and an interlock is present to close the shutter should the doors be open inadvertently. When the doors are opened
during sample change and alignment, the x ray generator remains on for optimum performance and thus radiation
leakage might occur between the source and the shutter. This can be expected to be no more than 0.12 µSv/h from a
count rate of 2c.p.s. It is possible for the shutter to be opened when the collimator is not in place but the shielding of the
enclosure is adequate.
It is necessary however, to override the interlock system in order to make initial coarse alignment adjustments of the x
ray tube but this is done at low operating generator powers. There is, therefore, the possibility of exposure to the
collimated primary beam particularly of the operator’s fingers. If the generator is inadvertently run at higher powers, as
well as the increased dose of the primary beam, there is also a risk of the backwards scattered (back towards the x ray
tube) fluorescence radiation. If a shorter collimator is used unnecessarily then there is a greater amount of exposed
beam in which to put body parts into.
Special arrangements therefore operate during any alignment procedure (Appendix 1. Systems of Work).
Note: Currently, the annual equivalent dose limit of X-rays to the skin (averaged over 1cm2) for workers aged 18 or
over is 500 mSv or 260 µSv/h averaged over a working year.
S. Clarke
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LOCAL RADIATION RULES – EXAMPLE COPY
2. Contingency Plans
2.1 Exposure
Direct access to the primary beam could deliver an overdose of radiation, perhaps leading to a burn, in only a few
minutes. (For a copper target this would be a few seconds).
Should any monitor reading be in excess of indicated levels steps should be taken to stop the radiation, taking extreme
care to protect yourself and the people in the room. If it is the result of the failure of any components of the system then
the equipment should be made safe by isolating it from the electrical mains supply and the RPS notified immediately. DO
NOT CONTINUE TO USE THE EQUIPMENT UNTIL THE FAULT HAS BEEN REPAIRED.
In the event of any defect to or failure of a safety feature or warning device, the equipment should be made safe by
isolating it from the electrical mains supply and the RPS notified immediately. DO NOT CONTINUE TO USE THE
EQUIPMENT UNTIL THE FAULT HAS BEEN REPAIRED.
If any person suspects that they or other persons have been exposed to a primary X-ray beam they must notify the RPS
and Company Safety Officer immediately. Record the X-ray parameters (kV, mA, and wavelength), position of exposure
and time of exposure. Unless it can be shown beyond any reasonable doubt that an overexposure did not occur, the
Health and Safety Executive must be notified forthwith.
If a customer who is a Classified Radiation worker wishes to enter the Controlled Area for the purposes of sample
alignment, the RPS must be informed prior to doing so in order for the estimation of dose rate to be made and entered in
to that worker’s passbook.
2.2 Fire
In the event of a fire or emergency requiring evacuation from the area and without endangering any persons’ safety, the
generator should be switched off before evacuation. If this is not possible then the Senior Fire Brigade Officer or
equivalent emergency service personnel must be informed that an X-ray generator is working and that a radiation hazard
exists. This should be done by:
Informing the Fire Marshall for that area at the fire assembly point
Or
Informing the presiding senior manager (outside normal working hours).
Or
Informing the security guard (outside normal working hours).
Note:
Remember that if you have visitors they need to be escorted to the Reception fire assembly point and for you
all to attend.
S. Clarke
Page 4
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
3. Names and Duties of Persons
3.1 Radiation Protection Supervisor (RPS)
The following person has been appointed by Oxford Diffraction, as RPS for this equipment:
David Warner
Telephone 01235 443630
The RPS should be consulted on all matters affecting radiation safety with this equipment.
3.1.1 Duties of the Radiation Protection Supervisor
To ensure that all staff (or outside contractors working on the X-ray crystallography equipment) are provided with copies
of these local rules, that they have read and understood them and that they are complying with the requirements of these
rules.
To arrange for the immediate repair of any defective interlock, warning light or other safety system.
In the event of a suspected accidental exposure of any person to supervise the implementation of the contingency plans,
(see section 0 ).
To consult the Radiation Protection Adviser on any other matter of radiation safety about which the RPS is uncertain of
the correct action to take.
To ensure that measurements to determine dose rates around the X-ray crystallography equipment and checks of safety
interlock systems, warning lights and emergency stops are carried out monthly or when used, which ever is the longer
time period, and that the results are recorded.
To arrange the regular calibration checks of any monitoring equipment.
S. Clarke
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July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
3.2 Radiation Protection Adviser (RPA)
The RPA is:
National Radiological Protection Board (NRPB)
Southern Centre
Chilton
Didcot
Oxon, OX11 0RQ
Tel: 01235 831600
Fax: 01235 822650
Primary contact:
Dr John O'Hagan
Tel: 01235 822673
Out of hours telephone number: 01235 834590 (Emergency use only)
The out-of-hours emergency telephone connects with the AEA Harwell Laboratory security control. The caller should
state that they require the emergency assistance of NRPB (Southern Centre) as RPA and give the name of the usual
contact.
The NRPB representative returning the call will not necessarily be the person named above.
3.3 Authorised Operators
The X-ray generator is to be used only by operators authorised by the RPS. To be authorised, the operators will be only
OXFORD DIFFRACTION personnel and Oxford Diffraction personnel trained by OXFORD DIFFRACTION and who have
completed the attached form in Appendix 4 Acknowledgement of Local Rules, confirming that they have read and
understood these Local Rules. As such, only an Authorised Operator may override the interlocks in order to perform the
maintenance alignment procedures.
S. Clarke
Page 6
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
3.3.1 Duties of an Authorised Operator
During any period of operation of the generator, the operator is responsible for measuring and recording the X-ray dose
rates, ensuring the cabinet doors are locked while the system is unattended and for the safety of themselves and other
occupants of the Supervised & Controlled Areas.
Also, during any demonstration of the equipment, non Authorised Operators such as customers may wish to enter the
Controlled Area either to observe or practise any alignment procedure. Before allowing this, the Operator must enquire if
the customer is a Classified Radiation Worker and if so, inform the RPS. Any such person then should make their
radiation passbook available to the RPS for entering into it the estimate of the dose received by that worker.
The authorised users are:
Mathias Meyer
OXFORD DIFFRACTION Poland Sp. z o.o.
Robert Pol
OXFORD DIFFRACTION Poland Sp. z o.o.
Andrzej Kowalski
OXFORD DIFFRACTION Poland Sp. z o.o.
Damian Kucharczyk
OXFORD DIFFRACTION Poland Sp. z o.o.
David Warner
OXFORD DIFFRACTION
Leigh Rees
OXFORD DIFFRACTION
Simon Clarke
OXFORD DIFFRACTION
Adam Limb
OXFORD DIFFRACTION
Neil Brooks
OXFORD DIFFRACTION
S. Clarke
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July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
4. Designated Areas
During normal operation the whole room containing the system is designated as a Supervised Area and access to it is
not restricted.
When the cabinet interlock is overridden, the entire room is designated a Controlled Area when the X-ray generator is
switched on. Only Authorised Operators who operate in accordance with the written system of work (Appendix 1.
Systems of Work) included in these local rules and visitors (generally customers) who are individually supervised by the
Authorised Operator are permitted access to the Controlled Area. All other people should leave the room.
S. Clarke
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July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
5. Monitoring Routines
This is to be done with the hand held Mini Instruments MM900X , serial number E0001495 scintillation counter with the
cap removed. Details of the X-ray generator voltage and current for the appropriate counter positions are to be recorded
in the Operations log book, an example page is given in Appendix 3. As no accessible dose rates are in access of 2.5
µSv/h, personal monitoring, including extremity monitoring, is not required.
The radiation monitor calibration will be annually checked by the NRPB.
5.1 New or replacement equipment
Any additional or replacement systems should undergo a Critical Examination to establish safe radiation leakage before
using it for sample measurements. Use the table and the associated monitoring point diagram of Appendix 2 Critical
Examination test sheets to record the results.
5.2 Normal conditions
Prior to changing a sample the X-ray leakage must be monitored at the front of the cabinet to see if there is a change as
the doors are opened. Upon opening the doors the leakage must be checked between the source and shutter. With a
sample in place and at the start of each measurement the integrity of the shielding cabinet must be carried out at the
optimal generator power, paying particular attention to the cabinet beam stop and surrounding area at the surface of the
cabinet with the camera in and out of the primary beam. Thereafter, during the period of operation, occasional random
monitoring from where any people are located in the room is recommended. If the period of operation is greater than
one month then this must be done regularly once a month.
5.3 Interlock over ridden
Authorised persons must exercise extreme care during open beam work and should never allow any part of the body to
intersect the X-ray beam. For the purposes of entry to the Controlled Area, Classified Radiation Workers will have their
dose rate checked and the result entered into their passbook.
S. Clarke
Page 9
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
6. Maintenance
6.1 Alignment of source
This should only be performed by an Authorised Operator in accordance with the written system of work (Appendix 1.
Systems of Work).
6.2 Exchange of X-ray source
This is a non-adjustable item and should be performed by OXFORD DIFFRACTION personnel only.
S. Clarke
Page 10
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LOCAL RADIATION RULES – EXAMPLE COPY
Appendix 1. Systems of Work
The use of the system is summarised below with its specific conditions of use in the sub-sections of this
appendix.
No person shall intentionally or recklessly interfere with or misuse the X-ray generator or its safety devices or shall
tamper with or override safety interlocks attached to the shielding cabinet in any way other than in accordance with the
written system of work detailed below.
No modification should be made to the X-ray generator, ancillary equipment, safety feature or warning device without first
notify the RPS. A record must be made of all modifications. Where such modification requires the disabling of an
interlock in any way, the written system of work below must be adhered to.
A record should be made of the interlock checks and dose rate checks by the person performing them in the Operation
Log Book. Each system will have its own log book.
Appropriate measurements of dose rates should be made to the tube shield (with the generator on and shutters closed)
and around the outside of the cabinet (cabinet closed, generator on and shutter open) or, for close coupled equipment,
around the tube shield and ancillary equipment while the generator is on and beam shutter open.
Proposals for new methods of work or projects should be placed before the RPS at least two weeks prior to the work
commencing and should not commence without prior authorisation from the RPS.
The interlock override and panel lock keys and shorting cables are kept by the RPS - they are only available to
Authorised Operators. Never leave the equipment unattended while any interlock is overridden.
a) System commissioning (Critical Examination)
Any additional or replacement systems should undergo a Critical Examination to establish the radiation leakage rate
before using it for sample measurements. Use the table and the associated monitoring point diagram of Appendix 2 to
record the results. First sweep all the cabinet faces as indicated by the green dotted line with a sensitive search monitor
such as a MM900-44B. Any above background readings should be investigated, their locations indicated on the result
sheets and the drawing and then the actual count or dose rate measured with a radiation measurement monitor such as
the MM900X. The reasons for all above background leakage levels should be ascertained and any solutions to reducing
them should be taken. If any leaks are above 2.5µSv/hr, the system should be made safe until the reason is found and
solved. Once it has been established that there are no excessive leaks the radiation levels at the numbered points
should be recorded.
b) Start-up procedure
Prior to a new period of use, check the interlocks on the doors and the indicator lamps for the shutter and X-ray warning
correctly function and record the results on a new page of the Operations Log. Ensure the rear and side panels are
locked. The X-ray generator needs to be progressively powered up as according to the system’s Start-up Guide.
S. Clarke
Page 11
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
c) Sample change and alignment
Ensure the interlock over ride key is removed from the system. Check the leakage of the shutter if the generator is on
when the doors are first opened. If it is necessary to look along the axis of the collimator, turn down the X-ray generator
to 30kV, 1mA . If the sample is held in a pressure cell then it is necessary to change to a different length of collimator.
d) Normal running conditions
Ensure the interlock over ride key is removed from the system. If the period of operation is greater than one month then
the interlock and warning lights check must be done regularly once a month.
e) Unattended operation of system
Ensure all cabinet doors and panels and the access panel door for the X-ray generator are locked and the keys placed in
the combination locked safe box. Upon vacating the room, the door is to be locked and a sign placed to prohibit
unauthorised entry to the room.
f) Alignment of X-ray tube without collimator
Ensure the interlock over ride key is removed from the system.
g) Shutdown
Lock all cabinet door and panels and the access panel for the X-ray generator. Switch off all equipment and disconnect
all electricity plugs. Turn off water supply to the chillers.
S. Clarke
Page 12
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
Appendix 2 Critical Examination test sheets
The critical examination has been carried out in accordance with the ionising radiation regulations
1999, Part VI, section 31. (2) for the x-ray diffraction equipment specified below.
Model:-
Xcalibur S
Location:Persons present during examination:Examination conducted by:Date of examination:Instrument used:Radiation:-
Oxford Diffraction Ltd, Demo Lab
Mini Instruments 900, S/N E0001495
Mo kα
Equipment tested
Equipment
Model
Serial Number
X-ray generator
X-ray tube
Optics
Spellman
MO CX-12 x 0.4-s
Enhance
Table of results
Generator power
settings
Shutter
Distance from source
Radiation
reading
Effective
Dose (CPS/.68)
µSv h-1
Counts s-1
0kV
0mA
50kV 40mA
50kV 40mA
50kV 40mA
50kV 40mA
50kV 40mA
50kV 40mA
*
Equivalent Dose
0kW
2.0kW
2.0kW
2.0kW
2.0kW
2.0kW
2.0kW
Closed
Closed
Open
Closed
Open
Open
Open
Background
Outside enclosure
Outside enclosure
Inside enclosure
At body position
20cm radius from sample
2cm radius from sample
System Safety Features
Passed
The shutter closes when the enclosure door is opened.
The shutter closes when each individual enclosure panel is removed.
The shutter remains closed when any indication lamp fails.
David Warner
Oxford Diffraction Ltd
Radiation Protection Supervisor
S. Clarke
Page 13
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
Figure 1 Critical Examination
monitoring point diagram
REAR SIDE
RIGHT SIDE
cent re line
Sample
Sample
cent re line
LEFT SIDE
Primary beam
Sample
cent re line
THETA
axis
CCD
Sample
cent re line
Primary beam
axis
FRONT SIDE
S. Clarke
Page 14
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
Appendix 3 Example of Operator Log Book
Note:
Start a new page for each new period of operation.
Use the following diagram to indicate the positions of the monitor in the log book entries.
ce
San t
m re
p l lin
10
9
8
11
7
12
6
Pr i m a r y
axis
14
15
1
D i m s:
13
5
2
Heig h t o f
m o n it o r
t o co i n ci d e
sa m p l e
S. Clarke
3
4
16
Page 15
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
Checked by (Sign)
and current)
generator voltage
button (low
Emergency Stop
mA
Shutter light
kV
X Ray on light
Operator
Front door check
Date
Generator on
Interlock checks:
(tick for pass)
X –ray dose rates:
Start
Date
Operator
S. Clarke
Time
X-ray
Exposure
Duration
kV
mA
Configuration
Monitor
leakage
Checked
change?
location
rate
by (Sign)
Page 16
July 2005
LOCAL RADIATION RULES – EXAMPLE COPY
Appendix 4 Acknowledgement of Local Rules
I have read and understood these Local Rules and I have received personal instruction in the use of the X-ray
generator.
Name:
Signed: -----------------------------------------------------------------------------------
Date: -------------------------------------------------------------------------------------Warning:
You must not use the X-ray generator and its associated equipment until you have signed
and returned this form to DW who is the Radiation Protection Supervisor in the Applications
Laboratory.
S. Clarke
Page 17
July 2005