Bruker RS User manual

NMR Spectroscopy
Service Manual
RS

Copyright © by Bruker Corporation
All rights reserved. No part of this publication may be
reproduced, stored in a retrieval system, or transmitted, in any
form, or by any means without the prior consent of the publisher.
Product names used are trademarks or registered trademarks of
their respective holders.
© May 2011: Bruker Corporation
Fällanden, Switzerland
ZTKS0156 / Z31820 / Rev.: 03
For further technical assistance on the NMR magnet system,
please do not hesitate to contact your nearest BRUKER dealer
or contact us directly at:
BRUKER Corporation
Industriestrasse 26
CH - 8117 Fällanden
Switzerland
Phone:+ 41 44 825 91 11
Fax: + 41 44 825 96 96
E-mail:[e-mail]
Internet:www.bruker.com

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ZTKS0156 / Z31820 / Rev.: 03
0 Contact ...........................................................................................................9
1 Introduction..................................................................................................11
2 Safety............................................................................................................15
3 Transportation .............................................................................................31
4 Assembling ..................................................................................................37
5 Operation......................................................................................................79
6 Troubleshooting ..........................................................................................87
7 Maintenance...............................................................................................113
8 Disassembling ...........................................................................................121
A Appendix ....................................................................................................133

4ZTKS0156 / Z31820 / Rev.: 03

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ZTKS0156 / Z31820 / Rev.: 03
Table of Contents
0 Contact ...........................................................................................................9
1 Introduction..................................................................................................11
1.1 General Information................................................................................................ 11
1.2 Limitation of Liability ............................................................................................... 11
1.3 Customer Service................................................................................................... 11
1.4 Warranty................................................................................................................. 11
1.5 Copyright ................................................................................................................ 11
1.6 General View.......................................................................................................... 12
2 Safety............................................................................................................15
2.1 Approved Persons.................................................................................................. 15
2.2 Customer Responsibilities...................................................................................... 16
2.3 Key Words.............................................................................................................. 17
2.4 Residual Risks........................................................................................................ 18
2.4.1 Persons .................................................................................................................. 18
2.4.2 Intended Use .......................................................................................................... 18
2.4.3 Safety Devices ....................................................................................................... 19
2.4.4 Spare Parts ............................................................................................................ 19
2.4.5 Signs and Labels.................................................................................................... 20
2.4.6 Technical Risks ...................................................................................................... 20
2.5 Personal Protective Equipment .............................................................................. 26
2.6 Description of Signs and Labels............................................................................. 27
2.7 Safety Devices ....................................................................................................... 28
2.8 Behavior in Danger and Emergency Situations...................................................... 30
2.9 Fire Department Notification................................................................................... 30
3 Transportation .............................................................................................31
3.1 Safety ..................................................................................................................... 31
3.2 Packaging............................................................................................................... 31
3.2.1 Disposal.................................................................................................................. 32
3.3 Transport Inspection............................................................................................... 32
3.4 Transportation by Fork Lift / Pallet Jack ................................................................. 33
3.5 Transportation with a Crane ................................................................................... 34
3.6 Storing .................................................................................................................... 35
4 Assembling ..................................................................................................37
4.1 Safety ..................................................................................................................... 37
4.2 Assembling Workflow ............................................................................................. 39
4.3 Assembling Work ................................................................................................... 40
4.3.1 Preparing the Cryostat ........................................................................................... 40
4.3.1.1 Removing the Transportation Locks....................................................................... 40

6ZTKS0156 / Z31820 / Rev.: 03
Table of Contents
4.3.1.2 Mounting the Getter Container ............................................................................... 43
4.3.1.3 Checking the Feedthrough Plate ............................................................................ 44
4.3.1.4 Assembling the Nitrogen Tube ............................................................................... 44
4.3.1.5 Assembling the RT Tube ........................................................................................ 46
4.3.1.6 Checking and Fitting the Drop-off Plate.................................................................. 49
4.3.2 Evacuating the Cryostat ......................................................................................... 50
4.3.2.1 Mounting the Vacuum Valve................................................................................... 50
4.3.2.2 Mounting the Vacuum Valve at Evacuated Cryostat .............................................. 51
4.3.2.3 Generating the Vacuum.......................................................................................... 52
4.3.2.4 Rebuilding the Vacuum .......................................................................................... 53
4.3.2.5 Removing the Vacuum Valve ................................................................................. 53
4.3.3 Mounting the Cryogenic Refrigerator Parts ............................................................ 54
4.3.3.1 Mounting the Cold Head......................................................................................... 54
4.3.3.2 Mounting the Rotary Valve Column........................................................................ 56
4.3.3.3 Mounting the Rotary Valve and Flex Lines............................................................. 61
4.3.3.4 Mounting the Compressor ...................................................................................... 67
4.3.3.5 Mounting the Helium Level Sensor......................................................................... 69
4.3.3.6 Mounting the Helium Flow System ......................................................................... 70
4.3.3.7 Mounting the Temperature Control......................................................................... 71
4.3.4 Cooling down from 300 K to 80 K........................................................................... 73
4.3.5 Cooling down to 4.2 K ............................................................................................ 77
5 Operation......................................................................................................79
5.1 Safety ..................................................................................................................... 79
5.2 Energizing............................................................................................................... 80
5.2.1 Inserting the Current Lead...................................................................................... 80
5.2.2 Energizing Procedure ............................................................................................. 81
5.2.3 Cycling Procedure .................................................................................................. 82
5.2.4 Shimming Procedure .............................................................................................. 83
5.2.5 Removing the Current Lead ................................................................................... 84
5.2.6 Complete Energizing .............................................................................................. 84
5.3 Set into Operation................................................................................................... 85
6 Troubleshooting ..........................................................................................87
6.1 Safety ..................................................................................................................... 87
6.2 Problem .................................................................................................................. 88
6.2.1 During Transportation............................................................................................. 88
6.2.2 During Assembling ................................................................................................. 88
6.2.3 During Cool Down .................................................................................................. 90
6.2.4 During Energizing and Shimming ........................................................................... 94
6.2.5 During Operation of the Magnet Stand................................................................... 96
6.2.6 During Standard Operation..................................................................................... 98
6.2.7 During De-energizing and Warming up ................................................................ 101
6.2.8 During Operation of the Cryogenic Refrigerator................................................... 102
6.3 Troubleshooting Work .......................................................................................... 107

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Table of Contents
6.3.1 After a Quench ..................................................................................................... 107
6.3.2 Replacement of the Helium Level Sensor ............................................................ 109
6.3.3 Procedure in case of an alarm signal ................................................................... 110
6.3.4 Procedure in case of Cryogenic Refrigerator failure ............................................ 111
7 Maintenance...............................................................................................113
7.1 Safety ................................................................................................................... 113
7.2 Cleaning ............................................................................................................... 114
7.3 Maintenance Timetable ........................................................................................ 114
7.4 Maintenance Work at the Cryogenic Refrigerator ................................................ 116
7.4.1 Service Kit ............................................................................................................ 116
7.4.2 Flex Lines ............................................................................................................. 117
7.4.3 Replacement of the Rotary Valve and the Cold Head.......................................... 118
8 Disassembling ...........................................................................................121
8.1 Safety ................................................................................................................... 121
8.2 Disassembling Work............................................................................................. 123
8.2.1 De-energizing ....................................................................................................... 123
8.2.2 Warming up from 4.2 K to 300 K .......................................................................... 124
8.2.3 Breaking the Vacuum ........................................................................................... 125
8.2.4 Removing of the Helium Flow System ................................................................. 126
8.2.5 Removing the Cryogenic Refrigerator Parts......................................................... 126
8.2.6 Removing of the RT Tube and the Nitrogen Tube ............................................... 127
8.2.7 Assembling of the Transportation Lock ................................................................ 129
8.2.8 Remount the Magnet Stand ................................................................................. 131
8.2.9 Prepare the Cryostat for Transportation............................................................... 131
A Appendix ....................................................................................................133
A.1 Warning Signs ...................................................................................................... 135
A.2 Figures ................................................................................................................. 137
A.3 Tables................................................................................................................... 141
A.4 Glossary / Abbreviations ...................................................................................... 143
A.5 Technical Data USR Service................................................................................ 145
A.6 Index..................................................................................................................... 153

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ZTKS0156 / Z31820 / Rev.: 03
0Contact
Manufacturer:
Bruker BioSpin AG
Industriestrasse 26
CH-8117 Faellanden
Switzerland
Phone: [phone]
Fax: [phone]
http://www.bruker.com
E-mail: [e-mail]
Please refer to the Model No., Serial No. and Internal Order No. in all correspondence
regarding the NMR system or components thereof.

10 ZTKS0156 / Z31820 / Rev.: 03
Contact

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ZTKS0156 / Z31820 / Rev.: 03
1 Introduction
1.1 General Information
This manual contains important information about the handling of the supplied magnet
system as a part of the magnet system used for NMR analyses. The compliance with all
safety and handling instructions, the applicable local accident prevention and general
safety regulations are necessary for safe work.
The manual is part of the product. It must be kept in the immediate vicinity of the magnet
system and unimpeded access must be ensured at any time. Read the manual carefully
before handling the magnet system or its components.
1.2 Limitation of Liability
The information in this manual will take into account the current state of the technology.
The manufacturer assumes no liability for damages resulting from:
• non-compliance with the instructions and all applicable documentation,
• use for purposes not intended,
• not sufficiently approved persons,
• arbitrary changes or modifications and
• use of not approved spare parts or accessories.
1.3 Customer Service
Technical support is provided by Bruker service via telephone or e-mail. For contact
information see page 9 of this document.
1.4 Warranty
The warranty terms can be found in the sales documents of the magnet system and in
the Terms and Conditions of Bruker BioSpin AG.
1.5 Copyright
No part of this publication may be reproduced, stored in a retrieval system, or transmit-
ted, in any form or by any means without the prior consent of the publisher. Product
names used are trademarks or registered trademarks of their respective holders.

12 ZTKS0156 / Z31820 / Rev.: 03
Introduction
1.6 General View
Figure 1.1: General view RS Cryostat of the Magnet System
1. Cryogenic Refrigerator Compressor
(noise protection cover optionally)
2. Cryogenic Refrigerator Flex Lines
3. Rotary Valve (RV) covered by the
Rotary Valve Column (RVC)
4. Connection Line
5. Helium flow system
6. Current lead turret
7. Cryogenic Refrigerator Cold Head
8. Helium fill-in turret with helium fill-in
port
9. RT bore
10. RT vessel
11. Magnet Stand

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Introduction
The heart of the NMR magnet system is a superconducting magnet located inside the
helium vessel, which is filled with liquid helium. The helium vessel is surrounded by a
radiation shield (RS) both cooled by a Cryogenic Refrigerator. The outer casing, the
room temperature (RT) vessel (10) contains the helium vessel and the radiation shield.
The vacuum inside the RT vessel reduces thermal conduction. RT vessel, helium
vessel, radiation shield, helium turrets, helium flow systems and the RT bore together
build the cryostat of the NMR magnet system. The RT bore (9) allows the access to the
magnetic centre of the NMR magnet system.
The cryostat is mounted on a magnet stand (8). The isolators in the magnet stand
absorb floor vibrations. Different heights and isolators are available optionally.
The helium turrets (5, 8) build the interface of the helium vessel to the outside. The
current lead turret (5) builds the interface for energizing the magnet coil and for
diagnostic. The helium fill-in turret (8) with access to the siphon and connecting plug for
the helium level sensor is used to fill the helium vessel. It is marked with a yellow label.
The helium flow system (6) connects the two helium turrets.
The Cryogenic Refrigerator is a closed loop helium expansion cycle. It consists of a
Compressor (1), two Flex Lines (2), a Remote Rotary Valve inside the Rotary Valve
Column (RVC; 3), a Cold Head (7) and a Connection Line (4) between Remote Rotary
Valve and Cold Head. The Remote Rotary Valve, Flex Lines, Connection Line and Cold
Head are covered with an applicable noise protection cover. For the Compressor a noise
protection is available optionally.
Depending on the customers site restrictions several opportunities for the additional
equipment of the Cryogenic Refrigerator are possible. Refer to the order subscription
and to the supplied manuals of the supplied equipment.

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Introduction

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ZTKS0156 / Z31820 / Rev.: 03
2 Safety
The supplied cryostat of the magnet system was designed and manufactured according
to best available technical knowledge and practice, archived in over 50 years of experi-
ence of Bruker Corporation. International standards for quality and approval recom-
mended for cryostats of superconducting magnets were certified.
Nevertheless non-compliance with the following instructions and safety advice may
cause serious hazards and property damage.
2.1 Approved Persons
Bruker BioSpin AG identifies the following qualifications for personnel performing tasks
on the magnet system or its components:
Approved Customer Personnel:
As a result of professional training by Bruker Service Personnel, experience and
knowledge of applicable regulations these persons are qualified to perform the specific
tasks on the magnet system and its components assigned to them in this manual.
Approved Customer Personnel are qualified to identify possible hazards and risks
associated with the tasks assigned to them and to perform all possible steps to eliminate
or minimize these risks.
Bruker Service Personnel:
These persons are qualified by appropriate qualification and professional training and
experience (including all necessary knowledge of applicable regulations and regulatory
requirements) to perform specific tasks on the magnet system and its components.
Bruker Service Personnel are qualified to identify possible hazards and risks and to
perform all possible steps to eliminate or minimize these risks.

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Safety
2.2 Customer Responsibilities
The customer of the magnet system must obey the security advice and the rules for
safety, accident prevention and environmental protection correctly for the magnet
systems. Furthermore, the customer is responsible for keeping the magnet system in
correct technical condition.
In particular:
• The customer must identify additional dangers resulting from the working conditions
at the site of the magnet system and provide applicable safety measures.
• The customer must ensure that the site plan meets the specified conditions for
operating the magnet system and supplied site planning document.
• The customer must clearly mark the danger area around the magnet system and
post the corresponding instruction plates.
• The customer has to ensure the intended use of the magnet system.
• The customer has to inform the local fire brigade about the special risks of the
magnet system and how to react in the event of an incident.
• The customer must clearly define the responsibilities for operation and main-
tenance.
• The customer must ensure that all employees working with the magnet system have
read and understood the manual.
• The customer has to provide the necessary personal protective equipment for his
employees.
• The customer has to instruct his employees at regular intervals on hazards and
safety measures.
• The customer has to instruct other persons not working on the magnet system but
carrying out work in the same room, for instance cleaning staff or guards.
• The customer has to consider the specific items of this cryostat equipped with a
Cryogenic Refrigerator. The customer is responsible for obeying the advice given in
this manual. In case the Cryogenic Refrigerator is not running correctly his
immediate reaction is mandatory. In case of an unexpected alarm his immediate
response is mandatory. For further instruction refer to chapter ”Troubleshooting”
on page 6-87.
• The customer must ensure that maintenance is performed according to the
schedule listed in chapter ”Maintenance Timetable” on page 7-114.

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ZTKS0156 / Z31820 / Rev.: 03
Safety
2.3 Key Words
iInformation and links for efficient and trouble-free handling and operation.
DANGER
Indicates a hazardous situation which, if not prevented, will result in
death or serious injury.
WARNING
Indicates a hazardous situation which, if not prevented, could result in
death or serious injury.
CAUTION
Indicates a hazardous situation which, if not prevented, may result in
moderate or minor injury.
NOTICE
Hazard, which could result in property damage.

18 ZTKS0156 / Z31820 / Rev.: 03
Safety
2.4 Residual Risks
In the following section, the residual risks from the risk analysis according ISO 14971 are
summarized. To prevent health hazards and hazardous situations obey all safety instruc-
tions and warnings in the manual.
2.4.1 Persons
2.4.2 Intended Use
The supplied magnet systems is designed and intended for NMR spectroscopy only.
WARNING
Risk of injury and property damage by not approved persons.
Incorrect handling of the magnet system from not approved persons may result in
significant bodily injury and property damage.
Thus:
• Work must only be carried out by approved persons with applicable qualifications.
The necessary qualifications are specified in the beginning of the relevant
chapter.
• In case of doubt, contact Bruker Service. Contact information see page 9 of this
document.
WARNING
Risk of damage to life and limb by incorrect use of the magnet system.
Incorrect use of the magnet system can lead to life-threatening situations and
destruction of the magnet system.
Thus:
• Only use the magnet system as intended.
• Do not change the magnet system.
• Do not exceed specified values for operating the magnet system.
• Do not use inserts inside the RT bore not approved by Bruker Service.
Damage claims from damages caused by other than the intended use of the magnet
system are excluded and the customer is held liable.

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ZTKS0156 / Z31820 / Rev.: 03
Safety
2.4.3 Safety Devices
2.4.4 Spare Parts
WARNING
Risk of damage to life and limb due to not sufficient safety devices.
Several safety devices ensure safe operation of the magnet system. They must
always be in correct working condition.
Thus:
• Do not block safety devices.
• Do not remove safety devices.
• Check the operational reliability of the safety devices before working on the
magnet system.
WARNING
Risk of injury and property damage from using incorrect or defective
spare parts and accessories.
Incorrect or defective spare parts can cause serious injuries. They may cause
damaging, malfunctioning and the destruction of the magnet system.
Thus:
• Only use original equipment manufacturer spare parts.
• Only use original equipment manufacturer accessories.

20 ZTKS0156 / Z31820 / Rev.: 03
Safety
2.4.5 Signs and Labels
2.4.6 Technical Risks
Magnetic Field
WARNING
Risk of damage to persons and property due to not readable signs and
labels.
Signs and labels with advice may become not readable.
Thus:
• Maintain signs and labels in a readable state.
• Replace damaged or not readable signs and labels immediately. New signs and
labels can be obtained from Bruker Service.
WARNING
Risk of damage to life and limb due to high magnetic fields.
A magnetic field of more than 0.5 mT (5 Gauss) is life-threatening for people with
pacemakers or metal implants. Ferromagnetic tools in the magnetic field are
significantly hazardous. Disks and electronic devices may be damaged. Duration of
exposure (8 h/day) above the limit of 200 mT can cause damage to health.
Thus:
• Mark the magnetic field of more than 0.5 mT (5 Gauss) before start up.
• The workplace must be outside the 0.5 mT area.
• Keep people with pacemakers and metal implants away from the identified area.
• Keep disks, credit cards and electronic devices away from the identified area.
• Do not use ferromagnetic tools or items within the identified area.
• Only use non-ferromagnetic transportation dewars for the cryogenic agents.
• Only use non-ferromagnetic ladders or steps.