Bruker NMR 600'89 Ascend DNP User manual

Version
Innovation with Integrity
600‘89 Ascend DNP
02
User Manual
NMR

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.
This manual was written by
Renate Petry
Faellanden, Switzerland
© May 8, 2018: Bruker Corporation
ZTKS0304 / Z33130 / 02
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 BioSpin AG
Industriestrasse 26
CH–8117 Faellanden
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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Table of Contents
Contact ...........................................................................................................7
1 Introduction....................................................................................................9
1.1 General Information.................................................................................................. 9
1.2 Limitation of Liability ................................................................................................. 9
1.3 Customer Service..................................................................................................... 9
1.4 Warranty................................................................................................................... 9
1.5 Copyright .................................................................................................................. 9
1.6 General View.......................................................................................................... 10
2 Safety............................................................................................................11
2.1 Approved Persons.................................................................................................. 11
2.2 Customer Responsibilities...................................................................................... 12
2.3 Key Words.............................................................................................................. 13
2.4 Residual Risks........................................................................................................ 15
2.4.1 Persons .................................................................................................................. 15
2.4.2 Intended Use .......................................................................................................... 15
2.4.3 Safety Devices ....................................................................................................... 16
2.4.4 Spare Parts ............................................................................................................ 16
2.4.5 Signs and Labels.................................................................................................... 17
2.4.6 Technical Risks ...................................................................................................... 17
2.5 Personal Protective Equipment .............................................................................. 23
2.6 Description of Signs and Labels............................................................................. 24
2.7 Safety Devices ....................................................................................................... 25
2.8 Behavior in Danger and Emergency Situations...................................................... 26
2.9 Fire Department Notification................................................................................... 26
3 Transportation .............................................................................................27
3.1 Safety ..................................................................................................................... 27
3.2 Packaging............................................................................................................... 27
3.2.1 Disposal.................................................................................................................. 28
3.3 Transport Inspection............................................................................................... 28
3.4 Transportation by Fork Lift / Pallet Jack ................................................................. 29
3.5 Transportation with a Crane ................................................................................... 30
3.6 Storing .................................................................................................................... 31
3.7 Disposal.................................................................................................................. 31
4 Assembling ..................................................................................................33
5 Operation......................................................................................................35
5.1 Safety ..................................................................................................................... 35
5.2 Set into Operation .................................................................................................. 36

4ZTKS0304 / Z33130 / 02
Table of Contents
6 Troubleshooting ..........................................................................................37
6.1 Safety ..................................................................................................................... 37
6.2 Problem .................................................................................................................. 38
6.2.1 During Transportation............................................................................................. 38
6.2.2 During Assembling ................................................................................................. 38
6.2.3 During Cooling Procedure ...................................................................................... 40
6.2.4 During Energizing and Shimming........................................................................... 44
6.2.5 During Operation of the Magnet Stand................................................................... 47
6.2.6 During Standard Operation..................................................................................... 49
6.2.7 During De-energizing and Warming ....................................................................... 51
6.3 Troubleshooting Work ............................................................................................ 52
6.3.1 After a Quench ....................................................................................................... 52
7 Maintenance.................................................................................................53
7.1 Safety ..................................................................................................................... 53
7.2 Cleaning ................................................................................................................. 53
7.3 Maintenance Timetable .......................................................................................... 54
7.4 Maintenance-free Components .............................................................................. 54
8 Disassembling .............................................................................................55
9 Technical Data MS 600‘89 D359 Ascend DNP...........................................57
9.1 Environmental Conditions....................................................................................... 57
9.2 Identification Plate .................................................................................................. 57
9.3 Dimensions............................................................................................................. 58
9.3.1 Weights................................................................................................................... 58
9.3.2 Dimensions for Transportation ............................................................................... 58
9.3.3 Dimensions Cryostat .............................................................................................. 59
9.4 Safety Valves.......................................................................................................... 62
9.5 Nitrogen Level Sensor ............................................................................................ 63
9.6 Helium Level Sensor .............................................................................................. 64
9.7 Temperature Sensors............................................................................................. 65
9.8 Technical Data Magnet........................................................................................... 67
9.9 Fringe Field Plot ..................................................................................................... 68
9.10 Technical Data Sweep Coil .................................................................................... 69
9.11 Filling Volume, Evaporation Rate and Hold Time................................................... 70
9.12 Nitrogen Level Graph ............................................................................................. 71
9.13 Helium Level Graph................................................................................................ 72
9.14 Resistance at Room Temperature.......................................................................... 73
9.15 Sweep Current Lead Resistance............................................................................ 74
9.16 Heater Currents ...................................................................................................... 74
9.17 Sweep Power Supply Settings ............................................................................... 74

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Table of Contents
9.18 Shim Switch Heater................................................................................................ 75
9.19 Energizing Assignment and Currents..................................................................... 76
9.20 Magnetic Center ..................................................................................................... 77
9.21 Cycling Assignment and Shim Currents................................................................. 78
9.22 Cryo Shim Currents................................................................................................ 79
9.23 Deenergizing Assignment and Currents................................................................. 79
9.24 Current Lead .......................................................................................................... 81
9.24.1 Sweep Current Lead .............................................................................................. 82
9.24.2 Shorting Plug.......................................................................................................... 83
9.24.3 Sweep Current Lead Mounting Device................................................................... 84
9.24.4 Wiring Diagram Magnet.......................................................................................... 85
9.24.5 Wiring Diagram Magnet Control and Shims ........................................................... 86
9.24.6 Wiring Diagram Magnet Diagnostic and Temperature Sensors ............................. 87
9.25 Nitrogen Refill Report ............................................................................................. 88
9.26 Helium Refill Report ............................................................................................... 90
Appendix A ...........................................................................................................93
A.1 Warning Signs ........................................................................................................ 93
A.2 Figures ................................................................................................................... 95
A.3 Tables..................................................................................................................... 97
A.4 Index....................................................................................................................... 99

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Table of Contents

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ZTKS0304 / Z33130 / 02
Contact
Manufacturer
Bruker BioSpin AG
Industriestrasse 26
CH–8117 Faellanden
Switzerland
Phone: + 41 44 825 91 11
Fax: + 41 44 825 96 96
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.

8ZTKS0304 / Z33130 / 02
Contact

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1 Introduction
1.1 General Information
This manual contains important information about the handling of the supplied magnet
system used for NMR spectroscopy and its components. The compliance with all safety
and handling instructions, the applicable local accident prevention and general safety
regulations are necessary for safe work.
This manual is part of the product. It must be kept nearby the magnet system and free
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 7 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.

10 ZTKS0304 / Z33130 / 02
Introduction
1.6 General View
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
nitrogen vessel filled with liquid nitrogen. The outer casing, the room temperature (RT)
vessel (2), contains the helium vessel and the nitrogen vessel. The vacuum in the RT
vessel reduces thermal conduction. The RT bore (3) allows the access to the magnetic
center. RT vessel, inner vessels, turrets, flow systems and the RT bore together build the
cryostat of the magnet system.
The cryostat is mounted on a magnet stand (1). The isolators in the magnet stand
absorb floor vibrations. Different heights and isolators are available optionally.
The nitrogen turrets (4) connected with the nitrogen flow system (6) and the heat
exchangers (5) are the interface to the nitrogen vessel. The nitrogen fill-in turret is
marked with a green label.
The helium turrets (8, 9) connected with the helium flow system (7) are the interface of
the helium vessel and the magnet coil. The helium fill-in turret (9) is marked with a yellow
label.
The current lead turret (8) is the interface for energizing the magnet coil and for
diagnostic.
Figure 1.1: General view of a magnet system with 2helium turrets
1 Magnet Stand
2 RT Vessel
3 RT Bore
4 Nitrogen Turrets
5 Heat Exchanger
6 Nitrogen Flow System
7 Helium Flow System
8 Current Lead Turret
9 Helium Fill-in Turret with
Helium fill-in port
10 Sample Case Support

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2 Safety
The supplied cryostat and further equipment of the magnet system were designed and
manufactured according to the best available technical knowledge and practice,
achieved in over 50 years of experience of the Bruker Corporation. International
standards for quality and approval recommended 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.

12 ZTKS0304 / Z33130 / 02
Safety
2.2 Customer Responsibilities
The customer must obey the security advice and the rules for safety, applicable local
accident prevention and environmental protection correctly for the magnet system.
Furthermore, the customer is responsible for keeping the magnet system in good
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
according to the site planning document for operating the magnet system.
• 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
maintenance.
• 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 about the
possible danger at the site of the magnet system.
• The customer must ensure that maintenance is performed according to the
schedule listed in chapter Maintenance Timetable on page 54.

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Safety
2.3 Key Words
Safety instructions in this manual and labels of devices are marked with symbols. The
safety instructions are introduced using indicative words which express the extent of the
hazard.
In order to avoid accidents, personal injury or damage to property, always observe safety
instructions and proceed with care.
DANGER
DANGER indicates a hazardous situation, which, if not avoided, will
result in death or serious injury.
This is the consequence of not following the warning.
1. This is the safety condition.
This is the safety instruction.
WARNING
WARNING indicates a hazardous situation, which, if not avoided, could
result in death or serious injury.
This is the consequence of not following the warning.
1. This is the safety condition.
This is the safety instruction.
CAUTION
CAUTION indicates a hazardous situation, which, if not avoided, may
result in minor or moderate injury or severe material or property
damage.
This is the consequence of not following the warning.
1. This is the safety condition.
This is the safety instruction.

14 ZTKS0304 / Z33130 / 02
Safety
NOTICE
NOTICE indicates a property damage message.
This is the consequence of not following the notice.
1. This is a safety condition.
This is a safety instruction.
SAFETY INSTRUCTIONS
SAFETY INSTRUCTIONS are used for control flow and shutdowns in the
event of an error or emergency.
This is the consequence of not following the safety instructions.
1. This is a safety condition.
This is a safety instruction.
This symbol highlights useful tips and recommendations as well as information
designed to ensure efficient and smooth operation.

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Safety
2.4 Residual Risks
In the following chapter the residual risks from the risk analysis according ISO 14971 are
summarized. To prevent health hazards and hazardous situations obey all safety
instructions and warnings in the manual.
2.4.1 Persons
2.4.2 Intended Use
The supplied magnet system is designed and intended for NMR spectroscopy only.
WARNING
Risk of injury and property damage due to handling by not approved
persons.
Incorrect handling of the magnet system by 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 7 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.

16 ZTKS0304 / Z33130 / 02
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.

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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 ordered 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 active metal implants. Exposure to more than 8 T can cause damage
to health. Duration of exposure (8 h/day) above the limit of 200 mT can cause
damage to health. Ferromagnetic tools in the magnetic field are significantly
hazardous. Disks and electronic devices may be damaged.
Thus:
Mark the magnetic field of more than 0.5 mT (5 Gauss) before start up.
Keep people with active medical implants away from the 0.5 mT (5 Gauss) area.
The permanent workplace of employees must be outside the 0.5 mT (5 Gauss)
area.
Do not stay or work at magnetic fields of more than 8 T.
Prevent exposure of more than 200 mT for more than 8 h/day.
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 or pressure cylinders for the
cryogenic agents.
Only use non-ferromagnetic ladders or steps.

18 ZTKS0304 / Z33130 / 02
Safety
Cryogenic Agents
Electricity
WARNING
Risk of damage to life and limb due to cryogenic agents.
Risk of damage to life and limb due to not correct handling of liquid cryogenic agents.
Within the transition from liquid to gas, helium and nitrogen expand their volume,
causing closed vessels or transportation dewars to burst. The evaporating cryogenic
agents will displace the breathing air. Helium displaces the breathing air in the upper
part of the room, nitrogen displaces the breathing air in the lower parts of the room. In
case of not sufficient ventilation this may result in death by suffocation.
Liquid and gaseous cryogenic agents are extremely cold. Contact with liquid or
gaseous cryogenic agents will lead to cold burns. Contact with the eyes may cause
blindness. Refer to Warning: Low Temperature on page 20.
Thus:
Only use cryogenic agents in well ventilated rooms. In case of doubt ask Bruker
Service.
Wear an oxygen monitor on the body during service and maintenance work.
Prevent any skin contact with liquid or gaseous cryogenic agents.
WARNING
Risk of damage to life and limb due to electricity.
Risk of damage to life and limb due to contact with electrical lines and damaged
insulation.
Thus:
Work on electrical equipment must be done by an approved electrical technician.
Keep moisture away from electrical lines to prevent short-circuits.
Check the magnet system electrical grounding before start.
Switch the power OFF before working on the Bruker Power Supply or further
equipment.

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ZTKS0304 / Z33130 / 02
Safety
Quench
Gas under Pressure
WARNING
Risk of suffocation during a quench of the magnet system.
A quench is the very fast de-energizing of the magnet by loss of its superconductivity.
The stored magnetic energy is converted into heat and thus large quantities of helium
evaporate. The evaporating helium will displace the breathing air. In case of not
sufficient ventilation this may result in death by suffocation.
Thus:
The magnet system site must be well ventilated. In case of doubt contact Bruker
Service.
The evaporating gas may resemble smoke. Never pour water on the magnet
system.
WARNING
Risk of injury due to gas under pressure inside the cryostat and further
equipment.
The helium or the nitrogen vessel of the cryostat may get sealed off due to ice
formation inside the helium or the nitrogen turrets in case of non-compliance with the
instruction given in this manual. This may lead to overpressure and damage of the
helium or the nitrogen vessel.
Manipulations of components with gas under pressure may lead to injury and
property damage.
Thus:
In case of ice inside the helium or the nitrogen turrets contact Bruker Service
immediately.
Release the pressure to the recommended value before working on components
with gas under pressure.
Do not seal cryogenic agent vessels of the magnet system or the transportation
dewars.
Do not connect high pressure transportation dewars to the magnet system.
Completely eliminate the high pressure from the transportation dewars before
connecting and transferring cryogenic agents.

20 ZTKS0304 / Z33130 / 02
Safety
Low Temperatures
Spontaneous Ignition and Explosion
Risk of Slippage
WARNING
Risk of injury due to low temperatures of liquids and metal parts.
Physical contact with extremely cold liquids and metal parts may cause serious
injuries. Contact with the skin may cause cold burns. Contact with the eyes may
cause blindness.
Thus:
Always wear protective goggles, protective gloves and protective clothes while
handling with liquid cryogenic agents or metal parts in contact with liquid cryogenic
agents.
Protect temperature sensitive components such as O-rings from contact with liquid
cryogenic agents.
WARNING
Risk of injury from spontaneous ignition and explosion caused by
liquid oxygen.
Pure oxygen condenses on extremely cold metal pieces. Together with oil it may
ignite spontaneously. In case of fire the pure oxygen may cause an explosion.
Thus:
Do not smoke near the magnet system.
Do not use open flames near the magnet system.
Keep the environment around the magnet system clean.
Do not leave oily rags near the magnet system.
WARNING
Risk of injury from slippage.
The accumulation of condensed water on the floor and ladders causes slippery
surfaces.
Thus:
Always wear safety shoes with an anti-slip sole.
Be careful using ladders.
Clean floor and ladders regularly.