Bruker BioSpin 500'154 USP User manual

NMR Spectroscopy
User Manual
500´154 USP

This Manual was written by
Peter van Bommel
Copyright by Bruker BioSpin AG
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.
© September 2010, Bruker BioSpin AG
Fällanden, Switzerland
ZTKS0160 / Z31926 / Rev.: 00

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ZTKS0160 / Z31926 / Rev.: 00
0 Contact ...........................................................................................................9
1 Introduction..................................................................................................11
2 Safety............................................................................................................13
3 Transportation .............................................................................................29
4 Assembling ..................................................................................................35
5 Operation......................................................................................................37
6 Troubleshooting ..........................................................................................39
7 Maintenance.................................................................................................55
8 Disassembling .............................................................................................57
A Appendix ......................................................................................................59

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ZTKS0160 / Z31926 / Rev.: 00
0 Contact ...........................................................................................................9
1 Introduction..................................................................................................11
1.1 General Information................................................................................................ 11
1.1.1 Limitation of Liability ............................................................................................... 11
1.1.2 Customer Service................................................................................................... 11
1.1.3 Warranty................................................................................................................. 11
1.1.4 Copyright ................................................................................................................ 11
1.2 General View.......................................................................................................... 12
2 Safety............................................................................................................13
2.1 Persons in charge .................................................................................................. 13
2.2 Customer Responsibilities...................................................................................... 14
2.3 Key Words.............................................................................................................. 15
2.4 Residual Risks........................................................................................................ 16
2.4.1 Persons .................................................................................................................. 16
2.4.2 Intended Use .......................................................................................................... 16
2.4.3 Safety Devices ....................................................................................................... 17
2.4.4 Spare Parts ............................................................................................................ 17
2.4.5 Signs and Labels.................................................................................................... 18
2.4.6 Technical Risks ...................................................................................................... 18
2.4.7 Cautions ................................................................................................................. 23
2.5 Personal Protective Equipment .............................................................................. 24
2.6 Description of Signs and Labels............................................................................. 25
2.7 Safety Devices ....................................................................................................... 26
2.8 Behavior in Danger and Emergency Situations...................................................... 27
2.9 Fire Department Notification................................................................................... 27
3 Transportation .............................................................................................29
3.1 Packaging............................................................................................................... 29
3.2 Transport Inspection............................................................................................... 30
3.3 Transportation by Fork Lift / Pallet Jack ................................................................. 31
3.4 Transportation with a Crane ................................................................................... 32
3.5 Storing .................................................................................................................... 33
4 Assembling ..................................................................................................35
4.1 Safety ..................................................................................................................... 35
5 Operation......................................................................................................37
5.1 Safety ..................................................................................................................... 37
5.1.1 Set into Operation .................................................................................................. 38

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6 Troubleshooting ..........................................................................................39
6.1 Safety ..................................................................................................................... 39
6.2 Problem .................................................................................................................. 40
6.2.1 During Transportation............................................................................................. 40
6.2.2 During Assembling ................................................................................................. 40
6.2.3 During Cool Down .................................................................................................. 42
6.2.4 During Energizing and Shimming ........................................................................... 46
6.2.5 During Operation of the Magnet Stand................................................................... 48
6.2.6 During Standard Operation..................................................................................... 50
6.2.7 During De-energizing and Warming up .................................................................. 52
6.3 Troubleshooting Work ............................................................................................ 53
6.3.1 After a quench ........................................................................................................ 53
7 Maintenance.................................................................................................55
7.1 Safety ..................................................................................................................... 55
7.2 Cleaning ................................................................................................................. 56
7.3 Maintenance Timetable .......................................................................................... 56
8 Disassembling .............................................................................................57
8.1 Safety ..................................................................................................................... 57
A Appendix ......................................................................................................59
A.1 Warning Signs ........................................................................................................ 61
A.2 Figures.................................................................................................................... 63
A.3 Tables..................................................................................................................... 65
A.4 Glossary / Abbreviations......................................................................................... 67
A.5 Technical Data MS 500‘154 USP ........................................................................... 69
A.6 Index..................................................................................................................... 101

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

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0Contact
Manufacturer:
Bruker BioSpin AG
Industriestrasse 26
CH-8117 Fällanden
Schweiz
Phone: [phone]
Fax: [phone]
http://www.bruker.com
Please refer to the Model No., Serial No. and Internal Order No. in all correspondence
regarding the NMR system or components thereof.

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ZTKS0160 / Z31926 / Rev.: 00
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.
1.1.1 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 unauthorized spare parts or accessories.
1.1.2 Customer Service
Technical support is provided by Bruker service via telephone or e-mail. For contact
information see page 9 of this document.
1.1.3 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.
1.1.4 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.

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1.2 General View
The heart of the 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 (1)
contain the helium and the nitrogen vessels. The vacuum within the RT vessel reduces
thermal conduction.
The RT bore (8) allows the access to the magnetic center of the cryostat. RT vessel,
inner vessels, turrets, flow systems and the RT bore together build the cryostat of the
magnet system.
The three helium turrets (2, 3, 5) build the interface of the helium vessel to the outside.
The high current lead turret (2) is for energizing the magnet coil and the current lead
turret is for magnet diagnostic (3). The helium fill-in turret (5) with access to the siphon
and connecting plug for the helium level sensor is used to fill the helium vessel. It is mar-
ked with a yellow label. The helium flow system (4) connects the helium turrets.
The four nitrogen turrets (7) connected with the nitrogen flow system (6) and the heat
exchangers build the interface to the nitrogen vessel.
The cryostat is mounted on a magnet stand (9). The dampers in the magnet stand
absorb floor vibrations. Different heights and dampers are available optionally.
Figure 1.1: General view Cryostat of the Magnet System
1 RT vessel
2 High current lead turret
3 Current lead turret
4 Helium flow system
5 Helium fill-in turret with helium
fill-in port
6 Nitrogen flow system
7 Nitrogen turrets
8 RT bore
9 Magnet stand

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2 Safety
The supplied cryostat of the magnet system was designed and manufactured according
best available technical knowledge and practice, archived in over 50 years of experience
of Bruker BioSpin AG. International standards for quality and approval recommended for
cryostats of superconducting magnets were certified.
Nevertheless non-compliance with the following instructions and safety advices may
cause serious hazards and property damage.
2.1 Persons in charge
In this manual the following qualifications are referenced:
Bruker Service
As a result of professional training, experience and knowledge of applicable regulations
they are approved to perform work on magnet systems. They are approved to self-iden-
tify dangerous situations and to take applicable measures.
Approved Persons of the Customer
As a result of professional training, experience and knowledge of applicable regulations
and instruction by the customer, this group of people is approved to perform the duties
assigned to them. They are approved to recognize dangerous situations and to take
applicable measures.

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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 determine additional dangers resulting from the working condi-
tions 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 has to mark the danger area around the magnet system and post the
corresponding instruction plates.
• 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.
• The customer has to obey the specified maintenance intervals given in this manual
(see chapter ”Maintenance Timetable” on page 7-56).

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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
minor or moderate injury.
NOTICE
Hazard, which could result in property damage.

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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
WARNING
Risk of injury and property damage from 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 use the magnet system to demonstrate strong magnetic fields.
• Do not exceed specified values for operating the magnet system.
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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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:
• Use only original equipment manufacturer spare parts.
• Use only original equipment manufacturer accessories.

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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.

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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
and their dewars. Within the transition from liquid to gas, Helium and Nitrogen
expands their volume, causing closed vessels to burst.
The evaporating cryogenic agents will displace the air. In case of not sufficient ven-
tilation this may result in death by suffocation. Helium displaces oxygen in the upper
part of the room, Nitrogen displaces oxygen in the lower parts of the room.
Liquid and gaseous cryogenic agents are extremely cold. Contact with liquid or
gaseous cryogenic agents will lead to cold burns.
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 accidental ground before start up.
• Switch power off before working on the power supply or further equipment.

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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 oxygen. 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 icing inside the Helium or the Nitrogen turrets contact Bruker Service
immediately.
• Release the pressure before working on components with gases under pressure.
• Do not seal cryogenic agent vessels of the magnet system or the transport
dewars.
• Do not connect high pressure transport dewars for liquid cryogenic agents to the
magnet system. Completely eliminate the high pressure from the transport
dewars before connecting and transferring.