Bruker NMR iProbe HR-Liquids User manual

iProbes HR-Liquids /
HR-MAS
User Manual
Version 001
Innovation with Integrity
●
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 re-
spective holders.
This manual was written by
© June 26, 2018 Bruker Corporation
Document Number: Z4D13588
P/N: Z33146
For further technical assistance for this product, please do not hesitate to contact your
nearest BRUKER dealer or contact us directly at:
Bruker Corporation
Industriestrasse 26
CH-Fällanden
Switzerland
Phone: [phone]
E-mail: [email protected]
Internet: www.bruker.com

Contents
Z33146_1_001 iii
Contents
1 About This Manual .............................................................................................................................5
1.1 Policy Statement .................................................................................................................5
1.2 Symbols and Conventions ..................................................................................................5
2 Introduction.........................................................................................................................................7
2.1 Overview .............................................................................................................................7
2.2 Intended Use.......................................................................................................................7
2.3 Installation and Initial Commissioning.................................................................................7
2.4 Limitation of Liability............................................................................................................7
2.5 Warranty Terms ..................................................................................................................7
2.6 Customer Service ...............................................................................................................8
2.7 Product Safety and Electromagnetic Compatibility .............................................................8
3 Safety...................................................................................................................................................9
3.1 System Owner's Responsibility...........................................................................................9
3.2 Personnel Requirements ..................................................................................................10
3.2.1 Qualifications ....................................................................................................................10
3.2.2 Unauthorized Persons ......................................................................................................11
3.3 Location of the Safety Label .............................................................................................11
3.4 Basic Dangers...................................................................................................................11
3.4.1 General Workplace Dangers.............................................................................................11
3.4.2 Dangers from Magnetic Fields ..........................................................................................12
3.4.3 Dangers Due to High Temperatures .................................................................................13
3.4.4 Danger from Chemical Substances ..................................................................................13
3.5 Environmental Protection..................................................................................................14
4 Transport, Packaging and Storage .................................................................................................15
4.1 Symbols on the Packaging ...............................................................................................15
4.2 Inspection at Delivery........................................................................................................15
4.3 Packaging .........................................................................................................................16
4.4 Storage .............................................................................................................................16
5 Design and Function ........................................................................................................................17
5.1 Overview ...........................................................................................................................17
5.2 Brief Description................................................................................................................18
5.3 Connections iProbe HR-Liquids........................................................................................19
5.4 Connections iProbe HR-MAS ...........................................................................................19
5.5 Connections at the Rear Side of iProbes..........................................................................20
6 Installation.........................................................................................................................................21
6.1 Quick-Lock Mounting ........................................................................................................21
6.2 iProbe Mounting with Quick-Lock .....................................................................................23
6.2.1 Installation of iProbe HR-Liquids.......................................................................................24
6.2.2 Installation of iProbe HR-MAS ..........................................................................................25
7 Operation...........................................................................................................................................27
7.1 General Operating Guidelines ..........................................................................................27

Contents
iv Z33146_1_001
7.2 Operating States of the iProbe..........................................................................................28
7.3 ATMA ................................................................................................................................29
7.4 Properties of the iProbe ....................................................................................................30
7.5 Sample Carrier and NMR Tubes for HR-Liquids...............................................................35
7.5.1 Glass Tubes......................................................................................................................36
7.5.1.1 Sample Depth and Filling Height ......................................................................................36
7.5.1.2 Sample Diameter ..............................................................................................................36
7.6 Specific iProbe HR-MAS Hardware and Operations.........................................................36
7.6.1 MAS Unit...........................................................................................................................36
7.6.2 Transfer System................................................................................................................37
7.6.3 Variable Temperature Unit (VTU) .....................................................................................38
7.6.4 Gradient Amplifier .............................................................................................................38
7.6.5 Tuning & Matching ............................................................................................................38
7.6.6 Shimming ..........................................................................................................................38
7.6.6.1 Mounting Angle .................................................................................................................39
7.6.6.2 Shimming in the TopShim Manual Mode ..........................................................................41
8 Maintenance......................................................................................................................................43
8.1 Cleaning............................................................................................................................43
8.1.1 Before Cleaning ................................................................................................................43
8.1.2 Cleaning the Outer Shell of the Device.............................................................................43
8.1.3 Other Cleaning Operations ...............................................................................................43
9 Troubleshooting ...............................................................................................................................45
9.1 Specific for iProbes HR-MAS............................................................................................45
10 Replacement of Parts.......................................................................................................................47
10.1 Returning the Unit for Repair ............................................................................................47
11 Dismantling and Disposal................................................................................................................49
11.1 Dismantling .......................................................................................................................49
11.2 Disposal Europe................................................................................................................49
11.3 Disposal USA and Other Countries ..................................................................................50
12 Technical Data ..................................................................................................................................51
12.1 General Information ..........................................................................................................51
12.2 Environmental Conditions .................................................................................................51
12.3 iProbe Type Plate .............................................................................................................52
13 Contact ..............................................................................................................................................53

About This Manual
Z33146_1_001 5 / 56
1 About This Manual
1.1 Policy Statement
It is Bruker’s policy to improve products as new techniques and components become
available. Bruker reserves the right to change specifications at any time.
Every effort has been made to avoid errors in text and figure presentation in this publication.
In order to produce useful and appropriate documentation, we welcome your comments on
this publication. Field Service Engineers are advised to check regularly with Bruker for
updated information.
Bruker is committed to providing customers with inventive, high-quality, environmentally-
sound products and services.
1.2 Symbols and Conventions
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.
uThis 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.
uThis 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.
uThis is the safety instruction.

About This Manual
6 / 56 Z33146_1_001
NOTICE
NOTICE indicates a property damage message.
This is the consequence of not following the notice.
1. This is a safety condition.
uThis 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.
uThis is a safety instruction.
This symbol highlights useful tips and recommendations as well as information designed to
ensure efficient and smooth operation.

Introduction
Z33146_1_001 7 / 56
2 Introduction
2.1 Overview
2.2 Intended Use
The device has been designed and constructed solely for the intended use described here.
The Bruker iProbe is a high resolution NMR probe for measuring NMR samples in a
spectrometer. The iProbe can only be operated when installed in a magnet, as described
within this manual. Operating the iProbe outside the magnet is not permitted.
Intended use also includes compliance with all specifications within this manual.
Any use which exceeds or differs from the intended use shall be considered improper use.
No claims of any kind for damage will be entertained if such claims result from improper use.
2.3 Installation and Initial Commissioning
Initial installation, initial commissioning, retrofitting, repairs, adjustments or dismantling of the
device must only be carried out by Bruker Service or personnel authorized by Bruker.
Damage due to servicing that is not authorized by Bruker is not covered by your warranty.
2.4 Limitation of Liability
All specifications and instructions in this manual have been compiled taking account of
applicable standards and regulations, the current state of technology and the experience and
insights we have gained over the years.
The manufacturer accepts no liability for damage due to:
• Failure to observe this manual.
• Improper use.
• Deployment of untrained personnel.
• Unauthorized modifications.
• Technical modifications.
• Use of inadmissible spare parts.
The actual scope of supply may differ from the explanations and depictions in this manual in
the case of special designs, take-up of additional ordering options, or as a result of the latest
technical modifications.
The undertakings agreed in the supply contract, as well as the manufacturer's Terms and
Conditions and Terms of Delivery, and the legal regulations applicable at the time of the
conclusion of the contract shall apply.
2.5 Warranty Terms
The warranty terms are included in the manufacturer's Terms and Conditions.

Introduction
8 / 56 Z33146_1_001
2.6 Customer Service
Our customer service division is available to provide technical information. See the chapter
Contact for contact information.
In addition, our employees are always interested in acquiring new information and experience
gained from practical application; such information and experience may help improve our
products.
2.7 Product Safety and Electromagnetic Compatibility
The device complies with the standard
• IEC 61010-1 and with UL 61010-1 / CSA C22.2 No. 61010-1-04 Safety Requirements for
Electrical Equipment.
• IEC 61326-1 for Electromagnetic Compatibility (EMC)

Safety
Z33146_1_001 9 / 56
3 Safety
3.1 System Owner's Responsibility
System Owner
The term system owner refers to the person who operates the device for trade or commercial
purposes, or who surrenders the device to a third party for use/application, and who bears
the legal product liability for protecting the user, the personnel or third parties during the
operation.
System Owner‘s Obligations
The device is used in the industrial sector, universities and research laboratories. The system
owner of the device must therefore comply with statutory occupational safety requirements.
In addition to the safety instructions in this manual, the safety, accident prevention and
environmental protection regulations governing the operating area of the device must be
observed.
In this regard, the following requirements should be particularly observed:
• The system owner must obtain information about the applicable occupational safety
regulations, and - in the context of a risk assessment - must determine any additional
dangers resulting from the specific working conditions at the usage location of the device.
The system owner must then implement this information in a set of operating instructions
governing operation of the device.
• During the complete operating time of the device, the system owner must assess whether
the operating instructions issued comply with the current status of regulations, and must
update the operating instructions if necessary.
• The system owner must clearly lay down and specify responsibilities with respect to
installation, operation, troubleshooting, maintenance and cleaning.
• The system owner must ensure that all personnel dealing with the device have read and
understood this manual. In addition, the system owner must provide personnel with
training and hazards information at regular intervals.
• The system owner must provide the personnel with the necessary protective equipment.
• The system owner must warrant that the device is operated by trained and authorized
personnel as well as all other work, such as transportation, mounting, start-up, the
installation, maintenance, cleaning, service, repair and shutdown, that is carried out on the
device.
• All personnel who work with, or in the close proximity of the device, need to be informed of
all safety issues and emergency procedures as outlined in this user manual.
• The system owner must document the information about all safety issues and emergency
procedures in a laboratory SOP (Standard Operating Procedure). Routine briefings and
briefings for new personnel must take place.
• The system owner must ensure that new personnel are supervised by experienced
personnel. It is highly recommended to implement a company training program for new
personnel on all aspects of product safety and operation.
• The system owner must ensure that personnel are regularly informed of the potential
hazards within the laboratory. This is all personnel that work in the area, but in particular
laboratory personnel and external personnel such as cleaning and service personnel.

Safety
10 / 56 Z33146_1_001
• The system owner is responsible for taking measures to avoid inherent risks in the
handling of dangerous substances, preventing industrial disease, and providing medical
first aid in emergencies.
• The system owner is responsible for providing facilities according to the local regulations
for the prevention of industrial accidents and generally accepted safety regulations
according to the rules of occupational medicine.
• All substances needed for operating and cleaning the device samples, solvents, cleaning
agents, gases, etc. have to be handled with care and disposed of appropriately. All hints
and warnings on storage containers must be read and adhered to.
• The system owner must ensure that the work area is sufficiently illuminated to avoid
reading errors and faulty operation.
• The system owner must ensure that the laboratory is equipped with an oxygen warning
device, in case the device is operated with nitrogen.
Furthermore, the system owner is responsible for ensuring that the device is always in a
technically faultless condition. Therefore, the following applies:
• The system owner must ensure that the maintenance intervals described in this manual
are observed.
• The system owner must ensure that all (electrical, mechanical, etc.) safety devices are
regularly checked to ensure full safety functionality and completeness.
3.2 Personnel Requirements
Only trained Bruker personnel are allowed to initially install, retrofit, repair, adjust and
dismantle the unit!
3.2.1 Qualifications
This manual specifies the personnel qualifications required for the different areas of work,
listed below:
Laboratory Personnel
Laboratory personnel are health care professionals, technicians, and assistants staffing a
research or health care facility where specimens are grown, tested, or evaluated and the
results of such measurements are recorded. Laboratory personnel are able to carry out
assigned work and to recognize and prevent possible dangers self-reliant due to their
professional training, knowledge and experience as well as profound knowledge of applicable
regulations.
The workforce must only consist of persons who can be expected to carry out their work
reliably. Persons with impaired reactions due to, for example, the consumption of drugs,
alcohol, or medication are prohibited from carrying out work on the device.
When selecting personnel, the age-related and occupation-related regulations governing the
usage location must be observed.

Safety
Z33146_1_001 11 / 56
3.2.2 Unauthorized Persons
WARNING
Risk to life for unauthorized personnel in the work area
Unauthorized personnel who do not meet the requirements described in this manual will not
be familiar with the dangers in the work area. Therefore, unauthorized persons face the risk
of serious injury or death.
3.3 Location of the Safety Label
The laboratory supervisor is responsible for ensuring that all the warning labels are
maintained in their proper place any time that the device is used.
3.4 Basic Dangers
The following section specifies residual risks which may result from using the device and
have been established by means of a risk assessment.
In order to minimize health hazards and avoid dangerous situations, follow the safety
instructions specified here as well as in the following chapters of this manual.
3.4.1 General Workplace Dangers
WARNING
Danger to life from nonfunctional or insufficient safety devices!
If safety devices are not functioning or are disabled, there is a danger of serious injury or
death.
uCheck that all safety devices are fully functional and correctly installed before starting
work.
uNever disable or bypass safety devices.
uEnsure that all safety devices are always accessible.
CAUTION
Risk of injury and property damage due to incorrect handling of the iProbe.
uDo not hold the iProbe by its tube. Always hold it by its body.
uNever touch the pins of the connectors and plugs.

Safety
12 / 56 Z33146_1_001
CAUTION
Accident hazard from pressurized air or nitrogen gas
There exists a small risk of injury when handling the gas supply of the iProbe incorrectly.
1. Pressurized air / nitrogen can enter the body via small skin injuries.
2. Pressurized air / nitrogen can cause eye injury or tinnitus.
uNever cover the flush gas supply by hand.
uWear protective googles and ear protection.
CAUTION
Danger of injury from tripping over dirt and scattered objects!
Dirt and scattered objects may cause people to slip or trip, resulting in personal injuries.
uAlways keep the work area clean.
uRemove objects which are no longer required from the work area and particularly from
the floor.
uIndicate unavoidable hazards using marking tape.
3.4.2 Dangers from Magnetic Fields
WARNING
Risk to life 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.
uMark the magnetic field of more than 0.5mT (5Gauss) before start up.
uKeep people with active medical implants or heart pacemakers away from the 0.5mT
(5Gauss) area.
uThe permanent workplace of employees must be outside the 0.5mT (5Gauss) area.
uDo not stay or work at magnetic fields of more than 8T.
uPrevent exposure of more than 200mT for more than 8h/day.
uKeep disks, credit cards and electronic devices away from the identified area.
uDo not use ferromagnetic tools or items within the identified area.
uOnly use non-ferromagnetic transportation dewars or pressure cylinders for the
cryogenic agents.
uOnly use non-ferromagnetic ladders or steps.
uRemove magnetic items (jewelry, watches, pens etc.) before carrying out maintenance
work.
The magnetic field of the device does not cause any personal injuries or property damage.
For further information see the manual of the magnet used.

Safety
Z33146_1_001 13 / 56
3.4.3 Dangers Due to High Temperatures
CAUTION
Accident hazard from contact with hot surfaces on the probe.
Contact with the hot surfaces of the probe may result in serious burns.
uCheck the probe temperature in TopSpin.
uPut on gloves before handling the probe.
3.4.4 Danger from Chemical Substances
WARNING
Danger of injury from glassware or ceramics breakage
Broken glassware or ceramics may cause minor injuries or material damage, but may also
result in a life threatening situation if hazardous substances are used.
uIf glassware or ceramics breaks, refer to the corresponding precautions and cleaning/
disinfection instructions.
uWear protective equipment.
uPerform all tasks with the glassware or ceramics carefully.
uBefore carrying out any maintenance work, remove the samples and use dummy
samples if necessary.
uStrictly observe the correct sample adjustment, i.e. the maximal sample depth.
uAlways transport the glassware or ceramics with the cover, if applicable. Never turn the
glassware or ceramics upside down or on its side.
uThe laboratory supervisor is responsible for:
ðEstablishing and enforcing standard sample handling and cleaning procedures.
ðEstablishing and enforcing the use of protective clothing and equipment.
ðTraining laboratory personnel.
ðPreparing an emergency procedure.
WARNING
Exposure and other health hazards to maintenance personnel.
If contaminated, the device must be cleaned before any maintenance work can be
performed.
uRegister all substances with which the device has come into contact.
uSign a certification form verifying that the device has been properly cleaned if
contaminated to protect maintenance personnel.
uObviously contaminated, insufficiently cleaned units, as well as units without a signed
cleaning certification will not be repaired and will be returned to the sender.

Safety
14 / 56 Z33146_1_001
NOTICE
Material damage hazard from material contact with NMR solvents
Material damage may result when the device comes in contact with NMR solvents.
uFollow instructions provided in the manual for correct handling of solvents.
uIf surface damage occurs, contact Bruker for repair of damaged parts.
3.5 Environmental Protection
NOTICE
Danger to the environment from incorrect handling of pollutants!
Incorrect handling of pollutants, particularly incorrect waste disposal, may cause serious
damage to the environment.
uAlways observe local environmental regulations regarding handling and disposal of
pollutants.
uTake the appropriate actions immediately if pollutants escape accidentally into the
environment. If in doubt, inform the responsible municipal authorities about the damage
and ask about the appropriate actions to be taken.
The following pollutants are used:
Cleaning
liquids
Cleaning liquids incorporating solvents contain toxic substances. They must
not be allowed to escape into the environment. Disposal must be carried out
by a specialist disposal company.

Transport, Packaging and Storage
Z33146_1_001 15 / 56
4 Transport, Packaging and
Storage
Initial installation, initial commissioning, retrofitting, repairs, adjustments or dismantling of the
device must only be carried out by Bruker Service or personnel authorized by Bruker.
Damage due to servicing that is not authorized by Bruker is not covered by your warranty.
4.1 Symbols on the Packaging
The following symbols are affixed to the packaging material. Always observe the symbols
during transport and handling.
Fragile Marks packages with fragile or sensitive
contents.
Handle the package with care; do not allow the
package to fall and do not allow it to be
impacted.
Table4.1: Symbols on the Packaging
4.2 Inspection at Delivery
Upon receipt, immediately inspect the delivery for completeness and transport damage.
Figure4.1: Shock Watch
Therefore, check the Shock watch on the package of the iProbe. In case the sensor has been
activated according to the description on the labels follow the procedure below.
Proceed as follows in the event of externally apparent transport damage:
• Do not accept the delivery, or only accept it subject to reservation.
• Note the extent of the damage on the transport documentation or the shipper's delivery
note.
• Initiate complaint procedures.
Issue a complaint with respect to each defect immediately following detection. Damage
compensation claims can only be asserted within the applicable complaint deadlines.

Transport, Packaging and Storage
16 / 56 Z33146_1_001
4.3 Packaging
About Packaging
The individual packages are packaged in accordance with anticipated transport conditions.
Only environmentally friendly materials have been used in the packaging.
The packaging is intended to protect the individual components from transport damage,
corrosion and other damage prior to assembly. Therefore do not destroy the packaging and
only remove it shortly before assembly.
Handling Packaging Materials
Keep the original container and packing assembly, at least as long as the warranty is valid, in
case the unit has to be returned to the factory. When the packaging material is no longer
needed dispose of it in accordance with the relevant applicable legal requirements and local
regulations.
4.4 Storage
Storage of the Packages
Store the packages under the following conditions:
• Do not store outdoors.
• Store in dry and dust-free conditions.
• Do not expose to aggressive media.
• Protect against direct sunlight.
• Avoid mechanical shocks.
• Storage temperature: 15 to 35 °C.
• Relative humidity: max. 60%.
• If stored for longer than 3 months, regularly check the general condition of all parts and
the packaging. If necessary, top-up or replace preservatives.
Under certain circumstances, storage instructions may be affixed to packages which expand
the requirements specified here. Comply with these accordingly.

Design and Function
Z33146_1_001 17 / 56
5 Design and Function
5.1 Overview
The Bruker iProbe is a high-resolution NMR probe for measuring NMR samples in a
spectrometer. The iProbe can only be operated when installed in a magnet, as described
within this manual. Operating the iProbe outside the magnet is not permitted.
The ATMA (automatic Tuning & Matching) unit is integrated in the iProbe, therefore no extra
unit has to be installed. Please refer to the section ATMA [}29].
The following diagrams show the connections for the different applications of the iProbe and
the necessary infrastructure around the magnet.
Setup with iProbe HR-Liquids
Figure5.1: Diagram of a setup with iProbe HR-Liquids
Setup with iProbe HR-MAS
High Resolution Magic Angle Spinning (HR-MAS) is a technique for the analysis of samples
with inhomogeneous magnetic susceptibilities, like, for example, semi-solids, gels, or tissues.
By spinning at the magic angle, line broadening effects due to dipolar interactions and
susceptibility differences within the sample are removed resulting in high resolution quality
spectra.
HR-MAS probes are configured with a Z-gradient aligned along the magic angle enabling the
researcher to access a wide variety of NMR experimental techniques including gradient
enhanced solvent suppression and artifact free 2D homo-nuclear and hetero-nuclear
experiments.

Design and Function
18 / 56 Z33146_1_001
Figure5.2: Diagram of a setup with iProbe HR-MAS
5.2 Brief Description
Figure5.3: iProbe installed in the magnet
The full support of all functionality of the iProbe is guaranteed only for AV NEO and newer
spectrometers. No external filters are required, unless differently stated in the documentation
accompanying the iProbe.

Design and Function
Z33146_1_001 19 / 56
5.3 Connections iProbe HR-Liquids
iProbe HR-Liquids Connections at the Front Panel
Figure5.4: iProbe HR-Liquids connections at the front panel
1 Z-gradient 3 BFB-cable (Bruker Field Bus coming
from the VT unit)
2 Flush gas 4 RF-cables
Connections at the Front
The BFB-cable (Bruker Field Bus) contains the electrical signals for ATM, PICS and the
temperature control. The flush gas provides the RF-circuits with dry air for cooling. Read the
Probe Instructions (P/N Z156810) about the flush gas supply use and requirements.
5.4 Connections iProbe HR-MAS
Figure5.5: iProbe HR-MAS connections at the front panel
1 Z-gradient 5 Flush gas
2 Drive 6 BFB-cable
3 Eject 7 RF-cables
4 Spinning rate
Connections at the Front
The BFB-cable (Bruker Field Bus) contains the electrical signals for ATM, PICS and the
temperature control. The flush gas provides the RF-circuits with dry air for cooling. Read the
Probe Instructions (P/N Z156810) for more information about the flush gas supply usage and
requirements.

Design and Function
20 / 56 Z33146_1_001
The iProbe HR-MAS uses only four pneumatic connections from the MAS Unit: Drive, Eject,
Bearing and Frame Flush. Bearing is connected to the VT-gas line using a T-piece and
Bearing Sens must branch off to the output of Bearing (see Figure 5.2 [}18] for the system
overview and Installation of iProbe HR-MAS [}25] for the details of the installation).
5.5 Connections at the Rear Side of iProbes
At the rear side the VT-gas hose is connected with a Johnston connector.
Figure5.6: VT-gas hose with Johnston connector.