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iProbes HR-Liquids /
HR-MAS
User Manual
Version 001
NMR
Innovation with Integrity

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Summary of Contents for Bruker NMR iProbe HR-Liquids

  • Page 1 iProbes HR-Liquids / HR-MAS ● User Manual Version 001 Innovation with Integrity...
  • Page 2 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: +41 44 825 97 97 E-mail: cryoprobe.service.ch@bruker.com...
  • Page 3: Table Of Contents

    Contents Contents About This Manual .......................... 5 Policy Statement ......................... 5 Symbols and Conventions .................... 5 Introduction............................ 7 Overview .......................... 7 Intended Use........................ 7 Installation and Initial Commissioning................. 7 Limitation of Liability...................... 7 Warranty Terms ........................ 7 Customer Service ....................... 8 Product Safety and Electromagnetic Compatibility ............. 8 Safety.............................. 9 System Owner's Responsibility................... 9 Personnel Requirements .................... 10 3.2.1 Qualifications ........................ 10...
  • Page 4 Contents Operating States of the iProbe.................. 28 ATMA .......................... 29 Properties of the iProbe .................... 30 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 Specific iProbe HR-MAS Hardware and Operations............ 36 7.6.1 MAS Unit........................... 36 7.6.2...
  • Page 5: About This Manual

    About This Manual 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.
  • Page 6 About This Manual NOTICE NOTICE indicates a property damage message. This is the consequence of not following the notice. 1. This is a safety condition. u This is a safety instruction. SAFETY INSTRUCTIONS SAFETY INSTRUCTIONS are used for control flow and shutdowns in the event of an error or emergency.
  • Page 7: Introduction

    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. Limitation of Liability...
  • Page 8: Customer Service

    Introduction 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.
  • Page 9: Safety

    Safety Safety 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.
  • Page 10: Personnel Requirements

    • The system owner must ensure that all (electrical, mechanical, etc.) safety devices are regularly checked to ensure full safety functionality and completeness. Personnel Requirements Only trained Bruker personnel are allowed to initially install, retrofit, repair, adjust and dismantle the unit! 3.2.1...
  • Page 11: Unauthorized Persons

    Safety 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.
  • Page 12: Dangers From Magnetic Fields

    Safety 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. u Never cover the flush gas supply by hand.
  • Page 13: Dangers Due To High Temperatures

    Safety 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. u Check the probe temperature in TopSpin. u Put on gloves before handling the probe. 3.4.4 Danger from Chemical Substances WARNING...
  • Page 14: Environmental Protection

    Material damage may result when the device comes in contact with NMR solvents. u Follow instructions provided in the manual for correct handling of solvents. u If surface damage occurs, contact Bruker for repair of damaged parts. Environmental Protection NOTICE...
  • Page 15: 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. Symbols on the Packaging The following symbols are affixed to the packaging material.
  • Page 16: Packaging

    Transport, Packaging and Storage 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.
  • Page 17: Design And Function

    Design and Function 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.
  • Page 18: Brief Description

    Design and Function Figure 5.2: Diagram of a setup with iProbe HR-MAS 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.
  • Page 19: Connections Iprobe Hr-Liquids

    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.
  • Page 20: Connections At The Rear Side Of Iprobes

    Design and Function 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...
  • Page 21: Installation

    Bruker Service or personnel authorized by Bruker. Damage due to servicing that is not authorized by Bruker is not covered by your warranty. Prior to installing the iProbe, the quick-lock needs to be mounted on the magnet. Please refer to the following instructions.
  • Page 22 Installation Installation • There are 3 pairs of equal threads arranged opposite to each other in the red bottom plate of the SB shim system as marked with the arrows (1). The quick-lock has to be mounted on one of these pairs with the fastening screws (M3 x 13).
  • Page 23: Iprobe Mounting With Quick-Lock

    Installation iProbe Mounting with Quick-Lock Overview Figure 6.3: iProbe Transport box Sample gauge (HR Liquids only) Gradient adapter cable Quick-lock iProbe Accessory for HRMAS CAUTION Risk of injury and property damage due to incorrect handling of the iProbe. u Do not hold the iProbe by its tube. Always hold it by its body. u Never touch the pins of the connectors and plugs.
  • Page 24: Installation Of Iprobe Hr-Liquids

    (also male connector). • Connect the gradient (1), the flush gas (2), the BFB-cable (3) (Bruker Field Bus coming from the BVT) and the RF-cables (4). • Read the iProbe Instructions (P/N Z156810) about the Flush Gas Supply use and requirements.
  • Page 25: Installation Of Iprobe Hr-Mas

    Installation The installation of the iProbe HR-Liquids is complete and the iProbe HR-Liquids can be detected by the software with the command edprobe. 6.2.2 Installation of iProbe HR-MAS NOTICE In the iProbe HR-MAS the bearing gas has two functions: supporting the rotor for spinning and regulating its temperature.
  • Page 26 • Connect the gradient (1), drive (2), eject (3), spinning rate (4), the flush gas (5), the BFB-cable (6) (Bruker Field Bus coming from the BVT) and the RF-cables (7). • At the rear side of the MAS III unit, connect the drive, eject, the flush gas pipes and the spin rate cable.
  • Page 27: Operation

    Operation Operation General Operating Guidelines There are several general rules and procedures that should be observed while operating the device. Warranty Limitations & Probe Instructions NOTICE Material damage hazard due to improper handling u Follow the warranty limitations and probe instruction (Z156810) given for the probe carefully to achieve optimal performance and maximum lifetime of the probe.
  • Page 28: Operating States Of The Iprobe

    Operation Operating States of the iProbe The meaning of the LED states and state types are listed below. The user should know them in order to operate the system correctly and safely. Figure 7.1: On the front of the iProbe shows an LED (1) the current status of the probe State Meaning Fast blinking green...
  • Page 29: Atma

    Operation ATMA ATMA for the iProbe The ATMA unit is integrated in the iProbe, therefore no extra unit has to be installed. ATMA - Automatic Tuning & Matching The iProbe can only be operated with ATMA/2, which is already integrated in AvanceNEO spectrometers.
  • Page 30: Properties Of The Iprobe

    Operation Properties of the iProbe To view the properties of the installed probe within TopSpin , type edprobe on the command line. • Select the desired probe (if not automatically detected). • Click on View Properties under the Manage menu on the top bar of the Edprobe window.
  • Page 31 Operation Figure 7.3: TopSpin Properties of probe window for another probe type. • Depending on the probe the relevant parameters are presented. Further details can be seen when opening the different categories. • Under Probe Identity the type of probe, part number and serial number are given. Figure 7.4: TopSpin Probe Identity window •...
  • Page 32 Operation Figure 7.5: TopSpin Product Info window • Information regarding the gradient system are provided under Gradient System Parameters window. Figure 7.6: TopSpin Gradient System Parameters window NOTICE! Never exceed the maximum permissible current. Figure 7.7: TopSpin Parameter of the Z Gradient System window •...
  • Page 33 Operation Figure 7.9: TopSpin Temperature Controlling Gas Flow window • MAS related parameters are listed is the MAS Parameters submenu. Figure 7.10: TopSpin MAS Parameters window • The coil parameters for an iProbe with one coil are listed as shown in Figure 7.11 [} 33] Figure 7.11: TopSpin Coil Parameters window •...
  • Page 34 Operation Figure 7.13: TopSpin Sample Parameters window provides the specific parameters of the sample, e.g. liquid sample. • The Sample Parameters window provides only the rotor diameter for iProbe HR-MAS. Figure 7.14: TopSpin Sample Parameter window provides the specific parameters of the sample, e.g. HR-MAS sample •...
  • Page 35: Sample Carrier And Nmr Tubes For Hr-Liquids

    Spinner SB CERAMICS 5mm TYP: A (H00804A). Spinner SB PLA (POM) 5+2,5 -A (Z42516A) with black marking inside. Table 7.2: Allowed Spinner Types with Yellow Rings Further information about available samples can be found under https://store.bruker- biospin.com/. Z33146_1_001 35 / 56...
  • Page 36: Glass Tubes

    Operation 7.5.1 Glass Tubes NOTICE Material damage of glass tubes u NMR tubes should always be handled carefully. In some rare cases they may break even without any force or impact e.g. when inserting an NMR glass tube into the iProbe. 7.5.1.1 Sample Depth and Filling Height The values of sample depth and filling height are defined in PICS which is accessible via...
  • Page 37: Transfer System

    Operation The stator is driven by an electromotor which allows to flip between eject and insert position. The movements from eject to insert and back last several seconds. The same motor is also responsible for the fine adjustment of the magic angle. The adjustment is done from the Magic Angle tab of the TopSpin MAS user interface shown in Figure 7.17 [} ...
  • Page 38: Variable Temperature Unit (Vtu)

    Operation 7.6.3 Variable Temperature Unit (VTU) Since the MAS unit regulates the gas flow of the bearing gas, the VTU will only regulate the temperature but not the flow. Therefore, the VTU must be configured to external gas flow control in the Temperature Control Suite (VTU user interface) as highlighted in Figure 7.19 [} 38].
  • Page 39: Mounting Angle

    Operation laboratory frame shims (Z, X, Y, etc.) is necessary. This linear combination is mathematically expressed by a matrix that represents the change of reference frame from the magic angle frame with the Z' axis parallel to the rotational axis, to the laboratory frame, with the Z axis parallel to the main magnetic field.
  • Page 40 Operation Mounting position of the Resulting angle φ1 for Resulting angle φ2 for iProbe for TopShim is TopShim in a Boss2/3-SB TopShim in a Boss1-SB dependent on the shim shim system shim system system (see Figure 7.22 [} 40]) 340 ° (standard installation) 340 °...
  • Page 41: Shimming In The Topshim Manual Mode

    Operation Figure 7.23: Standard Bore (SB) Shim System – View from Bottom a Projection of the φ1 Angle between X-axis Boss2/3 shim system and laboratory frame’s Z’-axis projection of laboratory frame’s Z’-axis b X-axis Boss2/3 shim φ2 Angle between X-axis Boss1 shim system and system projection of laboratory frame’s Z’-axis c X-axis Boss1 shim...
  • Page 42 Operation Figure 7.25: TopShim window to select the corresponding laboratory frame mas shim gradients Z’, Z2’, Z3’, and Z4’. • Continue to optimize the Z1’ – Z4’ shims by looking at the lock signal and also at the line shape. • Once the iProbe has successfully passed the initial shimming, this shim file can be used as a base for all other samples.
  • Page 43: Maintenance

    8.1.3 Other Cleaning Operations For all other cleaning operations contact Bruker service for advice and support. It may be necessary to return the device for a cleaning service. The device is not protected from contamination in case of leaking samples. Bruker accepts no responsibility for any damage which may occur when samples containing radioactive or other hazardous materials are used.
  • Page 44 Maintenance 44 / 56 Z33146_1_001...
  • Page 45: Troubleshooting

    Problem with iProbe in TopSpin • If a problem with TopSpin occurs during the iProbe installation, use the command savelogs to collect information about the installation setup and send it to your local Bruker support. Figure 9.1: TopSpin savelogs command...
  • Page 46 Troubleshooting 46 / 56 Z33146_1_001...
  • Page 47: 10 Replacement Of Parts

    10.1 Returning the Unit for Repair If the Bruker Hotline diagnoses an instrument failure that requires a part to be returned for repair, please follow the procedure listed here: 1. Contact your local Bruker office to start the repair process (see Contact). Repair is always handled by your local Bruker office.
  • Page 48 Replacement of Parts 48 / 56 Z33146_1_001...
  • Page 49: 11 Dismantling And Disposal

    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. 11.1...
  • Page 50: Disposal Usa And Other Countries

    Only 100% pre-decontaminated equipment can and will be accepted by Bruker BioSpin. A release document for decontamination can be inquired from your nearest Bruker BioSpin contact site, also to be used when repairs, going back to Bruker sites, are requested. In compliance with WEEE II directive: 2012/19/EU 11.3...
  • Page 51: 12 Technical Data

    Decreasing linear til relative humidity < 50 % at 40 °C, maximum Table 12.2: Operating Environment For the appropriate temperature see also the Bruker site planning guides on the BASH CD (Bruker Advanced Service Handbook): Manual Bruker Part Number Site Planning for AVANCE Systems...
  • Page 52: Iprobe Type Plate

    Technical Data 12.3 iProbe Type Plate The type plate is located on the iProbe and includes the following information: Figure 12.1: iProbe Type Plate Type Temperature range Manufacturer logo CE Symbol Sample type to use with the iProbe Manufacturer address Channels Part number / ECL: Engineering Change Level / Serial number Length type of the Probe...
  • Page 53: 13 Contact

    Contact 13 Contact NMR Hotlines Bruker Corporation provides dedicated hotlines and service centers. Please select the NMR service center or hotline you wish to contact from our list available at: https://www.bruker.com/service/information-communication/helpdesk.html Contact our NMR service centers, so that our specialists can respond as quickly as possible to all your service requests, application questions, software or technical needs.
  • Page 54 Contact 54 / 56 Z33146_1_001...
  • Page 55 Z33146_1_001 55 / 56...
  • Page 56 ● Bruker Corporation info@bruker.com www.bruker.com Order No: Z33146...

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