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Bruker NMR iProbe HR-Liquids User Manual Download Page 31

Operation

Z33146_1_001

31 / 56

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

• Further information is listed under 

Product Info

.

Summary of Contents for NMR iProbe HR-Liquids

Page 1: ...iProbes HR Liquids HR MAS User Manual Version 001 Innovation with Integrity NMR ...

Page 2: ...emarks 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 41 44 825 97 97 E mail cryoprobe serv...

Page 3: ...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 Connecti...

Page 4: ...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 Dis...

Page 5: ...bols 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 th...

Page 6: ...ty 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 u This is a safety instruction This symbol highlights useful tips and recommendations as well as information designed to ensure efficient and smooth operation ...

Page 7: ...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 t...

Page 8: ...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 ...

Page 9: ...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 interv...

Page 10: ...at 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 ...

Page 11: ...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...

Page 12: ...s 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 u Mark the magnetic field of more than 0 5 mT 5 Gauss before start up u Keep people with active medical implants or heart pacemakers away from the 0 ...

Page 13: ...samples if necessary u Strictly observe the correct sample adjustment i e the maximal sample depth u Always transport the glassware or ceramics with the cover if applicable Never turn the glassware or ceramics upside down or on its side u The laboratory supervisor is responsible for ð Establishing and enforcing standard sample handling and cleaning procedures ð Establishing and enforcing the use o...

Page 14: ... pollutants particularly incorrect waste disposal may cause serious damage to the environment u Always observe local environmental regulations regarding handling and disposal of pollutants u Take 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 t...

Page 15: ...ge 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 follo...

Page 16: ...e 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 sunlig...

Page 17: ...frastructure 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 an...

Page 18: ... 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 ...

Page 19: ...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...

Page 20: ...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 ...

Page 21: ...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 6 1 Quick Lock Mounting Overview Figure 6 1 iProbe installed in the magnet Figure 6 2 Quick lock a Bottom view b Top view of the iProbe 1 Fastening screws M3 x 13 3 Clip holders of the iProbe within the foreseen holes in...

Page 22: ...e The two holes for the clip holders 1 of the adapter determine the orientation of the iProbe The orientation of the iProbe has to be set in order to attain an easy access to the VT gas hose In standard installations the front of the iProbe is oriented towards the left when facing the front of the magnet The lever can be positioned to the right or the left side depending on your preference Mount t...

Page 23: ...rt box 1 Sample gauge HR Liquids only 4 Gradient adapter cable 2 Quick lock 5 iProbe 3 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: ...robe HR Liquids in the position using the quick lock lever Connections at the rear side Remove the white plastic cover and connect the Johnston connector of the VT gas hose or the BCU to the rear side of the iProbe HR Liquids Mount the support clamp Z53660 on the magnet as shown in the photo Position and support the transfer line using the Velcro tape of the support clamp Connections at the front ...

Page 25: ...t of the shim system according to the Quick Lock Mounting Instruction Z166745 Take the iProbe HR MAS out of the transport box and remove the protection cap Check that the quick lock lever is in the unlock position Slide the iProbe HR MAS into the magnet Mount the iProbe so that the clip holders 1 on the iProbe body fit exactly the holes for the clip holders in the quick lock so that the iProbe is ...

Page 26: ...esponding connectors on the MAS III are labeled accordingly The Bearing gas line must be connected to the Main VT gas line 1 using a T piece 2 Finally the output of Bearing should branch off to Bearing Sens with another T piece according to Figure 5 2 18 The other end of the Main VT gas line is connected to Main VT GAS on the rear side of the AvanceNEO console The installation of the iProbe HR MAS...

Page 27: ...for the probe carefully to achieve optimal performance and maximum lifetime of the probe u Always turn ON power check u Never exceed the maximum power level for short pulses as defined in PICS u Never exceed the maximum sample depth Temperature Changes NOTICE Material damage hazard due to significantly temperature changes When the ambient temperature changes significantly for example after moving ...

Page 28: ...d by the system Slow blinking green Initialization The probe has been recognized by the system and it is in the initialization phase Slow blinking yellow Thermal regulation preparation The probe will be prepared for thermal regulation Slow changes yellow green Standby The thermal regulation is in standby mode Constant yellow Thermal regulation The thermal regulation is running Blinking Red Thermal...

Page 29: ...e the commands edprobe and ii before using atma The next atma command can be executed by simply typing atma Successful tuning and matching parameter will be saved automatically ATMM Manual Tuning Matching The tuning and matching can be done by hand or via algorithms To save the result of a manual tuning and matching process an algorithm in ATMM must be started ATMM saves the channel core combinati...

Page 30: ...e Select the desired probe if not automatically detected Click on View Properties under the Manage menu on the top bar of the Edprobe window The properties of the probe are shown for the installed probe Figure 7 2 Window showing the properties of the selected probe The shown properties in Figure 7 2 30 and Figure 7 3 31 vary depending on the probe type ...

Page 31: ...e 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 Further information is listed under Product Info ...

Page 32: ...t System Parameters window NOTICE Never exceed the maximum permissible current Figure 7 7 TopSpin Parameter of the Z Gradient System window The Temperature Parameters of the probe can be found in the corresponding window Figure 7 8 TopSpin Temperature Parameters window The recommended and range for the gas flow controlling the temperature settings can be checked within the related submenu ...

Page 33: ...re 7 11 33 Figure 7 11 TopSpin Coil Parameters window The nuclei of each coil can be viewed in the window Parameters of Coil Figure 7 12 TopSpin Parameter of Coil window The TopSpin Sample Parameters window for liquid samples show important information about the sample depth below the magnetic center or the sample filling height see Figure 7 13 34 It is also possible to read this info by using edp...

Page 34: ... TopSpin Sample Parameter window provides the specific parameters of the sample e g HR MAS sample The peak power of the iProbe can be checked under the related submenu NOTICE Never use higher power settings than the given values and use the peak power only for short pulses otherwise the iProbe can be damaged Switch power check on in order to automatically limit the peak power to these values Figur...

Page 35: ...sample certificate to get information about the approved temperature range for your sample u Consult the Manual NMR Probes Variable Temperature Control for NMR Probes Z33073 Chapter 3 Table 3 4 to get the information about the approved temperature range of spinners and shuttles Spinner SB PLA PCTFE 5 2 5 A H00177A with black marking inside Spinner SB CERAMICS 5mm TYP A H00804A Spinner SB PLA POM 5...

Page 36: ...r 7 6 Specific iProbe HR MAS Hardware and Operations NOTICE Material damage hazard due to improper handling of rotors It is important that the rotors are correctly filled with the samples and that the rotor caps and the marker are in good condition Otherwise the spinning can become unstable or the rotor could crash Never exceed the temperature ranges and the allowed spinning rate of the rotor cap ...

Page 37: ... shown in Figure 7 17 37 It is offered in two modes an automatic and a manual adjustment The automatic adjustment lasts typically several minutes The side band used for automatic Magic Angle adjustment can be selected in the Configuration tab Figure 7 17 The MAS Angle tab of the TopSpin MAS user interface 7 6 2 Transfer System For manual sample insertion and ejection the modular transfer line H169...

Page 38: ...s Never exceed the allowed maximum current given in the TopSpin Gradient System Parameters window Figure 7 20 TopSpin Gradient System Parameters 7 6 5 Tuning Matching Tuning Matching of each channel is done with the atma or atmm command see also ATMA 29 Note that in order to see the wobble curve the stator must be in the insert position 7 6 6 Shimming In HR MAS spectroscopy the rotor axis is orien...

Page 39: ...o distribute the currents among several shim coils minimizing the risk of overcurrent on a single shim coil To build the matrix transformation correctly TopShim requires the input of the mounting angle of the probe i e the orientation of the probe in the shim system Please refer to section Table 7 3 40 for more details Currently TopShim offers only the manual mode for shimming in the laboratory fr...

Page 40: ... 190 190 250 160 160 220 130 130 190 100 100 160 70 70 130 40 40 100 10 10 70 Table 7 3 Conversion of the mounting angle needed for TopShim dependent on the SB shim system type for various mounting angles Figure 7 22 Standard Bore SB Shim System a Projection of the laboratory frame s Z axis φ1 Angle between X axis Boss2 3 shim system and projection of laboratory frame s Z axis b X axis Boss2 3 shi...

Page 41: ...itial shimming The sample must be rotating at a reasonable spinning rate Set all shim values to 0 BSMS panel or using setsh in TopSpin Load the corresponding lock solvent with lopo The lock should now be in sweep mode and the lock wiggles should be visible Otherwise adapt Field and Gain accordingly However the lock wiggles will probably be too broad for locking Run topshim changemasshims and set t...

Page 42: ... 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 In most cases only the Z and Z2 will then need an adjustment ...

Page 43: ... 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 In case of an accident ...

Page 44: ...Maintenance 44 56 Z33146_1_001 ...

Page 45: ...ll no dip in the wobble curve the correct routing of the current experiment should be checked with the command edasp 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 9 1 Specific for iProbes HR MAS Po...

Page 46: ...Troubleshooting 46 56 Z33146_1_001 ...

Page 47: ...ping address and also in most cases a Return Merchandise Authorization number RMA number that allows references to the repair case Always refer to this RMA number in case of questions 3 Send the defective part to the local Bruker office and include the following documents RMA sheet if RMA number was assigned Signed Equipment Clearance Form BBIOF002 H152631 The Equipment Clearance Form will be sent...

Page 48: ...Replacement of Parts 48 56 Z33146_1_001 ...

Page 49: ... 6 clause 3 of the German Act ElectroG To meet the demands of the European Directive 2012 19 EU WEEE 2 Waste of Electrical and Electronic Equipment and the national Equipment Safety Act electrical and electronic equipment that is marked with this symbol directly on or with the equipment and or its packaging must not be disposed of together with unsorted municipal waste or at local municipal waste ...

Page 50: ...ust be affirmed when the equipment is ordered from Bruker BioSpin Additional costs for dismantling and transport service will apply 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 wi...

Page 51: ...en gas only Use the Supply Kit P N Z111126 to couple the gas source with the Flush gas connector on the iProbe 12 2 Environmental Conditions Environment Data Value Unit Temperature range C Relative humidity at 31 C maximum 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 ...

Page 52: ...e and includes the following information Figure 12 1 iProbe Type Plate 1 Type 6 Temperature range 2 Manufacturer logo 7 CE Symbol 3 Sample type to use with the iProbe 8 Manufacturer address 4 Channels 9 Part number ECL Engineering Change Level Serial number 5 Length type of the Probe 10 Gradient ...

Page 53: ...oSpin AG BRUKER Instruments Inc Industriestrasse 26 44 Manning Road CH 8117 Fällanden Billerica MA 01821 Switzerland U S A phone 41 44 825 91 11 phone 1 978 667 9580 fax 1 978 667 0985 email info bbio ch bruker com email sales bbio ch bruker com email sales bbio us bruker com http www bruker com http www bruker com CryoProbe Service BRUKER BioSpin AG BRUKER Instruments Inc Service Department Indus...

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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