Bruker EPR 12T Cryogen Free User Manual
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Bruker EPR 12T Cryogen Free User Manual

Bruker EPR 12T Cryogen Free User Manual

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EPR 12T
Cryogen Free
User Manual
Version
01
EPR Spectroscopy
Innovation with Integrity

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Summary of Contents for Bruker EPR 12T Cryogen Free

  • Page 1 EPR 12T Cryogen Free User Manual Version EPR Spectroscopy Innovation with Integrity...
  • Page 2 ZTKS0213 / Z31939 / Rev.: 01 For further technical assistance on the EPR 12T Cryogen Free Cryogen Free magnet system, please do not hesitate to contact your nearest BRUKER dealer or contact us directly at: BRUKER BioSpin GmbH Silberstreifen 4 D–76287 Rheinstetten...

  • Page 3: Table Of Contents

    Mounting the Vacuum Valve at the Evacuated Cryostat ........29 5.2.3 Rebuilding Vacuum ................... 31 5.2.4 Removing the Vacuum Valve ................32 Bruker Cryogen Free Controller (BCFC) ..............33 Power Supply ......................36 5.4.1 Description ......................36 5.4.2 First Steps ......................37...
  • Page 4 Contents Cooling Down ......................39 Operation of the BCFC ................... 40 5.6.1 Compressor Status Check ................40 5.6.2 Emergency Button Test..................41 5.6.3 Energizing the Magnet ..................42 5.6.4 Emergency Quench................... 43 5.6.5 Warming up the Magnet ..................44 Power Supply Operation..................45 5.7.1 Selecting the Operation Mode................

  • Page 5: Contact

    Contact Manufacturer Bruker BioSpin GmbH Silberstreifen 4 D-76287 Rheinstetten Germany Phone: +49 721 5161 0 Fax: +49 721 5171 01 Email: epr@bruker-biospin.de http://www.bruker.com Please refer to the model no., serial no. and internal order no. in all correspondence regarding the EPR magnet system or components thereof.
  • Page 6 Contact ZTKS0213 / Z31939 / Rev.: 01...

  • Page 7: Introduction

    Introduction General Information This manual contains important information about the handling of the magnet system. The compliance with all safety and handling instructions and the applicable local accident prevention and general safety regulations is necessary for safe work. This manual is part of the product. It must be kept in the vicinity of the magnet system and unimpeded access must be ensured at any time.

  • Page 8: Customer Service

    Technical support is provided by our customer service via telephone or e-mail. For contact information see page 5 of this document. General View (1) EPR 12T Cryogen Free Magnet System (2) Bruker Cryogen Free Controller (BCFC) (3) Power Supply E700-1083...

  • Page 9: Safety

    (including all necessary knowledge of applicable regulations and regulatory requirements) to perform specific tasks on the magnet system and its components. Bruker Service Personnel are qualified to identify possible hazards and risks and to perform all possible steps to eliminate or minimize these risks.

  • Page 10: Customer Responsibilities

    Safety Customer Responsibilities The customer must obey the security advice and the rules for safety, accident prevention and environmental protection valid for magnet systems. Furthermore, the customer is responsible for keeping the magnet system in correct technical condition. In particular: •...

  • Page 11: Symbols And Convention

    Safety Symbols and Convention Safety instructions in this manual 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.

  • Page 12: Persons

    Work must only be carried out by approved persons with applicable qualifications. The necessary qualifications are specified at the beginning of the relevant chapters. • In case of doubt contact Bruker Service. Contact information see page 5 of this document.

  • Page 13: Residual Risks

    Safety Residual Risks In the following section, the residual risks from the risk analysis are summarized. To prevent health hazards and hazardous situations obey all safety instructions and warnings in the manual. Electricity 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.

  • Page 14: Inserting And Removing The Vti

    Metallic items in close vicinity of the magnet system get attracted from strong magnetic forces during a magnet quench. Thus: • Insert or remove the VTI and/or the sample holder only at zero field. • Only use VTIs and/or sample holders approved by Bruker Service. ZTKS0213 / Z31939 / Rev.: 01...

  • Page 15: Risk Of Injury Due To Gas Under Pressure

    Safety Gas under Pressure WARNING Risk of injury due to gas under pressure inside the cryostat and further equipment. Manipulations of components with gas under pressure may lead to injury and property damage. Thus: • Keep the Cryogenic Refrigerator circuit closed at any time. Overpressure can be released via the safety valve of the compressor, of the rotary valve and of the cold head.
  • Page 16 Safety Transportation CAUTION Risk of injury and property damage due to incorrect transportation. The box may tilt, movement may get out of control. Thus persons may get injured and the cryostat or further equipment may be damaged. Thus: • Be careful while unloading and moving the boxes. •...

  • Page 17: Signs And Labels

    • Replace damaged or not readable signs and labels immediately. New signs and labels can be obtained from Bruker Service. Signs and labels are always related to their immediate vicinity. The following signs and labels are found on the magnet system and in the vicinity: Prohibition sign: No person with pacemakers! People with pacemakers are endangered in the identified area of 0.5 mT (5 Gauss) and...
  • Page 18 Safety Hazard warning sign: Strong magnetic field! • No magnetic storage devices. • No jewelry. • No metallic items. Emergency exit! • Always keep the emergency exit clear. • Follow the arrows if necessary. • Emergency exit doors must open in direction of escape. ZTKS0213 / Z31939 / Rev.: 01...

  • Page 19: Safety Devices

    Safety Safety Devices WARNING Risk of damage to life and limb due to not sufficient safety devices. Several safety devices and safety valves ensure safe operation. They must always be in correct working condition. Thus: • Do not block safety devices. •...

  • Page 20: Behavior During Dangerous And Emergency Situations

    Safety Behavior During Dangerous and Emergency Situations Preparations • Keep the emergency exits free at any time. • Prepare and maintain an up-to-date list of emergency telephone numbers in the magnet system area. In Case of Emergency • Leave the danger zone immediately. •...

  • Page 21: Transportation

    Transportation The transportation is carried out by Bruker Service or by approved persons. However, it may happen that not approved persons have to take the delivery of the transport boxes. In this case the customer has to inform these persons about requirements for transpor- tation given in this chapter.

  • Page 22: Packaging

    Transportation Packaging The magnet system is packed in a transport box. It is secured inside with tightening straps against tilting and moving. Accessories such as cryogenic refrigerator parts and flex lines are packed in separate transport boxes. For handling of the cryogenic refrigerator parts refer to the supplied manuals (see "Further Appli- cable Documentation"...

  • Page 23: Transportation By Forklift / Pallet Jack

    Transportation The claim for damage expires after the fixed period. Thus: Report damages to Bruker Service immediately after detection. For contact information page 5 of this document. Transportation by Forklift / Pallet Jack Persons in charge • Approved forklift / pallet jack operator Precondition •...

  • Page 24: Storage

    Transportation Transport Check the route of transport for the minimum height and width. Check sufficient floor capacity on the route of transport. In case of doubt ask a stress analyst. Check sufficient carrying capacity while using an elevator. Position the forks between the bars of the transport box as shown in the figure.

  • Page 25: Assembling

    Assembling Approved persons: Bruker Service only ZTKS0213 / Z31939 / Rev.: 01...
  • Page 26 Assembling ZTKS0213 / Z31939 / Rev.: 01...

  • Page 27: Operation

    Operation Safety WARNING Magnetic Field (see page Electricity (see page Safety Devices (see page ZTKS0213 / Z31939 / Rev.: 01...

  • Page 28: Evacuating The Cryostat

    Operation Evacuating the Cryostat A turbomolecular pump (pumping speed ≥ 80 l/s N ) is required to evacuate the cryostat. Do not use a diffusion pump. 5.2.1 General View The vacuum valve (Material No. Z53420) is necessary to evacuate the vacuum chamber of the cryostat after assembling the magnet system.

  • Page 29: Mounting The Vacuum Valve At The Evacuated Cryostat

    Operation 1 Cryocooler noise protection hood 2 Vacuum valve 3 Top plate 4 Pumping line Figure 5.2: Vacuum valve mounted at the magnet system 5.2.2 Mounting the Vacuum Valve at the Evacuated Cryostat Precondition • Magnet system deenergized. • Magnet system at 300 K. Procedure Remove the earthing cable (1).
  • Page 30 Operation Install the valve stem (6) onto the sealing plug (2) and tighten it slightly. Do not yet fix the valve operator body (5) to the cryostat. NOTICE: The sealing plug can not be moved until a correct vacuum was applied at the KF 40 flange of the vacuum valve.

  • Page 31: Rebuilding Vacuum

    Operation 5.2.3 Rebuilding Vacuum Precondition • Vacuum valve mounted. Procedure Use the KF connector to connect the vacuum pumping unit with the KF 40 flange (5) of the vacuum valve (2). Use a short pumping line with a large diameter. Evacuate the vacuum valve and the pumping line to a pressure of better than 5 x 10...

  • Page 32: Removing The Vacuum Valve

    Operation 5.2.4 Removing the Vacuum Valve Vent the pumping line. Remove the pumping line at the KF 40 flange (7). Release the valve stem (6) from the sealing plug (2) and pull out the valve stem. Remove the four M6 x 12 screws (4) from the half rings (3).

  • Page 33: Bruker Cryogen Free Controller (Bcfc)

    Operation Bruker Cryogen Free Controller (BCFC) The functionality of the Bruker Cryogen Free Controller (BCFC) is described from the left to the right on the front panel (see Figure 5.8). 1. Remote compressor status display. 2. Warming up the magnet system.
  • Page 34 Operation To activate the heater the following conditions have to be met: The magnet system must be deenergized. If the magnet is energized, the heater cannot be activated, and the indicator remains inactive ("OFF"). The magnet must be below ambient temperature (300 K). While the magnet is at ambient temperature the heater and the indicator remain inactive.
  • Page 35 Operation Figure 5.9: Bruker Cryogen Free Controller (BCFC) – Rear View • The green indicator (1, "ARMED") is active while the "MAGNET QUENCH" button is in stand by mode. It should always be active ("ON"), otherwise the magnet quench safety functionality is not available.

  • Page 36: Power Supply

    Persons in charge • Approved customer personnel, Bruker Service Precondition • After system cool down the magnet must be kept below 3.5 K for at least 4 hours before the energizing procedure can be started.

  • Page 37: First Steps

    In the "DISPLAY CERNOX" mode the measured Cernox temperatures of the main coil are displayed. The "DISPLAY Shim" mode is not relevant for the EPR 12T Cryogen Free magnet as cryo-shims are not implemented. ZTKS0213 / Z31939 / Rev.: 01...
  • Page 38 Operation • Set the current rate and the voltage rate of the main coil (refer to "Magnet Parame- ters" on page 70): Set the maximum current rate according to "Magnet Parameters" on page 70 while the magnet system is in main mode. Press "RATE".

  • Page 39: Cooling Down

    Operation Cooling Down Precondition • Magnet system is evacuated to a vacuum of better than 1 x 10 mbar at room tem- perature(see section "Evacuating the Cryostat" on page 28). • Vacuum pump still running. • Power supply operation Cernox mode. •...

  • Page 40: Operation Of The Bcfc

    Operation • The compressor status is displayed on the BCFC (see "Remote Compressor Status Display" on page 33). The four indicators of the compressor (temperature okay, gas pressure okay, input power, running) must be active (green). • Use the "DISPLAY CERNOX" mode of the power supply to monitor the temperature of the main coil.

  • Page 41: Emergency Button Test

    Operation 5.6.2 Emergency Button Test The functionality of the emergency button "MAGNET QUENCH" must be checked on a regular basis (at zero field!). Precondition • Compressor status checked. • Compressor running. • Magnet system cooled down as described in section "Cooling Down"...

  • Page 42: Energizing The Magnet

    Operation 5.6.3 Energizing the Magnet Precondition • Magnet system at base temperature (less than 3.5 K). • All green indicators on the front panel of the BCFC "ON". • Safety check passed. Figure 5.16: Energizing the magnet and checking the indicator Procedure Energize the magnet according to section "Energizing and Deenergizing in Main Mode"...

  • Page 43: Emergency Quench

    Operation 5.6.4 Emergency Quench Precondition • "HIGH MAGNETIC FIELD" indicator is ON; • Indicator "ARMED" is ON. Procedure Push the magnet quench button. Check that the rhythmic noise of the compressor stops and the red indicator ("TRIGGERED") is ON. Wait until the magnetic field indicator is turned OFF. It can take up to a few minutes until the magnetic fringe field has disappeared after pushing the emergency button "MAGNET QUENCH".

  • Page 44: Warming Up The Magnet

    Operation 5.6.5 Warming up the Magnet Precondition • Magnet deenergized (refer to "Energizing and Deenergizing in Main Mode" on page • Magnet cold (below 300 K) Procedure Turn off the compressor (see Figure 5.12 on page 39 Figure 5.13 on page 40).

  • Page 45: Power Supply Operation

    Operation Power Supply Operation 5.7.1 Selecting the Operation Mode Select the Sweep Mode: • The current in the current leads has to be zero. • Press "SWEEP MODE". • Press "SET". Select the Main Mode: • The current in the current leads has to be zero. •...
  • Page 46 Operation • Define the maximum voltage for the energizing/deenergizing procedure: 1. Press "VLT" 2. Enter <Max. Voltage in Volts> 3. Press "SET" to validate the entry. The value "Max. Voltage in Volts" cannot exceed the value "U main level" defined in "Power Supply Parameters"...

  • Page 47: Energizing And Deenergizing In Sweep Mode

    Operation 5.7.3 Energizing and Deenergizing in Sweep Mode Calculate the current required in the sweep coil current to achieve the desired field change by multiplying the field with the ratio "Sweep Current / Magnetic Field" in "Mag- net Parameters" on page Perform the following steps to change the field in the sweep coil: •...
  • Page 48 Operation ZTKS0213 / Z31939 / Rev.: 01...

  • Page 49: Troubleshooting

    Troubleshooting In case of doubts or problems not specified in the following list contact Bruker Service immediately (see page 5 of this document for contact information). Safety WARNING Magnetic Fields (see page Gas under Pressure (see page Power Supply (see...

  • Page 50: Problems

    The following table gives a summary of problems which may require troubleshooting action to be carried out either by approved customer personnel or by Bruker Service. Possible reasons indicated in the list of problems refer to solution keys and detailed description of solutions listed in Table 6.2...

  • Page 51: Solutions

    Press "RES" to reset the power supply. Additional information: For the EPR 12T Cryogen Free system the interlocks based on the magnet temper- ature are not in use. Therefore the threshold values have been set to 300 K (see section "Power Supply Parameters"...
  • Page 52 Cool down the magnet to base temperature (indicated on the power supply). Read and write down the base temperature (see "Base Temperature Report (Monthly)" on page 74). Send all information from the base temperature report to Bruker Service. Deenergize the magnet. Activate the warm-up switch. none Replace UPS battery.

  • Page 53: Maintenance

    Approved customer "MAGNET QUENCH" at zero personnel field Replace cold head every 10 000 hours Bruker Service for refurbishment of sliding parts of the cold head Replace compressor adsorber every 20 000 hours Bruker Service UPS battery replacement every 4 –...
  • Page 54 Maintenance ZTKS0213 / Z31939 / Rev.: 01...

  • Page 55: Disassembling

    Disassembling Approved persons: Bruker Service only ZTKS0213 / Z31939 / Rev.: 01...
  • Page 56 Disassembling ZTKS0213 / Z31939 / Rev.: 01...

  • Page 57: A Appendix

    Appendix Warning Signs Danger Key Word and Symbol .................. 11 Warning Not approved persons ................... 12 Not readable signs and labels ............... 17 Blocked safety devices .................. 19 Electricity, high voltage ................. 13 High magnetic fields ..................13 Incorrect use of the magnet system .............. 12 Inserting and removing the VTI ..............
  • Page 58 Warning Signs ZTKS0213 / Z31939 / Rev.: 01...

  • Page 59: Figures

    Removing the vacuum valve..............32 Figure 5.7: Mounting the earthing cable..............32 Figure 5.8: Bruker Cryogen Free Controller (BCFC) – Front View ......33 Figure 5.9: Bruker Cryogen Free Controller (BCFC) – Rear View ......35 Figure 5.10: Magnet quench indicators on the BCFC front panel ......35 Figure 5.11:...
  • Page 60 List of Figures ZTKS0213 / Z31939 / Rev.: 01...

  • Page 61: Tables

    Tables Table 6.1: Troubleshooting table................50 Table 6.2: Solution keys (part 1) ................51 Table 6.3: Solution keys (part 2) ................52 Table 7.1: Maintenance schedule of the EPR 12T magnet system ..... 53 Table A.1: Glossary....................63 Table A.2: Abbreviations ..................
  • Page 62 List of Tables ZTKS0213 / Z31939 / Rev.: 01...

  • Page 63: Glossary / Abbreviations

    The superconducting magnet inside the cryostat is energized. Table A.1: Glossary Abbreviations Description BCFC Bruker Cryogen Free Controller Cryogen Free Electron Paramagnetic Resonance Room Temperature; used for room temperature level and as prefix of parts, which are at room temperature...
  • Page 64 Glossary ZTKS0213 / Z31939 / Rev.: 01...

  • Page 65: Technical Data

    Cryogenic Refrigerator consists of RDK–415D • 4K Cold Head • Compressor Unit F–50H (water cooled) CNA–61 (air cooled) Bruker Cryogen Free Controller BCFC Power Supply E700–1083 Table A.1: Components of the EPR 12T magnet system A.5.2 Dimensions A.5.2.1 Weights Value...

  • Page 66: Cryostat Dimensions

    Technical Data EPR 12T Cryogen Free A.5.3 Cryostat Dimensions Figure A.1: Dimensions of the cryostat (front view) ZTKS0213 / Z31939 / Rev.: 01...
  • Page 67 Technical Data EPR 12T Cryogen Free Cryostat Dimensions Value Unit 1212 Height of cryostat (without cold head) 1630 Height of cryostat (including cold head) Cryostat diameter D–RT RT bore diameter Distance magnetic center – bottom plate (calculated) Distance magnetic center – top flange...

  • Page 68: Specifications

    Technical Data EPR 12T Cryogen Free A.5.4 Specifications Figure A.3: Fringe field plot of the EPR 12T magnet system Scale division is 0.5 m. Position Distance Magnetic center distance above floor level 814.05 mm Magnetic center distance from top flange 497 mm Table A.6: Position of the magnetic center...
  • Page 69 Technical Data EPR 12T Cryogen Free Fringe Field Fringe Field R [m] Z [m] 0.5 mT 3.40 4.30 1 mT 2.75 3.45 3 mT 1.95 2.45 5 mT 1.65 2.05 200 mT 0.50 0.70 max. magnetic field B at top access point 401 mT max.
  • Page 70 Technical Data EPR 12T Cryogen Free Magnet Parameters Description Value Unit Main Coil Main current / magnetic field _____ A / T Main coil current rate A / min Main coil voltage rate V / min Sweep Coil Sweep current / magnetic field...

  • Page 71: Power Supply Parameters

    Technical Data EPR 12T Cryogen Free A.5.5 Power Supply Parameters To enter the parameters into the power supply a service code is requested. Only Bruker Service is allowed to set the parameters in the PARA menu of the power supply (Table A.10,...
  • Page 72 Technical Data EPR 12T Cryogen Free EPR 12T Cryogen Free, Serial No. ____ Position Explanation Command Unit Value U main level 3 VM3/, VM3= I main level 4 CM4/, CM4= ____ U main level 4 VM4/, VM4= I main heater...
  • Page 73 Technical Data EPR 12T Cryogen Free EPR 12T Cryogen Free, Serial No. ____ Position Explanation Command Unit Value Cernox S2 R4 C24/, C24= Ω ____ Cernox S2 R5 C25/, C25= Ω ____ Cernox S2 R6 C26/, C26= Ω ____ Tc1 50 A...

  • Page 74: Base Temperature Report (Monthly)

    Technical Data EPR 12T Cryogen Free A.5.6 Base Temperature Report (Monthly) Date Temperature * Temperature * Compressor Remarks Signature Sensor S1 [K] Sensor S2 [K] Elapsed Time [h] Table A.13: Base temperature report (monthly) (continued) * Refer to section "First Steps" on page...
  • Page 75 Technical Data EPR 12T Cryogen Free Date Temperature * Temperature * Compressor Remarks Signature Sensor S1 [K] Sensor S2 [K] Elapsed Time [h] Table A.14: Base temperature report (monthly) * Refer to section "First Steps" on page ZTKS0213 / Z31939 / Rev.: 01...

  • Page 76: Other Applicable Documentation

    Technical Data EPR 12T Cryogen Free A.5.7 Other Applicable Documentation List of Spare Parts and Accessories Description Type Material No. Usage O-ring 57 x 2.5 40695 Vacuum valve O-ring 44 x 2.5 40693 Vacuum valve O-ring 36.14 x 2.5 40692...

  • Page 77: Index

    Hazard from Magnetic Field .......... 34 Indicator .... 70 Main Current / Magnetic Field Cernox Maintenance Schedule ...... 53 ......37 Manufacturer, Bruker BioSpin ..... 5 Display Cernox Mode ......72 Para Menu Settings Compressor .... 37 Drive Switch CNA-61 Para Menu ......
  • Page 78 Index Technical Data ........65 Tilt Watch ........... 22 Tilting ..........15 Transportation, Dimensions for Trans- portation ..........65 Troubleshooting ......... 50 Problems .......... 51 Solutions UPS, Uninterruptible Power Supply ... 34 Vacuum Valve ........29 ....29 Mounting the Vacuum Valve ......
  • Page 79 EPR 12T Cryogen Free User Manual Revision History List Index: Date: Alteration Type: April 2011 First release Updated work flow for cool down to base temperature. Added August 2014 position of magnetic center. Implemented new directives on fringe field data.
  • Page 80 Bruker Corporation info@bruker.com www.bruker.com Order No: Z31939...

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