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Agilent Technologies Cryogenic User Manual

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Cryogenic Systems
Operation
User Guide
Agilent Technologies

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  • Page 1 Cryogenic Systems Operation User Guide Agilent Technologies...
  • Page 2 Further, to the max- agreement and written consent from imum extent permitted by applicable Agilent Technologies, Inc. as governed by C A U T I O N law, Agilent disclaims all warranties, United States and international copyright either express or implied, with regard laws.

  • Page 3: Table Of Contents

    Removing the Agilent Cold Probe from the Magnet Removing the Agilent Cold Probe from magnet when <285 K Agilent Cold Probe/Cryogenic System Care When Not in Use Agilent Cold Probe will remain attached to the CryoBay Agilent Cold Probe disconnected from the CryoBay...
  • Page 4 Compressor Maintenance Closed-Cycle Chiller (CCC) Maintenance Changing Cooling-Water Filters (Water-Cooled Compressor) Cooling-water requirements Changing cooling-water filters Principles of Operation Cryogenic System Components Principles of Operation External CryoBay Controls and Connections Internal CryoBay Assemblies Operation Cycle, Status Messages, and States Idle...
  • Page 5 Turning on or off the CryoBay sample eject air Adjusting the CryoBay sample eject air Inserting a sample using a sample catcher Ejecting and removing a sample using a sample catcher Swagelok and Aeroquip Fittings Swagelok connector installation Retightening swagelok connectors Cryogenic Systems Operation...
  • Page 6 Aereoquip connectors Connecting to helium compressor and CCC Disconnecting from helium compressor Cryogenic Systems Operation...

  • Page 7: Introduction

    Cryogenic Systems Operation User Guide Introduction A Cryogenic system consists of an Agilent Cold Probe and closed- cycle cryogenic system. The cryogenic system circulates cold He gas to maintain key probe components at an operating temperature of approximately 25 kelvin.

  • Page 8: Safety

    Unless restrained, such objects can suddenly fly towards the magnet, causing possible personal injury and extensive damage to the probe, dewar, and superconducting Cryogenic Systems Operation...
  • Page 9 Operation with flammable gases or fumes present creates the risk of injury or death from toxic fumes, explosion, or fire. Leave area immediately in the event of a magnet quench. WA R N I N G If the magnet dewar should quench (sudden appearance of Cryogenic Systems Operation...
  • Page 10 The magnet dewar has a high center of gravity and could tip over in an earthquake or after being struck by a large object, injuring personnel and causing sudden, dangerous release of nitrogen and helium gasses from the dewar. Therefore, the Cryogenic Systems Operation...

  • Page 11: Caution Notices

    Refer to the manuals supplied with the magnet for the size of a typical 5- gauss stray field. This gauss level should be checked after the magnet is installed. Check helium and nitrogen gas flow meters daily. C A U T I O N Cryogenic Systems Operation...

  • Page 12: Radio-Frequency Emission Regulations

    RF interference within the instrument and may increase the RF energy transmitted by the instrument in violation of regulations covering RF emissions. It is the operator’s responsibility to maintain the instrument in a condition that does not violate RF emission requirements. Cryogenic Systems Operation...

  • Page 13: Agilent Cold Probes

    Introduction Agilent Cold Probes Agilent Cold Probes, Figure 1, achieve significant gains in sensitivity through the application of advanced cryogenic technologies for cooling key probe components. Figure 1 Agilent Cold Probes Cryogenic Systems Operation...

  • Page 14: Closed-Cycle Cryogenic System

    The Closed- Cycle Cryogenic system consists of the following units: CryoBay (cryogenics bay) • Closed- cycle chiller (CCC) or helium (He) refrigerator The CCC supplies cold He gas to the cryogenic heat exchanger inside the Agilent Cold Probe. • Valve Box / Control Board Cryogenic Systems Operation...

  • Page 15: He Compressor

    Agilent Cold Probe. • Vacuum System The vacuum system automatically pumps down the cryogenic system and the probe. The vacuum system is connected to the probe's vacuum pump- out port using a flexible pumping line.
  • Page 16 Introduction Cryogenic Systems Operation...

  • Page 17: Cryogenic Operation

    Final System Checks, Cautions and Warnings Configuring VnmrJ for Cryogenic Operation Starting Cryogenic Operation Stopping Cryobay Operations Disconnecting the Agilent Cold Probe from the CryoBay Removing the Agilent Cold Probe from the Magnet Agilent Cold Probe/Cryogenic System Care When Not in Use Agilent Technologies...

  • Page 18: Preparing For Cryogenic Operation

    For normal operation, begin preparation for cryogenic operations with the Agilent Cold Probe at room temperature in the magnet. Connect the CCC transfer arm (stinger) to the probe Verify that the side arm of the probe is firmly clamped to the magnet using the side- arm support provided.
  • Page 19 Cryogenic Operation • Inspect the interior of the cryogenic arm of the probe for foreign objects and extra bushings. Remove any foreign materials and bushings. • Verify that the brass stinger tip is screwed on tightly and is not loose.
  • Page 20 Cryogenic Operation Figure 5 Connect CryoBay to Agilent Cold Probe Slide the flexible cryogenic transfer line into the probe side arm until the coupling is well seated. If the coupling does not seat properly, extract the transfer line and inspect the cryogenic arm and stinger for multiple plastic bushings.
  • Page 21 Open the snap clips on the vibration damping pier and remove the top. Lay the cryogenic transfer line into the large slot on the left on the vibration damping pier. Lay the vacuum line into the large slot on the right.

  • Page 22: Connect The Vacuum System To The Probe Vacuum Chamber

    Verify that the system status is Idle or Safe. • If in Safe state, see “Recovering from an Unexpected Event” on page 103, before proceeding. • Click on the Controls button. The CryoBay Controls popup window appears. Load the Correct Temperature Calibration File. Cryogenic Systems Operation...
  • Page 23 Cryogenic Operation This is only necessary if multiple Agilent Cold Probes are in use on the same system. “CryoBay Controls - Loading Files” on page 72. Verify all utilities are attached and turned ON. Cryogenic Systems Operation...

  • Page 24: Final System Checks, Cautions And Warnings

    Review check list and verify that all the conditions are met before starting cryogenic operations. If any checked list items are not connected, functioning, or turned on the cryogenic system will not function or will not function correctly, and in some cases the equipment could be damaged.
  • Page 25 Cryogenic Operation The stinger at the end of the flexible cryogenic transfer line could WA R N I N G be ejected and cause injury to personnel in the area, damage to equipment, or both. This step pressurizes the system. DO NOT uncouple the probe from the CCC while the system is pressurized.

  • Page 26: Configuring Vnmrj For Cryogenic Operation

    Cryogenic Operation Configuring VnmrJ for Cryogenic Operation Open the VnmrJ window. The CryoBay page is hidden. In the menu, click edit and then System Settings. You must be the system administrator, typically Vnmr1. The system settings window opens, as seen in Figure Click on the System tab.
  • Page 27 Cryogenic Operation CryoBay Figure 10 Configuration window and cryo page Cryogenic Systems Operation...

  • Page 28: Starting Cryogenic Operation

    • Cooling down the probe • Regulating the probe internal temperature at the set point. • Monitor and control all cryogenic functions and systems. “Operation Cycle, Status Messages, and States” page 57. Click the Start button for information on the operation cycle.
  • Page 29 Close the valve on the helium cylinder. b. Close the helium regulator valves. Tighten the side- arm coupling nut on the cryogenic transfer arm periodically during cool- down. Adjust the nut at approximately 100 K and 30 K, or roughly every 30 minutes.

  • Page 30: Stopping Cryobay Operations

    31. appears: • Warm up the system — Click Ok. • Continue with cryogenic operation — Click Cancel. The cryogenic system will proceed to its warming cycle. • Status displays Warming. • Accelerated warm- up takes about nine hours. Do not disconnect the probe at this time, keep the probe attached to the CCC.
  • Page 31 Cryogenic Operation Stop Pop-up warning appears after Stop button is clicked Figure 12 CryoBay controls popup and stop warning screen Cryogenic Systems Operation...

  • Page 32: Disconnecting The Agilent Cold Probe From The Cryobay

    Injury to personnel in the area, damage to equipment, or both WA R N I N G could result if the stinger at the end of the flexible cryogenic transfer line is ejected. The system is pressurized. DO NOT uncouple the probe from the CryoBay while the system is pressurized.

  • Page 33: Disconnecting The Agilent Cold Probe From The Cryobay

    Release the vibration damping pier clamps. Remove the top of the pier. Unscrew cryogenic transfer line coupling nut. Separate the CryoBay cryogenic transfer line from the Agilent Cold Probe. A portion of the He working gas will be vented during cryogenic transfer line separation.
  • Page 34 Do not attempt to extract the plastic sleeve as it is easy to damage it. Immediately cap off the cryogenic couplers, both on the CryoBay cryogenic transfer arm and the Agilent Cold Probe.

  • Page 35: Removing The Agilent Cold Probe From The Magnet

    The Agilent Cold Probe can be removed from the magnet during any point in the cryogenic operation (provided adequate VT gas flow is maintained). It is easier to manage this operation if the cryogenic system is in the Idle state, as VT gas is not required. Remove any sample.
  • Page 36 Release the vibration damping pier clamps. Remove the top of the pier. Unscrew cryogenic transfer line coupling nut. Separate the CryoBay cryogenic transfer line from the Agilent Cold Probe. A portion of the He working gas will be vented during cryogenic transfer line separation.

  • Page 37: Removing The Agilent Cold Probe From Magnet When <285 K

    Removing the Agilent Cold Probe from magnet when <285 K The Agilent Cold Probe may be removed from the magnet during Cryogenic operation or while cold if the Removable Agilent Cold Probe accessory has been purchased. The Removable Agilent Cold Probe accessory is designed to route dry gas through the Agilent Cold Probe’s center tube while...
  • Page 38 Failure to supply nitrogen gas to the Agilent Cold Probe's center C A U T I O N tube during cryogenic operation can result in condensation and frost in the bore of the probe with potential damage to the probe.

  • Page 39: Agilent Cold Probe/Cryogenic System Care When Not In Use

    40, after the system status returns to Idle to stop vacuum pumping of the probe. The cryogenic transfer line is vented as a normal part of Detach. N O T E The system state changes to Detaching Probe and then returns to Idle.
  • Page 40 Cryogenic Operation Pump Probe Figure 14 CryoBay controls - pump probe Detach Figure 15 CryoBay controls - detach Cryogenic Systems Operation...

  • Page 41: Agilent Cold Probe Disconnected From The Cryobay

    Click OK or cancel. The vacuum pumping automatically stops and returns the system to Idle when the CryoBay vacuum system has been pumped out to a system- specified vacuum level. Vacuum Purge Figure 16 CryoBay controls - vacuum purge Cryogenic Systems Operation...
  • Page 42 Cryogenic Operation Cryogenic Systems Operation...
  • Page 43 Cryogenic Systems Operation User Guide Maintenance and Service Preventative Maintenance and Service Intervals Changing the Helium Gas Supply (Compressed Gas Cylinder) Filling the Helium Compressor Turbo Pump Operation Compressor Maintenance Closed-Cycle Chiller (CCC) Maintenance Changing Cooling-Water Filters (Water-Cooled Compressor) This section provides an overview of the closed- cycle system, maintenance and service operations.

  • Page 44: Maintenance And Service

    If problem still occurs, call for service Compressed helium Replace helium cylinder. May be delayed until just cylinder pressure before starting cryogenic < 500 psi. operations. Every 2 months Operate vacuum pump CryoBay automatically performs this service.

  • Page 45: Changing The Helium Gas Supply (Compressed Gas Cylinder)

    Required: 99.999% helium gas cylinder with > 500 psi (3.4 mPa) pressure, 400 psi regulator compatible with high purity helium. Cryogenic system must be in either the Idle or Operating state. Close the valve on the helium cylinder. Close the helium regulator valves.

  • Page 46: Filling The Helium Compressor

    Required: 99.999% Helium gas cylinder with > 500 psi (3.4 mPa) pressure, 400 psi regulator compatible with high purity helium. Cryogenic system must be in the Idle state. Close the valve on the helium cylinder. Close the helium regulator valves.
  • Page 47 Loosen the nut slowly. If the helium line was pressurized, a hissing C A U T I O N will be heard. Remount the helium line to the CryoBay. See “Changing the Helium Gas Supply (Compressed Gas Cylinder)” page 45. Cryogenic Systems Operation...

  • Page 48: Turbo Pump Operation

    The compressor oil adsorber must be serviced (before 20,000 hours for air cooled or 30,000 hours for water cooled of operation) or damage to the cryogenic system may occur. To check the hours of compressor operation: • Check the hour meter located on the compressor.

  • Page 49: Closed-Cycle Chiller (Ccc) Maintenance

    The following layout of dual water filters and valves is recommended, as seen in Figure 18, to allow easy replacement of filters without interrupting cryogenic operation. The instructions assume that filter set 2 is in use initially. Open valve to compressor Filter set 1...
  • Page 50 Damage to the He compressor from over-heating can result from air C A U T I O N bubbles in the cooling water line. Remove all air bubbles from the cooling-water lines before operating the He compressor. Cryogenic Systems Operation...

  • Page 51: Principles Of Operation

    Cryogenic Systems Operation User Guide Principles of Operation Cryogenic System Components Principles of Operation External CryoBay Controls and Connections Internal CryoBay Assemblies Operation Cycle, Status Messages, and States This section provides an overview of the closed- cycle system, maintenance and service operations.

  • Page 52: Cryogenic System Components

    • The CCC assembly contains a Gifford- McMahon refrigerator, heat exchanger (within a vacuum dewar), and computer and pneumatic controlled flow control valves and sensors. A special cryogenic transfer line mates the CCC to the probe. • Turbo pump system •...

  • Page 53: Principles Of Operation

    (PID) feedback loop to regulate the temperature of the gas at the set point. All of the cryogenic portions of the system are insulated from room temperature by means of vacuum insulation. Helium gas circulates in a closed loop and is not consumed during normal operations.
  • Page 54 57. • Purging air from the system and helium into the system before cryogenic operation, which is necessary to decontaminate the cryogenic lines whenever a probe is interchanged. • Vacuum pump operations. • Control of the helium gas flow during operation.
  • Page 55 The CCC takes approximately 48 hours to warm- up if the accelerated warm- up is not used (because of power failure). • Purging of helium from the cold loop in preparation for probe detachment from the CryoBay. Cryogenic Systems Operation...

  • Page 56: External Cryobay Controls And Connections

    Pneumatic Probe Valve line Figure 20 CryoBay front connections Helium Helium Supply Return Figure 21 CryoBay back panel The CryoBay Back panel contains the main power switch, control lines and gas connections, as seen in Figure Cryogenic Systems Operation...

  • Page 57: Internal Cryobay Assemblies

    • All valves closed except CryoBay sample eject • CryoBay sample eject valve open • Compressor off • Vacuum pumps off • Temperature control (CCC warm- up off) pump Turbo pump controller Ion pump power supply Figure 22 CryoBay left side Cryogenic Systems Operation...
  • Page 58 Principles of Operation Turbo pump Scroll pump Figure 23 CryoBay right side Cryogenic Systems Operation...

  • Page 59: Start

    Smart valve Figure 24 CryoBay right rear view Start Table 3 Start - Initial state: Idle State CryoBay order of operations/conditions • Vacuum Turbo pump is on (a high pitch hum may be heard –this is pumping normal). Cryogenic Systems Operation...
  • Page 60 Purge helium and fill helium for cold loop (repeated 5 times, fill to 215 psi (1.55 mPa)). • Turn on compressor. • Cool probe until probe reaches set-point temperature. • Operating Temperature controller regulates probe internal temperature. • Ion pump on. • Turbo pump off. Cryogenic Systems Operation...

  • Page 61: Stop

    Turns off turbo pump and closes valves (if on and open). • Open purge out valve. • Wait until inlet pressure < 20 psi (0.14 mPa). • Close purge out valve. • Detach Probe window appears. • Idle Close valves Cryogenic Systems Operation...

  • Page 62: Vacuum Purge

    Close probe vacuum valve (popup button on probe valve will disappear). • Turbo pump off. • Continues with the Detach operation. Figure 25 on page 63 and Figure 26 on page 64 show the software state transition diagram Cryogenic Systems Operation...
  • Page 63 Principles of Operation Figure 25 Software state transition diagram part 1 Cryogenic Systems Operation...
  • Page 64 Principles of Operation Figure 26 Software state transition diagram part 2 Cryogenic Systems Operation...

  • Page 65: Cryobay Monitor

    Cryogenic Systems Operation User Guide CryoBay Monitor Opening the CryoBay Monitor (Vertical Panel) CryoBay Controls Window CryoBay Controls - Loading Files CryoBay Controls – Advanced CryoBay Data Log CryoBay Controls–Help Menu The CryoBay Monitor is the user interface to the CryoBay's internal control board computer.

  • Page 66: Opening The Cryobay Monitor (Main Window)

    VnmrJ If after starting VnmrJ, the Cryo tab does not display among the the vertical panel choices, confirm that VnmrJ is configured for cryogenic operation see section Configuring VnmrJ for Cryogenic Operation on page Open an account with access to the CryoBay controls.
  • Page 67 Table 8 Displays Displays Probe Agilent Cold Probe NA = temperature internal temperature (in controller is off or the degrees Kelvin) probe sensor is not plugged in. Status Cryogenic system status Idle Vacuum pumping Cooling Warming Operating Safe Cryogenic Systems Operation...
  • Page 68 0 = no heater power applied 100 = full heater power applied NA = temperature controller is off or the probe sensor is not plugged in Setpoint Setpoint for Agilent Cold Probe internal temperature control (in degrees Kelvin) Cryogenic Systems Operation...

  • Page 69: Stand-Alone Cryobay Control Computer

    Figure Figure 28 Stand-alone CryoBay control panel CryoBay connections OK should be displayed in the CryoBay message window. The Info button for the Stand- Alone CryoBay Controls software brings up the history of error and notification messages. Cryogenic Systems Operation...

  • Page 70: Cryobay Controls Window

    • Main - CryoBay Main display is duplicated. • Info - Click additional sensor information for the cryogenic system. This is an advanced feature for Stand- Alone CryoBay Controls software. • Actions - User- prompted operation cycles. Figure 29 CryoBay controls popup window Cryogenic Systems Operation...
  • Page 71 Also see “Operation Cycle, Status Messages, and States” on page 57. • Start Starts the system. Only enabled when cryogenic system is in the Idle state. • Stop Stops the system and begins active warm-up. • Disabled when cryogenic system is in the Safe or Warming state.

  • Page 72: Cryobay Controls - Loading Files

    File allows the user to load configuration and calibration files to the CryoBay and the temperature controller, as seen Figure 30. Files may only be loaded when the cryogenic system is in the Idle state. Set the cryogenic system into the IDEL state.
  • Page 73 Click here to load the CryoBay parameter set, as seen in Figure 31 on page 74. An updated parameter set may be loaded if necessary. The default file name is cryo.setup. This will load the CryoBay parameter set. Cryogenic Systems Operation...
  • Page 74 Do not change the temperature controller parameter file unless C A U T I O N instructed to do so by a Service representative. Changes to the parameter file may cause damage to the system. Figure 31 Load CryoBay parameter set - firmware Cryogenic Systems Operation...
  • Page 75 CryoBay Monitor Figure 32 Load temperature controller parameters - firmware Cryogenic Systems Operation...

  • Page 76: Cryobay Controls - Advanced

    “CryoBay Data Log” on page 79. Improperly entering commands into the command lines can C A U T I O N over-ride an existing operation, potentially causing damage to equipment. If in doubt, check with Agilent Customer Service. Cryogenic Systems Operation...
  • Page 77 A range of dates may also be specified. (The "FROM" and "TO" keywords in these commands are case- insensitive.) <UPLOAD FROM 1308855120> sends all data with a date- stamp equal to or larger than the given value. (This is the Unix date- stamp in GMT.) Cryogenic Systems Operation...
  • Page 78 (skipping does not apply to fault messages). So "<UPLOAD 100 4> will return 25 data messages and all the fault messages that occurred during the same time interval. Cryogenic Systems Operation...

  • Page 79: Cryobay Data Log

    Open using Word- pad or Excel. (Do not use Notepad.) Data log sequence of readings displayed DATA: Event, Time Zone, State, Inlet, Exhaust, Mass Flow, Vacuum, Ion Pump, CLI, Probe, CCC1, CCC2, Heater FAULT: 1XX: Fault Message Cryogenic Systems Operation...

  • Page 80: Cryobay Controls-Help Menu

    CryoBay Controls–Help Menu Figure 34 shows the help menus for the stand- alone version Figure 35 shows the help menus for the VnmrJ version. Figure 34 Help menu - stand alone version Figure 35 Help menu - About Cryogenic Systems Operation...

  • Page 81: About Cryobay

    Gives the service- counter run time since the last reset. (Resets performed by Agilent Field Service.) The compressor run time may also be checked by looking at the hour meter on the compressor. About panel Gives the stand- alone software version. Figure 37 About panel Cryogenic Systems Operation...
  • Page 82 CryoBay Monitor Cryogenic Systems Operation...
  • Page 83 Cryogenic Systems Operation User Guide Error Messages Fault Codes CryoBay Actions Under Fault Conditions General Operation Faults Fault Code Causes, Actions, and Corrections Agilent Technologies...

  • Page 84: Fault Codes

    No Mass Flow Single Phase Power Loss UPS on Battery Temperature Out of Regulation Temperature Fault Soft Vacuum Ion Pump Maintenance Needed Turbo Pump Fail Loss of Helium Loop Pressure Pressure Transducer HW Error Probe Sensor HW Error Cryogenic Systems Operation...
  • Page 85 Stage 2 Sensor Fail GM Compressor Alarm GM Compressor Trip CLI Error Purging Timeout Vacuum A Timeout Vacuum B Timeout Vacuum C Timeout Vacuum D Timeout Vacuum E Timeout Vacuum F Timeout Cooling Timeout Warming Timeout GM Compressor Alarm Cryogenic Systems Operation...

  • Page 86: Cryobay Actions Under Fault Conditions

    VnmrJ: Open the Vnmrj Message Bar, then close it. • Stand-Alone CryoBay Control Computer: Click Info, opening a message window, then close ALWAYS confirm that the cause of the cryogenic system shutdown C A U T I O N has been correctly identified and resolved before restarting cooling.

  • Page 87: General Operation Faults

    Cause: system failed to purge the helium to less than 20 psi (0.14 mPa) within 10 minutes. Action: Idle Check: • Pneumatic gas supply to CryoBay is at 80 - 100 psi (5.5- 7.5 bar, 552 - 689 kPa). Cryogenic Systems Operation...
  • Page 88 Error Messages “Compressed Air for Pneumatics Failure” page 101. Cryogenic Systems Operation...

  • Page 89: Fault Code Causes, Actions And Corrections

    “Single-Phase Power Failure” on page 99 Check: CryoBay/UPS power cable is connected Stability and voltage of single phase power source are correct. See Cryogenic System Site Requirements, p/n 91-002698-00A. 103: UPS on Battery Cause: Loss of single phase power to CryoBay Action: Warning UPS running on battery power If Vacuum Pumping >...
  • Page 90 Fault Code Actions and Corrections Check: CryoBay/UPS power cable is connected Stability and voltage of single phase power source are correct. See Cryogenic System Site Requirements. 104: Temperature Out of Regulation Cause: Failure to regulate at set point Action: Stop NMR (VnmrJ only). Warning.
  • Page 91 Five minutes there is no warning, the fault happens five minutes after cause. Vacuum pumping - return to idle. Other - Safe Check: Contact Agilent Service. 114: Probe Control Drop Cause: Temperature regulation failure or loss of communication with temperature controller Action: Warning Cryogenic Systems Operation...
  • Page 92 Action: Warning, CCC warmup disabled. Check: Contact Agilent Service. 121: GM Compressor Alarm Cause: Compressor temperature alarm Action: Vacuum Pumping -> Idle All other states - Warning. Usually, other faults will occur (such as, 105 Temperature Fault). Cryogenic Systems Operation...
  • Page 93 Mass flow and helium pressure are normal. CLI is calculated based on mass flow and pressure transducer readings. Probe is connected properly to cryogenic transfer arm. Pneumatic gas supply to CryoBay is at 80 - 100 psi (5.5 - 7.5 bar, 552 - 689 kPa).
  • Page 94 127: Vacuum C Timeout Cause: Pumping probe takes too long Action: Return to Idle Check: Contact Agilent Service. 128: Vacuum D Timeout Cause: Poor vacuum while in the Operating state Action: Warming Check: Contact Agilent Service. 129: Vacuum E Timeout Cryogenic Systems Operation...
  • Page 95 Compressor pressure alarm (helium pressure too low) Action: Vacuum Pumping -> Idle All other states - Warning. Usually, other faults will occur (such as, 105 Temperature Fault). Check: Ensure the CryoBay cryogenic transfer arm O-ring seal is well seated (source of leak). Cryogenic Systems Operation...
  • Page 96 Fault code causes, actions and corrections Fault Code Actions and Corrections Agilent Cold Probe cryogenic arm o-ring seal is in good condition The Helium level at compressor Compressor / CCC Cold Head cable is connected to compressor All Aeroquip fittings on compressor helium lines are tight and are not missing O-rings Check for correct pressures while at Idle (room temperature).

  • Page 97: Unexpected Events

    Cryogenic Systems Operation User Guide Unexpected Events Advanced Notice of Utility Shutdown Single-Phase Power Failure Three-Phase Power Failure (Compressor) Cooling-Water Failure (Water-Cooled Compressor) Compressed Air for Pneumatics Failure Temperature Controller Gas Failure Host Computer Failure Recovering from an Unexpected Event...

  • Page 98: Advanced Notice Of Utility Shutdown

    If possible, this should be done at least 10 hours before the utility shutdown. If using a water- cooled compressor, allow the water cooling to continue for at least 15 minutes after the compressor has stopped. Cryogenic Systems Operation...

  • Page 99: Single-Phase Power Failure

    CryoBay sample eject air needle valve. After the UPS battery has been exhausted, it will take approximately three N O T E hours for the battery to recharge when power is restored. Normal CryoBay operation is available while the UPS is charging. Cryogenic Systems Operation...

  • Page 100: Three-Phase Power Failure (Compressor)

    Temperature Fault). It takes some time for the compressor to cool enough to resume operation and usually requires a warm up of the system. The customer should initiate a standard Stop operation before additional faults are incurred. Cryogenic Systems Operation...

  • Page 101: Compressed Air For Pneumatics Failure

    The vacuum gauge or ion pump will display an increasing pressure. The error code seen will depend on the state the cryogenic system is in at that time. The probe vacuum valve pop- up indicator should be up during Cooling, Operating, or Warming. If it is not, there may be a problem with the pneumatic gas or pneumatic gas connection to the probe.

  • Page 102: Host Computer Failure

    Operating state. It will continue in the Operating state until an error occurs or a new command is received from the host computer. When the host computer is operating again, open the CryoBay Monitor and click the Connect button. See “CryoBay Monitor” on page 65. Cryogenic Systems Operation...

  • Page 103: Recovering From An Unexpected Event

    Generally, the only condition that warrants a routine use of <SETWARM> is a power failure. To resume the Warming operation: Open the CryoBay Controls Advanced window. Verify that the cryogenic system is in either the Idle or Safe state. In the Send CryoBay command line enter, Figure 41 page 104: <SETWARM>...

  • Page 104: Ccc Has Reached Room Temperature

    CryoBay sample eject air. “CryoBay Sample Eject Air and Sample Catcher” on page 110. The system may be restarted using the standard Start procedure. Do not forget to review “Final System Checks, Cautions and Warnings” on page 24. Cryogenic Systems Operation...

  • Page 105: Safety Shutdown

    The compressor supplies power to the CCC cold head via the cold head control cable. Safety shutdown of the system Cryogenic system is in the Idle state. Press the UPS OFF switch, located on the panel opposite the CryoBay transfer arm and labeled Main Power Switch.
  • Page 106 Unexpected Events Temperature Controller Smart valve Figure 42 CryoBay right rear view Cryogenic Systems Operation...

  • Page 107: Powering System Back On After Safety Shutdown

    UPS, and is labeled Battery Connector. Plug in the main power cord. Replace the CryoBay panel. Press the UPS ON switch. Located on the panel opposite the CryoBay transfer arm (labeled Main Power Switch). Cryogenic Systems Operation...
  • Page 108 Switch the Main Power switch (breaker) to ON. Switch the Drive switch to ON. Verify that the Cold Head Drive switch is OFF. Verify that the Remote Drive switch is set to remote (or EXT). Resume normal cryogenic operations. Cryogenic Systems Operation...

  • Page 109: Appendix

    Cryogenic Systems Operation User Guide Appendix CryoBay Sample Eject Air and Sample Catcher Turning on or off the CryoBay sample eject air Adjusting the CryoBay sample eject air Inserting a sample using a sample catcher Ejecting and removing a sample using a sample catcher...

  • Page 110: Cryobay Sample Eject Air And Sample Catcher

    Changes in the house pneumatic gas supply, probe or sample may C A U T I O N affect the adjustment of the sample air eject. It is advisable to verify both console and CryoBay sample eject performance when changing probes or samples of significantly different weights. Cryogenic Systems Operation...

  • Page 111: Turning On Or Off The Cryobay Sample Eject Air

    Do not click Stop if the system is in the Operating state. It will stop C A U T I O N cryogenic operations and begin warm up. If in the Operating state, in the Send CryoBay command line enter: <DO0 0>. Click Send CryoBay.
  • Page 112 If in the Operating state: From the CryoBay Controls Advanced window, as seen in Figure In the Send CryoBay command line enter: <DO0 1> Click Send CryoBay. Enter <DO0 1> (on) or <DO0 0> (off) in command line Figure 46 Sample eject air Cryogenic Systems Operation...

  • Page 113: Adjusting The Cryobay Sample Eject Air

    Locate the CryoBay sample eject air valve. It will be in line with the CryoBay sample eject pneumatic line, which exits from the CryoBay on the same side as the cryogenic transfer arm. Close the needle valve attached to the eject line. Open the CryoBay sample eject pneumatic valve (instructions above).
  • Page 114 Close the CryoBay sample eject pneumatic valve. Repeat step 12 through step 19 as necessary to properly adjust the eject air. Cryogenic Systems Operation...

  • Page 115: Inserting A Sample Using A Sample Catcher

    Turn on the eject air from VnmrJ or VNMR using the eject button or eject command. Remove the turbine and sample held in place by the sample catcher release lever. Turn off the eject air or insert a new sample. Cryogenic Systems Operation...

  • Page 116: Swagelok And Aeroquip Fittings

    1 1/4 turns. Insert tube into Swagelok and tighten the nut finger-tight Scribe line at 6 o’clock position Body nut Finger-tighten then tighten the Swagelok nut 1 1/4 turns Figure 47 Swagelok installation Cryogenic Systems Operation...

  • Page 117: Retightening Swagelok Connectors

    Tighten the nut slightly from the position of resistance. Insert tubing with the ferrule until it seats Body nut Finger-tighten the Swagelok until resistance increases then tighten slightly with a wrench Figure 48 Retightening swagelock connectors Cryogenic Systems Operation...

  • Page 118: Aereoquip Connectors

    I G H L I U I G H I N G T E R I N L U L U L Flexible line I N G T E R T L E Figure 49 Aereoquip connectors Cryogenic Systems Operation...

  • Page 119: Connecting To Helium Compressor And Ccc

    Hold the body nut and unscrew the union nut the remainder of the way. Some venting of gas may occur, this is normal. Cryogenic Systems Operation...
  • Page 120 Appendix Cryogenic Systems Operation...
  • Page 122 Agilent Technologies © Agilent Technologies, Inc. Printed in USA, August 2011...

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