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CryoProbe System Installation Version 1 BRUKER...
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The information in this manual may be altered without notice. BRUKER accepts no responsibility for actions taken as a result of use of this manual. BRUKER accepts no liability for any mis- takes contained in the manual, leading to coincidental damage, whether during installation or operation of the instrument.
Personnel safety ..............9 Safety of CryoProbe equipment ......... 11 First aid ................11 Introduction ............13 How to use this manual ............. 13 CryoProbe System overview ..........13 Conventions ..............14 Initial setup ............17 Before delivery ..............17 Transport ................17 Check the site preparations ..........
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........54 3.24 Put HPPR CRP assembly into operation ......54 3.25 How to proceed ..............55 Customizing the CryoProbe System ....57 Experimental parameters ..........57 RF power levels ............57 Safety attenuators ............57 Standard parameter sets ..........57 Lock power ..............
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Site preparation checks ............. 75 Preparations for the installation visit ........75 User training ..............76 Related documents ..........79 Conversion of metric units ......... 81 Glossary .............. 83 Figures ..............89 Tables ..............91 CryoProbe Installation BRUKER 5 (93)
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Contents 6 (93) BRUKER CryoProbe Installation...
Safety 1000000 Read these safety instructions carefully and make them accessible to everybody working with the CryoProbe System. A CryoProbe can be operated easily and safely provided the correct procedures are obeyed and certain precautions ob- served. Terms and symbols WARNING: Disregard of this may lead to personal injury.
Disclaimer is not responsible or liable for any injury or damage that occurs as a con- RUKER sequence of non-approved manipulations on the CryoProbe System. Emergency The main switch on the CryoCooling Unit front serves as an E . It...
Personnel safety Personnel safety All persons who work with or in the close vicinity of a CryoProbe System must be informed about its safety issues and emergency procedures. WARNING: Do not disconnect any tube or cable from a running CryoProbe Sys- tem unless W light up on the CryoCooling Unit front panel.
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Safety NOTE: If a pressure or vacuum leak appears, the CryoProbe System will be auto- matically stopped and warmed up to ambient temperature. Pressurized helium gas supply WARNING: Move, connect, and operate the He steel-cylinder carefully. Obey all safety precautions pertinent to high pressure gas containers and magnetic ob- jects.
‘L ’ sheet. See also IMITATIONS ARNINGS User Manual. First aid If cold helium gas comes in contact with eyes or skin, immediately flood the affect- ed area with cold or tepid water. CryoProbe Installation BRUKER 11 (93)
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Safety 12 (93) BRUKER CryoProbe Installation...
How to use this manual This CryoProbe System Installation Manual guides you through the initial setup and test of a CryoProbe System. Several procedures are the same as in daily use, so they are described in the CryoProbe System User Manual. The two man- uals are complementary and must both be available for an installation.
With 2m Transferline: European Z45447 Version: Transferline BH 0420 Support Mounting Kit for 500 MHz BRUKER SB Magnet with Boss2 shim system: Z 46554 HPPR CRP (Cryo-compatible HPPR Z003422 AVANCE Console Conventions setting of a hardware switch or button MALL CAPS ITALIC...
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Courier italic bold RUKER Times bold Unix or Windows NT object clicked with the mouse NMR Suite object clicked with the mouse Times italic bold RUKER Times italic host name, ser name etc. < > place holder CryoProbe Installation BRUKER 15 (93)
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Introduction 16 (93) BRUKER CryoProbe Installation...
RUKER personnel will connect all units of a the CryoProbe System as far as re- RUKER quired for test and operation but they will not work on the laboratory infrastructure (e.g.
Transport pathways Check transport pathways and transportation means before sale. Do size or weight of the CryoProbe System exceed the capabilities of elevators, floors etc.? Usually, the same transport pathway as used for the magnet delivery will be fine (see Avance Site Planning 200-700, § 1.5). A pallet truck suffices as transport aid.
Is a NMR performance reference data set available (sensitivity, lineshape, water suppression, etc.)? Are any spectral artifacts visible like spikes or noise? IMPORTANT: Before installing the CryoProbe System, make sure there are no performance problems with the conventional parts of the spectrometer. The Cryo-...
See section 2.5 in the He Compressor operation manual which is delivered with the CryoPlatform. NOTE: On the backside of the He Compressor, keep the protective cap on the . This connector is never used. ELIUM HARGE 20 (93) BRUKER CryoProbe Installation...
Install the He Compressor on a level surface. Two of its four casters should be locked. Provide extra space around the units as required for connections, ventilation, and service (details are given in the CryoProbe System Site Planning Guide). NOTE: Orientation of the Transferline Support: the screw fixture of the vacuum tube must face the CryoCooling Unit.
VT gas enters the CryoProbe no colder than the lowest permitted sample temperature. This temperature is specified on the CryoProbe’s L IMITATIONS sheet. The test can be run conveniently while the CryoProbe System is ARNINGS installed. In the presence of an isolated VT gas port that is integrated with the Tuning Adapter, this BCU05 cooling test can be skipped.
Replace the second brace only after the first brace has been tightened. Remove the 9 fixing screws from the magnet stand. Do not switch O the magnet’s air suspension yet but wait until the Cry- oProbe is mounted. CryoProbe Installation BRUKER 23 (93)
Do not untie the red clamping ring from the shim upper part at the top of the magnet because it determines the cor- rect position of the shimcoils. CAUTION: Do not touch the Allen key screws in the magnet’s flat top flange! 24 (93) BRUKER CryoProbe Installation...
M5⌠20 Allen key screws, non-magnetic (11127 each) instead of M5⌠12 Table 3.5. Attach the Mounting Hardware step action Switch O the magnet’s air suspension. CryoProbe Installation BRUKER 25 (93)
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Mounting Hardware, shim system, desired CryoProbe orientation, and magnet parts like drop-off plates. See the CryoProbe System Site Planning Guide for a 1:1 draw- ing of the Mounting Hardware interface plate (the interface plate is the part that touches the magnet).
Figure 3.3. Never hold a CryoProbe at its tube! CAUTION: Do not heat or cool the CryoProbe housing from the outside (e.g. do not try to speed up the evacuation process by heating the CryoProbe with a heat gun). CryoProbe Installation BRUKER 27 (93)
Prepare the CryoProbe support plate: all five screws should be moved almost out of the plate. Verify without a CryoProbe that the support plate will snap into the notches on the rails (Figure 3.4.). Remove it afterwards again. 28 (93) BRUKER CryoProbe Installation...
Carry the CryoProbe at its bottom when moving it from its storage place to the magnet. It is fragile but weights about 12 kg. CAUTION: Never hold a CryoProbe at its tube! CryoProbe Installation BRUKER 29 (93)
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CryoProbe tube by keeping it close to the rails - but do not press it against them. Do not use any extra force to push it up, it should slide without resistance. 30 (93) BRUKER CryoProbe Installation...
Check the orientation of the CryoProbe in the magnet: Its front must be able to meet the He Transferline. IMPORTANT: If cranked pillar braces are present in the magnet stand, the CryoProbe must be centered in their gap at all times (see Figure 3.6.). CryoProbe Installation BRUKER 31 (93)
Turn the other four screws on the support plate in an alternate fashion such that they support the CryoProbe gently. Take care not to tilt its body by forcing one screw more that the other screws. 32 (93) BRUKER CryoProbe Installation...
Check the magnet alignment Check the magnet’s vertical position with a level and correct if necessary. Spinning test Insert a typical sample into the magnet and check if it can be spun. Remove the sample after the test. CryoProbe Installation BRUKER 33 (93)
CryoCooling Unit is on or at least flashing. For recommendations on sample tube quality, filling heights, and spinners, refer to the CryoProbe System User Manual, "Samples and spinners" on page 55. If spinning does not work, see "Spinning problems" on page 60. Joining the CryoCoupler 3.12...
3.9.): are they in place, clean and undamaged? If not replace with the o-rings found in the spare parts box delivered with each CryoProbe System. The o-rings are of type viton and size 7.1 by 1.6 mm. Figure 3.9. O-rings on the CryoCoupler CryoProbe Installation BRUKER 35 (93)
Figure 3.10. Turn the CryoCoupler Hold the CryoCoupler on the He Transferline with one hand. Take the vacuum joint which is 1 m away from the CryoCoupler into the other hand (see Figure 3.11.). 36 (93) BRUKER CryoProbe Installation...
The He Transferline Support may be in the way during the insertion process. If this is the case, remove the CryoCoupler, move the Trans- ferline Support a little aside and repeat the insertion process. When a smooth insertion fails, take the CryoCoupler out and try again. CryoProbe Installation BRUKER 37 (93)
If the versions of UniTool and CryoController Firmware are not the most current ones, they need to be updated. Directory structure On the CryoProbe System laptop, the following directories are required: UniTool program D:\app\Bruker\unitool Firmware file crcoxx.abs...
If a crossing cannot be avoided, burry or cover them. NOTE: There is no point in testing components of the CryoProbe System sepa- rately. Fault analysis is easiest when the CryoProbe System is tested as a whole CryoProbe Installation...
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VT Interface Box to the B socket on the CryoController inside the CryoCooling Unit. Extent the other line from the VT Interface Box with cable Z14278 which will go to the CryoProbe. 40 (93) BRUKER CryoProbe Installation...
Start the CryoTool on the laptop by either clicking its desktop icon or Start - Bruker - CryoTool - CryoTool. Select COM1, double-click the ‘ ’ in the word with the right (!) mouse button, and click Service to Firmware bring up the full interface and Log to see the system messages.
IMPORTANT: The He Regulator and Hose have to be flushed to keep impurities out of the He steel-cylinder. 1st leak test: mark the actual pressure on the primary gauge and close the He steel-cylinder main valve. 42 (93) BRUKER CryoProbe Installation...
CryoPlatform. CAUTION: Lay all tubes and cables such that they don’t cross the floor on a walk- way. If a crossing cannot be avoided, bury or cover them. Necessary tools: CryoProbe Installation BRUKER 43 (93)
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He Compressor front. It should read a bit more than 0 bar without a drop during several minutes. IMPORTANT: If the pressure gauge indicates plain 0 bar, contact : this is a major problem and a lengthy gas purifying cycle is RUKER required. 44 (93) BRUKER CryoProbe Installation...
Open the He steel-cylinder main valve by ~one turn. Warning labels 3.17 Stick a warning label (Figure 3.13.) on all mobile units of a CryoProbe System that contain magnetic materials and could be attracted by the NMR magnet. CryoProbe Installation...
The reading in edte should indicate room temperature. Attach the Tuning Adapter (Figure 3.14.) to the CryoProbe bottom. Use the blue Tuning Tool to lock its mounting screws. NOTE: There are specific Tuning Adapters for each type of CryoProbe. 46 (93) BRUKER CryoProbe Installation...
(Figure 3.15.). Turn the actuator screw clockwise. Its thread must grip into the thread of the CryoProbe’s vacuum plug. Continue gently until the stop is reached but do not force it into the stop. CryoProbe Installation BRUKER 47 (93)
Probe RF Electronics Technical Manual). Regulate the VT gas flow rate to (at least) the value specified on the sheet. IMITATIONS ARNINGS j.10 Set the VT heater power limit as given on the L IMITATIONS ARNINGS sheet. 48 (93) BRUKER CryoProbe Installation...
O and ready. CAUTION: Before powering-up a CryoProbe System for the first time, e.g. during an installation, double-check if the voltages and fuses in the laboratory meet the requirements given on the backpanels of CryoCooling Unit, He Compressor, and (optional) water chiller.
CAUTION: Do not initiate a cool-down if no regulated VT gas flows. Do not insert a sample if the CryoProbe is not at its operating temperature or if the tem- perature in its sample cavity does not stabilize at the desired value. 50 (93) BRUKER CryoProbe Installation...
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CryoProbe. NOTE: Damages of this kind are not covered by the warranty. B is not li- RUKER able for destroyed samples due to disregard of the instructions given in the Cryo- Probe documentation. CryoProbe Installation BRUKER 51 (93)
3.22 NOTE: If any detectable malfunction appears, a cool-down will be automatically stopped and the CryoProbe System is automatically warmed-up to ambient tem- perature. CAUTION: Do not move a cryogenically cold device. Do not try to fix a leak on a cold part because cracking of frozen o-rings, valves etc.
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54 and "Put HPPR CRP assembly into operation" on page 54. Do not leave the CryoProbe System unattended during the first cool-down. While the cool-down is in progress for about 2 h, there is plenty of time to do the "HPPR CRP configuration"...
This can be done conveniently while the first cool-down is in progress. Get the software release Connect to the B ftp.bruker.de server and login either as or anonymous RUKER with your full e-mail address as password. Transfer the crponoff.* files from /pub/nmr/XWINNMR/utilities/ to the...
HPPR modules. How to proceed 3.25 When the CryoProbe is cold and ready, continue in the CryoProbe System User Manual with “HPPR CRP configuration” on page 44. This Installation Manual will be used again later for the installation of options and for customizing the system.
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Initial setup 56 (93) BRUKER CryoProbe Installation...
Customizing the CryoProbe System 4000000 Experimental parameters RF power levels 4.1.1 Maximum RF powers are specified in Watt for each CryoProbe on its ‘L IMITATIONS ’ sheet. Since the relation between absolute power and pl values de- ARNINGS pends on the actual spectrometer hardware, the RF limits must be translated into power levels pl.
Customizing the CryoProbe System when entering the CryoProbe. Special care must be taken to avoid leaks such that the VT gas remains dry and its flow rate constant. Sample tubes and spinners 4.1.6 A CryoProbe has smaller tolerances for sample spinning that conventional probes.
To reset an E on the CryoCooling Unit front panel, press if the RROR COOL DOWN system is already cold or cooling down. If the CryoProbe System is warm or warming up, press ’. WARM UP CryoController The CryoController is located inside the CryoCooler cabinet (see "How to open the CryoCooling Unit"...
Had the shim system been removed some time ago? If the gap is larger, do the five screws in the Mounting Hardware fail to support the CryoProbe? If they are ok, lower the CryoProbe by a few mm and re-insert it 60 (93) BRUKER CryoProbe Installation...
Reboot the CryoController via the mains O on CryoCooling Unit front. See “Emergency Off” on page 71 in the User Manual for the consequences of a mains O The CryoController inside the CryoCooler cabinet has an overheat protection. CryoProbe Installation BRUKER 61 (93)
5.3.1 OOL DOWN A cool-down can only be initiated when the whole CryoProbe System is at room temperature. If a passive warm-up has occurred a few hours ago, the system may not be completely warm yet. In this case, the CryoTool will display Waiting for system to passively warm up.
3. Check phasing of input power. finished. 4. DC control circuit malfunction. 4. Check DC 24 V circuit and fuses. remains O 1. Abnormal static He pressure. 1. Adjust He supply pressure. OWER but D flips back to RIVE CryoProbe Installation BRUKER 63 (93)
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Charge He Compressor Usually, the CryoProbe System is charged with He at the CryoCooling unit and not at the He Compressor. If there’s too little pressure in the He Compressor, i.e. its gauge reads less than 17.5 bar, it is recharged automatically upon cool-down after the preparations have been finished.
ColdHead. UPPLY Open its relief valve compleatly! 1.10 Open V5, V7 and V9 1.11 Switch on the O the D of the ColdHead (which is located on the RIVE back side of the He compressor) CryoProbe Installation BRUKER 65 (93)
B RUKER When cooling down a CryoProbe System for the first time, the flow of cold He may not be adjusted in an optimum fashion for the given environment, e.g. if the Cryo- Cooling Unit was tested at a different mains frequency and voltage settings.
Table 5.2. below. When a substantial amount of He is lost continuously during operation, the Cryo- Controller will give up automatic refilling and warm-up the system. Wait until are lit before refilling He. UNPLUG CryoProbe Installation BRUKER 67 (93)
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Table 5.2. Refill He step action To prevent errors due to other causes, the CryoProbe System should be ready for a cool-down in all other respects. Check if the 1) cooling water supply is active (if applicable); 2) He steel-cylinder is connected and open. Its primary pressure must be larger than 40 bar and its secondary pressure stable at 22-25 bar;...
CryoPlatform 6000000 Relocation This section applies to moving a CryoProbe System to either a storage room or to another NMR spectrometer. If storage in a pressureless state is required (not rec- ommended!), see "Pressure release" on page 70. For disassembling the CryoProbe System, use the reverse order of the installation sequence "Initial setup"...
Lead insulation in CryoCooling Unit The panels of the CryoCooling Unit cabinet contain a lead-enforced polymer foam for maximum sound insulation. Remove the lead/foam insulation. Recycle or dis- pose it according to the local regulations for lead-containing materials. 70 (93) BRUKER CryoProbe Installation...
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Lift the plate. The two indium o-rings make the seal between the ring-shaped plate and the body. Indium must be recycled or disposed according to local regulations. CryoProbe Installation BRUKER 71 (93)
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Relocation of a CryoPlatform 72 (93) BRUKER CryoProbe Installation...
CryoProbe installation or does it have to be switched off? ❢ Is the path for all cables and tubes associated with the CryoProbe System pre- pared (space, cable channels, holes...)? ❢ Is the space below the magnet between shim system bottom plate and floor cleared? ❢...
Check lists ❢ Is there a definite drawing of the CryoProbe System layout for the customer’s NMR lab? ❢ Will all connectors on the Bruker parts fit the supplies in the customers labora- tory (mains, gas, water, ...)? Mind the different national standards.
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User training CryoProbe Installation BRUKER 77 (93)
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Check lists 78 (93) BRUKER CryoProbe Installation...
RUKER tem to the customer’s needs and for preparing its installation. CryoProbe System Site Preparation Manual (P/N Z31553) This manual accompanies the Site Preparation Set which is delivered before oth- er devices are sent. After being installed by the customer, the set provides the in- frastructure for the actual CryoPlatform.
User mount remove Manual CryoProbe CryoProbe P/N Z31551 swap CryoProbes RF Electronics Manual power-down power-up P/N Z31474 CryoProbe System CryoProbe System operate CryoProbe System basic maintenance basic troubleshooting maintenance troubleshooting He Compressor Manual Service Manual 80 (93) BRUKER CryoProbe Installation...
1 mT =10 Gauss 1 Gauss =0.1 mT °C to °F: °F to °C: Ε Φ Ε ⌠ Φ – °F °C °C °F Table B.1. Conversion between °C and °F temperature scales °C °F CryoProbe Installation BRUKER 81 (93)
A cryogenically cooled preamplifier module inside the CryoProbe housing. There is a frequency-specific preamp module for each channel of a CryoProbe. A Cryo- Preamp cannot be separated from its CryoProbe. It always requires an additional external HPPR assembly, the cryo-compatible HPPR CRP. CryoProbe Installation BRUKER 83 (93)
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CryoProbe System A CryoProbe and all components necessary for its operation. CryoTool A software interface for monitoring the CryoProbe System parameters. It runs on a separate laptop or PC. Dump Tool A short gas tube with a silencer. This service tool is used to release the He supply pressure at the joint between He Regulator and CryoCooling Unit before the He steel-cylinder is exchanged.
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A white plastic cap to protect the CryoProbe sample cavity against dirt during transport, testing, or storage. Q factor The quality factor Q is a measure of the efficiency of reactive devices such as in- ductors, capacitors, or resonant circuits. CryoProbe Installation BRUKER 85 (93)
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CryoProbe’s Tuning Adapter. UniTool Software tool on the CryoProbe System laptop to interact with the CryoController or other units. Started the Bruker menu in Windows NT by clicking UniTool. Uninterruptable Power Supply, a kind of battery that compensates for fluctuations and interruptions in the mains.
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‘primary’ water cycle by exchanging its heat to a ‘secondary’ cycle, and a radiator unit that fans the heat from the secondary cycle into the air, usually at the outside of the building. CryoProbe Installation BRUKER 87 (93)
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Glossary 88 (93) BRUKER CryoProbe Installation...
Figure 3.14. Connecting VT sensor cable and VT hose (bottom view) ..47 Figure 3.15. Open the CryoProbe vacuum plug ........48 Figure 3.16. Switching on the He Compressor ........50 Customizing the CryoProbe System Troubleshooting Relocation of a CryoPlatform Figure 6.1.
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Figures 90 (93) BRUKER CryoProbe Installation...
Table 3.13. VT setup ................ 51 Table 3.14. Cool-down ..............52 Table 3.15. Installing the HPPR CRP ..........54 Customizing the CryoProbe System Troubleshooting Table 5.1. Troubleshooting the He Compressor ......63 Table 5.2. Refill He ................ 68 Relocation of a CryoPlatform...
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Tables 92 (93) BRUKER CryoProbe Installation...
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Lastpage End of Document CryoProbe Installation BRUKER 93 (93)
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