1 The world leader in serving science picoSpin 45 & 80 Maintenance, Troubleshooting & LRU’s

2 Key Learning Cartridge Exchange Hints & Tips Troubleshooting LRU’s

3 Capillary Cartridge Exchange Sub-panel Flange

4 Cartridge Exchange Cartridge Maintenance is important aspect of maintaining a picoSpin 45 & 80 Pre-filter sample or use a syringe filter Displace samples with clean solvents Avoid precipitation reactions (important for dissolved solid sampling) o Displace samples using appropriate solvents Leave water, ethanol or acetone in the cartridge for overnight storage Clean cartridges with µL injections of o EtOH, acetone, CHCl 3 or other compatible solvents Replace frit-filter on inlet fitting (outlet fitting does not have a frit-filter) In extreme cases where damage has occurred to the cartridge it will have to be replaced Following are instructions for replacing the cartridge and re-shimming the magnet

5 Cartridge Exchange Step 1 Turn off and unplug the unit 1.Loosen and remove the (4) knurled screws on the corners of the cartridge sub-panel. 2.Screw the threaded end of the aluminum cartridge removal tool into the cartridge flange as shown in Figure 1. 3.Gently pull the sub-panel away from the front panel of the unit a few millimeters and lower it to rest on the U-shaped channel. Figure 1. Installing the cartridge removal tool

6 Cartridge Exchange Step 2 1.Loosen the (2) two hex head screws, as shown in Figure 3. securing the cartridge flange to the magnet using the long- handled hex wrench supplied with the replacement cartridge. The bushings will retain the bolts so that they cannot fall out and become lost inside the unit. 2.Holding the cartridge removal tool with one hand and the cartridge sub-panel with the other, gently remove the cartridge from the spectrometer as shown in Figure 3. Figure 2. Loosening the cartridge screws

7 Cartridge Exchange Step 3 1.Reinstall new cartridge by reversing the above steps. Before inserting the cartridge into the spectrometer, check that it is free of dirt and dust. Blow the cartridge off with clean, filtered air if available. 2.After the new cartridge has been installed the unit can be switched on again. Wait for the magnet temperature to stabilize and the follow the instructions for Shimming After a Cartridge Change. Figure 3. Removing the cartridge from the spectrometer

8 Cartridge Exchange Shimming: 1 Cartridge shimming requires additional steps: Step 1 1.Browse to the autoShim script 2.Check/adjust the parameters in Red 3.Run the script 4.Position your signal within ±500 Hz 5.Run the script again 6.When finished continue to Step 2 ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runChecked linear increments0.05 quadratic increments0 target rms1 pulse width90° from test report acq. Points1000 zero filling8000 rx recovery delay500 us T1 recovery delay8 s bandwidth64 kHz post-filter atten.7 phase correction0 degrees (or any value) exp. Filter0 Hz max plot points400 max time to plot12 ms min freq. to plot Hz max freq. to plot Hz magnitudeChecked

9 Cartridge Exchange Shimming: 2 Step 2 1.Check/adjust the parameters in Red 2.Run the script 3.Position your signal within to ±500 Hz 4.Run the script again 5.Uncheck test run and execute script 6.Continue to Step 3 ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runChecked linear increments0.05 quadratic increments0 target rms1 pulse width90° from test report acq. Points1000 zero filling8000 rx recovery delay500 us T1 recovery delay8 s bandwidth16 kHz post-filter atten.9 phase correction0 degrees (or any value) exp. filter0 Hz max plot points400 max time to plot62 ms min freq. to plot Hz max freq. to plot Hz magnitudeChecked

10 Cartridge Exchange Shimming: 3 Step 3 1.Check/adjust the parameters in Red 2.Run the script 3.Position your signal within to ±500 Hz 4.Run the script again 5.Uncheck test run and execute script 6.Continue to Step 4 ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runChecked linear increments0.01 quadratic increments0.1 target rms1 pulse width90° from test report acq. Points200 zero filling1000 rx recovery delay500 us T1 recovery delay8 s bandwidth4 kHz post-filter atten.11 phase correction0 degrees (or any value) exp. filter0 Hz max plot points400 max time to plot250 ms min freq. to plot Hz max freq. to plot Hz magnitudechecked

11 Cartridge Exchange Shimming: 4 Step 4 1.Check/adjust the parameters in Red 2.Run the script 3.Position your signal within to ±500 Hz 4.Run the script again 5.Uncheck test run and execute script Your instrument is now shimmed! ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runChecked linear increments quadratic increments0.02 target rms1 pulse width90° from test report acq. Points1000 zero filling8000 rx recovery delay500 us T1 recovery delay8 s bandwidth4 kHz post-filter atten.10 phase correction0 degrees (or any value) exp. Filter0 Hz max plot points400 max time to plot250 ms min freq. to plot-2000 Hz max freq. to plot+2000 Hz magnitudechecked

12 Shimming From Scratch In rare situations it may be necessary to shim a spectrometer with no prior knowledge of the Larmor frequency and with no starting shim settings. In this case we use the Search script to find the signal. These steps are required if shimming from scratch: 1.Browse to the search script 2.Check/adjust the parameters 3.Run the script 4.Locate signal 5.Browse to autoShim script 6.Follow Cartridge-change Shimming procedure ParameterValue start frequency46.0 Hz stop frequency43.5 Hz frequency step-8 kHz SNR20 noise window start-4000 Hz noise window stop-1000 Hz pulse width40 us or best 90-deg time acq. Points200 zero filling8000 rx recovery delay500 us T1 recovery delay8 s bandwidth16 kHz post-filter atten.8 phase correction0 degrees (or any value) exp. Filter0 Hz max plot points400 max time to plot12 ms min freq. to plot-8000 Hz max freq. to plot+8000 Hz magnitudechecked

13 Hints and Tips PicoSpin

14 Shimming Do’s and Don’ts DO Do keep your instrument temperature stabilized 24/7 Do start with the signal between Do check the shim daily when in use Periodically when not in use Do perform Maintenance shimming daily when in use Do include quadratic increments for in maintenance shimming Do save named shim files weekly Do include date and magnet temp in name Do capture a screen shot of shimmed FID/spectrum DO NOT Do not use less than 100 iterations when shimming Do not shim when the magnet temperature is fluctuating Do not allow the peak to drift outside the Hz range Do not shim using more than 1000 acquisition points or 400 plot points Other Tips A successful shim will write values to the UI – SAVE THEM You must execute the autoShim script with test run to write values to shim electronics An aborted shim WILL NOT write values to the UI unless autoShim has made improvements

15 Is the picoSpin Properly Shimmed? There are two methods to determine if your instrument is properly shimmed: Evaluate the FID and spectrum signal:  Look for a slow decay of the FID. The intensity of the FID at 250ms should decrease to no less than about half the initial intensity as shown below. Compare spectrum peak height value to the test report:  Upon completion of the shim script, adjust the Tx frequency to position the peak about the same offset as show in y our test report. Then compare the shimmed spectrum peak height to the factory spectrum peak height show in your test report. The spectrum peak height from your shim should be within 5% of the factory spectrum peak height for your instrument or higher.

16 Troubleshooting

17 Troubleshooting The most common troubleshooting service calls arise a lack of understanding of the Tx frequency, and misinterpretation of the FID and spectrum plots. These are the typical reasons underlying a troubleshooting call:  Air in in the RF coil  Poor shim  Misplaced Tx frequency  Sample handling  Computer connection On the following pages are examples of typical troubleshooting scenarios for:  Good FID, good spectrum  Poor FID  No FID, good spectrum  Good FID, no signal  No FID, no spectrum

18 Good FID Both FID and Spectrum suggest a well shimmed instrument Good Spectrum

19 No FID? Good spectrum, but at 0 Hz The spectrum appears good but is placed on 0 Hz Position signal between +200 Hz and Hz

20 Poor FID The FID and spectrum are of poor quality Shim the instrument Poor FID? Poor spectrum?

21 Good FID, No signal? No spectrum Good FID The FID looks good, but the signal is missing from the spectrum Expand the spectrum plot window to the full bandwidth

22 No FID? ? No FID can mean air is in the coil or the Tx frequency is very far off

23 Computer Trouble Cannot establish a connection to the Instrument Is the instrument physically connected to the network or LAN? Is your network adapter properly configured?

24 Sample Handling High back-pressure Blocked filter: o Back flush the filter with a clean solvent Back flush the filter with a clean solvent o Replace the in-line filter assembly Replace the in-line filter assembly Complete loss of signal: Immediately after injection o Injected a bubble, re-inject sample Injected a bubble, re-inject sample During acquisition Sample/solvent is too volatile for the setpoint temperature o Lower setpoint temp. and reshim Lower setpoint temp. and reshim o Use an alternative solvent Use an alternative solvent Loss of signal strength over time Inject shim solvent and run autoShim script. Compare to historical values

25 Least Repairable Units (LRU’s) The capillary cartridge is the only replaceable part in the field that may need to be replaced because of problems. Note part number differences for the picoSpin 45 and picoSpin 80. The following page contains other consumable part numbers.

26 Least Repairable Units (LRU’s)