1 The world leader in serving science picoSpin 45 & 80 Pre-installation, Site, Safety and Installation 2 Key Learning Pre-installation check list Site & Safety Information Installation check list Installation and Setup Sample Injection Shimming Measuring SNR Summary 3 Pre-installation Checklist 4 Site and Safety Information Guide 5 Installation Checklist 6 Installation and Setup 7 Out of Box Setup for picoSpin 45 and 80 1.Unpack the picoSpin 2.Remove the shipping restraint* 3.Make power connections 4.Turn on the picoSpin unit 5.Connect the Ethernet cable 6.Make network adapter modifications 7.Using Firefox, browse to picoSpin 8.Browse to theTemperature page 9.Adjust set-point to 42C** and submit 10.Let the picoSpin unit warm up Controlling the picoSpin using a direct/static connection to the computer. ** The pS-45 is shipped with a set-point temperature of 42C RJ-45 Ethernet Connector RS-232 Port Power Connection +12 V: VAC ON/OFF Switch * The picoSpin 80 system does not have a shipping restraint 8 Network Adapter Settings for Direct Connection Windows 7 Navigate to the networking configuration: 1.Select Control Panel Network and Internet Network and Sharing Center 2.Select Change adapter settings 3.Select Local Area Connection 4.Select Internet Protocol Version 4 (TCP/IPv4) 5.Click Properties 6.Select Alternate Configuration 7.Select User configured 8.Type in the following fields: IP address: Subnet mask: Click OK, Click Close Windows XP Navigate to the networking configuration: 1.Select Control Panel Network Connections 2.Select Local Area Connection 3.Click Properties 4.Select Internet Protocol Version (TCP/IP) 5.Click Properties 6.Select Alternate Configuration 7.Select User configured 8.Type in the following fields: IP address: Subnet mask: Click OK, Click Close, Click Close * Other Operating Systems 9 picoSpin spectrometer including Pre-fitted capillary cartridge 12 VDC modular power supply Power cord Ethernet cable Accessory packet Disposable syringe and needle Port plugs Inlet and outlet port adapters Inline filter Contact details 12 month licence to Mnova Installation and Setup guide Documentation DVD and factory test report Whats in the Box 10 Documentation Documentation for the picoSpin 45 and 80 is available on the PSE Website Available documents Software revision: (current release) o User Guide User Guide o Installation and Setup guide Installation and Setup guide o FAQ FAQ o Site and Safety Information Site and Safety Information o Product Warranty Product Warranty Accessory Kits for 1-16 inch fittings o picoSpin Teaching Kit for 1-16 inch Fittings picoSpin Teaching Kit for 1-16 inch Fittings o picoSpin Laboratory Kit for 1-16 inch Fittings picoSpin Laboratory Kit for 1-16 inch Fittings o picoSpin Cartridge Maintenance Guide picoSpin Cartridge Maintenance Guide 11 Factory Test Report The factory Test Report provides default settings, serial numbers, shim values and images of FIDs verifying and certifying that the shipped picoSpin spectrometer as having met factory specifications. Shimmed FIDShim SettingsSNR Test Report 12 Web Browser Interface There are four main pages of the interface: Run Files Temperature System And two menu buttons: scripts shims Accessing the web browser user interface (UI) Using Firefox point your web browser to the unit's IP address The IP address is shown on the front-panel LCD display at power-up 13 System Page Preferences Run Name o Enables saving of named runs Expert Mode o Controls the starting condition of the show more/show less button in scripts Display Plots at Right o Controls position of the data plots wrt to parameters list Settings Set the default IP address when DCHP is not available (OS reboot required) Set Date & Time (used for labeling saved runs) Set Time Zone Version Currently installed software and firmware versions Restart Restart the web server CPU System Update Update system software and web browser interface Use only when update file and installation instructions are received 14 The Temperature page UI provides access to the control interface to magnet temperature controller Plot Features Displays latest 6 hours of data Data refresh every 30 seconds Automatic Y-axis re-scaling Plot Types Magnet temperature plot o Magnet temperature sensor data displayed in Celsius ( C) o Magnetization dependence on magnet temperature Ambient/case temperature o Room temperature + heated dissipated from inner-enclosure electronics Heater output o +10 volts; 16-bit, 0 to (2 16 ) full scale Controller Button Magnet set-point temperature maximum setting 45/60 C (high temperature unit). Adjustable PID controls Heater On/Off switch Closed loop On/Off switch Controller settings are not changed until the Submit button is pushed. From Ambient, 30 min 2 hours ( picoSpin 45) and 60 min 4 hours (picoSpin 80) is required to reach stabilized magnet set-point Temperature Page The picoSpin 45 default temperature set-point is 42C The picoSpin 80 default temperature set-point is 36C 15 Files Page The Files page UI provides access to data, settings and scripts stored on the instrument for download and reuse. Run Data o onePulse experimental parameter and spectrum archive o autoShim parameter archive o Individual file download and named, compressed archiving Shims o Saved shim files Scripts o Factory default experiment scripts Notice: Parameters dont automatically update between pages in picoSpin software version and prior. Record and/or copy your Tx frequency before browsing from one script to another. 16 Run Page The Run page UI provides access to pulse sequence experiment scripts onePulse autoShim search Experiment scripts are selected via the scripts button and values are adjusted in the parameter fields according to script and experiment onePulse script fields 1.Execute script 2.Expert/basic mode 3.Parameter fields 17 Sample Injection Samples are introduced into the capillary cartridge by injection picoSpin 45 & 80 spectrometers are shipped with an Accessory Packet containing: 1- 1 mL disposable polypropylene syringe gauge blunt tip dispensing needle 2 PEEK plugs 1 Syringe Port 1 Inline Filter 1 Disposable 0.22 m syringe filter Classroom accessory kits replicate the Accessory Packet included with every order & include syringe filters. 18 Sample Injection Attach the drain tube 1. Insert the tip of the drain tube assembly into outlet fitting 2. Finger tighten PEEK nut by applying gentle pressure 3. Place the end of drain tube into small waste container Inject the sample 1.Using a polypropylene syringe 2.Draw up 40 L of the sample solution 3.Draw solution slowly to avoid bubble formation 4.Insert needle into inlet fitting 5.Finger tighten PEEK nut by applying gentle pressure 6.Gently press the syringe plunger to inject sample 7.Monitor drain tube to ensure residual bubbles have been purged 8.After injection replace fill and drain tubes with PEEK plugs 19 Sample Injection Inject water for shimming 20 The autoShim Script Magnets Field Z Shim Field Z BoBo Z Shimming is a process of optimizing the magnetic field homogeneity over the sample volume of the RF coil. Shimming is accomplished by passing small DC currents through coils. The picoSpin-45 has 9 shim coils: 3 for generating linear gradients 5 for generating quadratically varying fields 1 for generating a uniform field The autoShim script uses a search algorithm to find optimal shim settings. 21 Shimming Q&A When to check the shim quality of the picoSpin? When instrument is first turned on and after temperature stabilization When instrument is power cycled for more than a few minutes When the magnet set-point temperature is changed Once daily (during normal operational use) Are there different types of shim procedures? Yes, there is: Maintenance shimming Set-up shimming Cartridge-change shimming Shimming from scratch Are the shim procedures the same? No, some shim procedures are complex and take longer How often should one shim the picoSpin? Maintenance shimming should be performed daily Do I need to shim after changing the sample? No, loss of shim will not occur upon changing samples What sample requirements is there for shimming? Shimming is performed on a water Acetone and cyclohexane can also be used autoShim Script Parameters **Detailed Parameter Fields Description 22 Shimming picoSpin 45 Shimming is a critical step in maintaining the picoSpin-45 in top operational form This table shows typical autoShim script parameters for the picoSpin 45 The minimum factory specifications for a properly shimmed picoSpin 45 are as follows: SNR>1000:1 single pulse on water. FWHM line width of >40 ppb. Good shims yield High resolution spectra High signal sensitivity Bad shims yield Low signal resolution Reduced signal sensitivity ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test run linear increments0.005 quadratic increments0.02 target rms1 pulse widthbest 90 from test report acq. points1000 zero filling8000 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 magnitude 23 Finding the Signal Set-up shimming picoSpin 45 Find your signal using Zoom Search Step 1: Find the signal 1.Browse to the autoShim script 2.Check/adjust the following parameters 3.Run the script with test run checked 4.Position your signal near 0 Hz Moving the Tx frequency MHz 2.9 100 KHz 3.3 10 kHz 4.7 1 kHz 5.0 100 Hz 6.2 10 Hz 5.If signal is at Hz then Add Hz to Tx frequency If the signal is at 2200 Hz then Add Hz to Tx frequency Run the script again to verify peak position is near 0 Hz. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test run linear increments0.01 quadratic increments0 target rms1 pulse widthbest 90 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 Magnitude 24 Finding the Signal Set-up shimming picoSpin 45 Step 2: Find the signal 1.Adjust the parameters in RED 2.Run the script with test run checked 3.Position your signal between Hz Moving the Tx frequency MHz 2.9 100 KHz 3.3 10 kHz 4.7 1 kHz 5.0 100 Hz 6.2 10 Hz 1.If signal is at -700 Hz then Add -950 Hz ( MHz) to the Tx frequency If the signal is at 700 Hz then Add +450 Hz ( MHz) to the Tx frequency Run the script again to verify the peak position is between Hz. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test run linear increments0.01 quadratic increments0 target rms1 pulse widthbest 90 from test report acq. points1000 zero filling8000 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 Magnitude 25 Finding the Signal Set-up shimming picoSpin 45 Step 3: Coarse shimming 1.Adjust the parameters in RED. 2.Run the script with test run unchecked. 3.When completed, check test run and execute the script once again. This will take approximately 20 min Terminology 1.Iteration one complete Simplex loop 2.Cycle pulse within an iteration 3.Increment step size On average the algorithm will make 1.4 cycles/iteration when running linear increments only. Do the math: At T1 = 8s, 1000 pts and 1.4 cycle/iteration. (8s )*1.4*120 = 20 minutes. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runUNCHECKED linear increments0.01 quadratic increments0 target rms1 pulse widthbest 90 from test report acq. points1000 zero filling8000 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 Magnitude 26 Finding the Signal Set-up shimming picoSpin 45 Step 4: Fine shimming 1.Recheck the test run box 2.Position your signal between Hz 3.Adjust the parameters in RED 4.Run the script 5.When completed, check test run and execute the script once again. This will take approximately 33 min On average the algorithm will make 1.4 cycles/iteration when running linear increments only. 6.Upon completion, wait 30 seconds, recheck the test run box and run the script. 7.Evaluate your shim by comparing the spectrum peak height reported at the bottom of the script to the value shown in the test report. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runUNCHECKED linear increments0.005 quadratic increments002 target rms1 pulse widthbest 90 from test report acq. points1000 zero filling8000 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 Magnitude 27 Shimming picoSpin 80 Shimming the picoSpin 80 follows the same process as the picoSpin 45 but with slightly different parameters. See the following pages for details. This table shows typical autoShim script parameters for the picoSpin 80 The minimum factory specifications for a properly shimmed picoSpin 80 are as follows: SNR>4000:1 single pulse on water. FWHM line width of >20 ppb. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test run linear increments quadratic increments0.005 target rms1 pulse widthbest 90 from test report acq. points1000 zero filling8000 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 magnitude 28 Finding the Signal Set-up shimming picoSpin 80 Step 1: Find the signal 1.Browse to the autoShim script 2.Check/adjust the following parameters 3.Run the script with test run checked 4.Position your signal near 1000 H Moving the Tx frequency MHz 2.9 100 KHz 3.3 10 kHz 4.7 1 kHz 5.0 100 Hz 6.2 10 Hz 1.If signal is at Hz then Add Hz ( MHz) to the Tx frequency If the signal is at 7000 Hz then Add Hz ( ) to the Tx frequency Run the script again to verify peak position is near 0 Hz. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test run linear increments0.01 quadratic increments0.2 target rms1 pulse widthbest 90 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 Magnitude 29 Finding the Signal Set-up shimming picoSpin 80 Step 3: Coarse shimming 1.Adjust the parameters in RED. 2.Run the script with test run checked. 3.Position your signal to approximately 1000 Hz 4.Uncheck the test run box and allow the script to run to completion 5.Recheck the test run box and run the script again. 6.Verify that the FID amplitude at 62 ms is at least 0.5 (preferarably >0.75) of the initial amplitude. 7.Adjust the Tx frequency to poition the peak near 250 Hz 8.Run the script again to verify the peak position between Hz. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test run linear increments0.01 quadratic increments0.2 target rms1 pulse widthbest 90 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 Magnitude 30 Finding the Signal Set-up shimming picoSpin 80 Step 4: Fine shimming 1.Adjust the parameters in RED 2.Run the script 3.When completed, check test run and execute the script once again. This will take approximately 33 min On average the algorithm will make 1.4 cycles/iteration when running linear increments only. 6.Upon completion, wait 30 seconds, recheck the test run box and run the script. 7.Evaluate your shim by comparing the spectrum peak height reported at the bottom of the script to the value shown in the test report. ParameterValue tx frequencyproton Larmor frequency (MHz) max iteration100 test runUNCHECKED linear increments quadratic increments0005 target rms1 pulse widthbest 90 from test report acq. points1000 zero filling8000 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 Magnitude 31 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. 32 Shimming Dos and Donts DO Do keep your instrument temperature stabilized 24/7 Do start with the signal between Do check the shim daily when in use o 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 33 Measuring SNR Using the search Script peak height baseline RMS noise Signal-to-noise ratio (SNR) is a measure of the sensitivity of an instrument With the picoSpin we can measure SNR using the search script 34 Search Script 1. Navigate to the search script 2. Check/adjust the following parameters 3. Shift your Tx frequency so that it appears at +600 Hz Hint: you can read the signal position in the text window below. 1. Once your signal is positioned wait 30 seconds and run the script 2. Make a note of your SNR ParameterValue start frequencyproton Larmor frequency (MHz) stop frequencyproton Larmor frequency (MHz) frequency step-10 kHz SNR10 noise window start-800 Hz noise window end-400 Hz pulse width40 us or best 90-deg time acq. Points4000 rx recovery delay500 us T1 recovery delay8 s bandwidth4 kHz post-filter atten.11 phase correction0 degrees (or any value) exp. filter0.5 Hz max plot points4000 max time to plot1000 ms min freq. to plot-100 Hz max freq. to plot+800 Hz live plot Magnitude 35 Calculating Theoretical SNR 600 = manufacturing SNR spec (wrt H 2 O) LW = Signal line weight 1/2 = 2 water protons M i = sample molarity 1/55 = molarity of water N = number of scans 600 = manufacturing SNR spec (wrt H 2 O) LW = Signal line weight 1/2 = 2 water protons M i = sample molarity 1/55 = molarity of water N = number of scans 36 Summary
