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Nanalysis Corp. This book was carefully produced to describe the setup and operation of the NMReady-60 spectrometers. However, the authors do not claim that the information herein is completely free of errors. Readers are...
Laboratory temperature specification .................... 4 2.3.3 Supplying power to the Spectrometer .................... 4 2.3.4 Networking the Spectrometer ........................ 4 Powering up for the first time ...................... 6 Temperature Stabilization ......................6 Initializing the system ........................6 Regulatory Specifications ......................8 3.0 Acquiring NMR Data on the NMReady-60 ................9 Sample Preparation ......................... 9 NMReady Operation ......................... 9 3.2.1 Quick Select Buttons ........................... 10 3.2.2 Experiment Settings ............................ 12 4.0 Data Processing ........................ 3 7 1D Data Processing ........................ 3 7 4.1.1...
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10.13.2 Specifications ............................99 11.0 Frequently Asked Questions ..................... 100 11.1 General Queries ..........................100 11.1.1 Haven’t benchtop NMR spectrometers been around for years? ........ 1 00 11.1.2 Is the NMReady-60 spectrometer really a true benchtop NMR spectrometer? .. 1 00 11.1.3 How does it work? .......................... 1 00 11.1.4 How stable is the NMReady-60? Can I use signal averaging to improve the signal-to- noise ratio? .................................. 1 00 11.1.5 Can I look at flowing Samples? ...................... 1 01 11.1.6 Should I power down the spectrometer when I go home at night? ........ 1 01...
Frequency. w = g The principal difference between the NMReady-60 and higher field superconducting magnets is the method used to generate the static magnetic field. Instead of generating a magnetic field using a cryogenically cooled superconducting solenoid, the NMReady uses carefully engineered permanent rare-earth magnets.
1.3 Using this Manual This document is a resource to facilitate the incorporation of the NMReady-60 into routine laboratory use. This manual contains: (1) instructions for installing the spectrometer (section 2) (2) specific details of the operational features of the NMReady interface (section 3 –...
NMR applications, it requires the use of very precise mechanical and electrical means. To ensure that these systems are not damaged upon shipment, the NMReady-60 is transported in a wooden crate and labeled as fragile. This helps to ensure that the unit is handled with care and that the instrument remains at the correct orientation.
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More information can be found regarding networking in section 6.4.2.2. Please note that Nanalysis Corp. will not be able to provide remote updates/customer support if you are unable to connect to the network. However, we can still provide assistance. Please submit offline inquires for customer support via email at service@nanaylsis.com.
2.4 Powering up for the first time Once the location of the NMReady-60 has been designated, the first step is to plug the system either directly into the main power or into an uninterruptable power supply (UPS) that is plugged into the main power line.
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There is no need to remain in front of the spectrometer for the full duration of the installation process. Intermittent supervision, however, is recommended. While there is no need to contact Nanalysis’ customer service about this process, we do recommend contact us once it’s complete so it’s performance can be assessed.
H and either F or P as was specified by the user at the time of purchase. Unless requested the NMReady-60 uses a standard deuterium ( H) Lock Nucleus, but there is also a proton lock ( H) feature.
Custom and using the pop-up keyboard to input the exact number of scans you desire. The scans in the list are multiples of four as the NMReady-60 uses a phase alternating pulse sequence (PAPS), however it is not necessary to customize to a multiple of 4.
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The appearance of cross peaks is evidence of proximity of the spins within the molecule. There are many COSY variants described in the NMR literature. The NMReady-60 runs a standard COSY-90 (i.e., X=90 in figure 2) and displays and stores its data in magnitude mode.
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8. It can also be helpful to select 6 or 8 dummy scans to help reach a steady state magnetization for the sample. The NMReady-60 HSQC program includes an optional “BIRD” (BIlinear Rotation Decoupling) filter as part of the further suppression of the spurious...
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~ 150 Hz coupling. For the NMReady-60 HMBC pulse program, the purge pulse is used to suppress the resonances from protons bonded to C. The length of that Purge Pulse , as well as the Purge Amplitude can be optimized as desired.
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The spin-spin, or transverse, relaxation time, (T ) quantifies the time required for the bulk magnetization to dephase after an RF pulse due to interactions with other spins. NMReady-60 spectrometers provide three types of experiments to measure T relaxation in a sample. The T...
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Start Width to the End Width in the defined by the Number of Steps . The NMReady-60 uses the 180° null as the point of reference so End Width should be greater than twice the expected 90°...
4.1.3.1 Phase The NMReady-60 has onboard tools to adjust the spectrum. The Phase can let you modify the spectrum either automatically or manually using the onscreen controls. To phase automatically, simply press Auto. The manual phase adjustment is performed using on-screen sliders by either dragging the cursor or tapping on the lighter green side rail.
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4.1.4.3 Chemical Shift Reference The NMReady-60 monitors the deuterium channel to lock at the beginning of each scan to ensure that there is a minimal drift. This process affords reasonably accurate chemical shifts. However, to ensure that the observed chemical shifts are precise, they can be further referenced upon workup if desired.
5.0 Saving and Exporting Data After data processing is complete, the data can be saved directly to the NMReady-60 (as either a dx, pdf or a png file, see section 6.3.2 and 5.1), exported to a network folder or sent to a network printer once those features have been enabled.
User Manual 6.0 Nanalysis User Interface: The Task Bar The main screen of the NMReady-60 user interface is divided into two sections from which the spectrometer can be operated. 1) The task bar is located at the top of the main screen and can be accessed from most windows in the user interface.
6.2.1 Temperatures The NMReady-60 tracks the temperature of the: (1) electronics board; (2) magnet; and (3) enclosure. Fluctuations are expected within the boards and enclosure, but the magnet temperature should remain constant.
6.2.7 Messages When a warning appears on the Status button, the NMReady-60 will provide a recommendation to improve the overall performance of the instrument. These are based on numerous measurements of system parameters and performance characteristics.
6.2.8.3 Full Finally, a full shim performs a full electronic tune-up. For the NMReady-60 this shims down to fourth order gradients. It takes approximately 20 minutes to complete and will be recommended by the system status function every 24 hours.
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Please note that based on the file type, only the relevant buttons will be enabled (e.g., .png files cannot be loaded back into the NMReady-60 processing window for further processing and therefore Load will remain greyed out).
The set-up of this folder will be further discussed in section 6.4.2.2. To export a file to a USB drive, the USB key must be inserted into the NMReady-60. This will render the Export to USB and Eject USB keys active. Next, select the desired file and touch Export to USB button.
On or Off by toggling the button, similarly one can choose to share generic usage statistics with Nanalysis with an On or Off toggle. There is also an option to skip the pre scan delay. It is recommended that the user does not use this.
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Any time the screen has gone to sleep, touching it will turn it back on. 6.4.2.2 Network Settings As discussed in section 2.3.4 connecting the NMReady-60 to a network enables: (1) access to a network folder for exporting data; (2) using a network printer; (3) software updates; and (4) advanced customer service.
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This functionality is not included in the basic instrument package, but if enabled can be easily accessed from Setup è System è Network è Remote. If you are interested in more information about this functionality, please visit the product page (Nanalysis.com/nmready-connect), login to the developer website (Nanalysis.com/developer-zone) or notify your Nanalysis representative.
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The desired printer can be selected by highlighting it and then hitting Add. Again, to ensure the printer is properly configured, the NMReady-60 must be restarted after the printer installation. To restart, click the power button on the right-hand side of the NMReady-60, chose Restart and wait for the instrument to reboot itself.
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Date/Time This tab enables the date and time of the NMReady-60 to be changed depending on the time zone you are in. If you are without a network and find that the time is not correct, it can be modified by hour, minute and second as is necessary.
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To restart, click on the power button on the right-hand side of the NMReady, choose Restart and wait for the instrument to reboot itself. The NMReady-60 is defaulted to lock on deuterated solvents, although non-deutero options are also available.
The Shim History Tab displays a chronological list of the most recent shims that were applied to the NMReady-60. Both auto and manual shims are included in this list. To re-apply an old shim set, select the desired entry in the list and touch the Load Shims button. It is rare that recalling a shim set from the shim history is required.
The Service tab contains very powerful operations that govern the configuration of the NMReady-60 and is primarily intended for use by Nanalysis service personnel. It can be restricted by a separate PIN access than the Setup panel to prevent unauthorized users from accessing this screen. There are four subtabs (1) Maintenance;...
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6.4.6.2 Tests The Tests tab is meant primarily as a diagnostic tool for Nanalysis Customer Service representatives to assess the radiofrequency system, the instrument, and temperature performance over time. This allows them to perform diagnostic testing using the Shim Test, Stability Test, RF Self Test 1, RF Self Test 2, System Test and OS Test.
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6.4.6.3 Updates The Updates tab is meant to simplify software and firmware updates. Nanalysis will notify you when it is necessary to update the software. It can be done either through the Ethernet network connection, or by putting the updated files on a USB key. When a software update is selected, the software will automatically detect any versions that are higher than that being run on the spectrometer.
OS. 6.5 Help The Help Panel is present in virtually every window of the NMReady-60 interface. It can be used to offer assistance for proper operation of your spectrometer, as well as for diagnosis and fixing issues that may arise during routine use.
Share my screen with customer service is activated. The Stop sharing option will remain in the top right-hand corner of the screen for the entire duration in the spectrometer is connected to the Nanalysis service network. To terminate the connection at any time, simply press Stop sharing.
If Queuing is enabled on a spectrometer an orange ‘+’ will appear in the right-hand corner of the Go button. To set-up a queue: 1. Select the desired Observe Nucleus (choices depend on which NMReady-60 model you have) Lock Nucleus ( H or H lock), Solvent, and Experiment on the front screen.
7.2 Installation Qualification and Operational Qualification (IQ/OQ) Adherence to regulatory compliance is critical in many work places, especially with contract research and manufacturing organizations (CRO and CMO). Nanalysis offers an optional software package for Installation Qualification (IQ) and Operational Qualification (OQ). These packages test the instrument’s performance on initial siting, as well as in routine workflow to help validate result integrity over time.
It is used to lock and provide evidence of B homogeneity and instrument performance. The NMReady-60 is preset with basic shimming protocols (e.g., quick, medium and full, see section 6.2.8 and more advanced auto-shim (section 6.4.4) and manual shim (section 6.4.5) options.
8.4.5 Progress Ring This has been introduced to the NMReady-60 so the user has an easy visual identification of the progress of an experiment and the status of the instrument. The process ring can be disabled in the Setup è...
The colour blue indicates that the NMReady-60 is still in use, whether that means it is shimming or collecting data. A green light ring means that the NMReady-60 is ready for use. A red light ring means there was an error and the spectrometer requires some diagnostic maintenance.
10.0 AUTOsample-60 10.1 Introduction The AUTOsample-60 is designed as an accessory to the NMReady-60 family of benchtop spectrometers, to improve workflow and allow for automated sample tube changing. The AUTOsample-60 can help automate NMR spectrometer experiment workflow when more than one sample is used.
To install the AUTOsample-60 onto your NMReady, first remove the sample tube from the NMReady, grasp the AUTOsample-60 by its sides, and place it onto the round top cover of the NMReady-60. The top cover of the NMReady-60 mates to the bottom of the AUTOsample-60 and locates the two instrument pieces together.
AUTOsample-60 and use it to change to the desired tube. Note that the NMReady-60 must have the AUTOsample-60 feature enabled in its license. When the AUTOsample-60 feature is enabled on the NMReady, the front screen will have a button for “Tube Number”.
To queue experiments using different tubes, the procedure is similar to queuing (section 7.1), but the user must also specify the Tube Number: 1. Select the desired Observe Nucleus (choices depend on which NMReady-60 model you have) Lock Nucleus (...
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AUTOsample-60 tube warmer 4. The NMReady-60 will perform the current experiment(s) on the first NMR sample 5. After the current experiment is completed, the sample is moved back to its original location in the carousel 6.
User Manual 10.9 Standby Shimming The NMReady-60 has a standby shimming protocol that can be used to maintain optimal line shape through times when the instrument is not being used. The Standby Shimming button is in the upper left-hand corner of the main screen ( ).
All of the components are packaged in a single enclosure. 11.1.4 How stable is the NMReady-60? Can I use signal averaging to improve the signal-to- noise ratio? The NMReady uses a deuterium (or proton) internal lock to stabilize the transmitter position in the magnetic field.
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11.1.5 Can I look at flowing Samples? The basic design of the NMReady magnet is compatible with custom sample-flow systems! We offer a flow accessory, please inquire with your local Nanalysis representative about the NMReady-flow to use your NMReady as on online NMR detector.
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2 minutes in the magnet before acquiring NMR data on the sample. 11.2.4 What experiments can I do? All the NMReady-60 instruments are configured with a standard one-pulse 1D experiment, a nutation experiment for pulse calibrations, standard T...
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