Recording spectra during Phase 2 reopening of the NMR core lab

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Justin Douglas (justindouglas@ku.edu) – KU NMR lab v1.0 6/3/20

Starting on Tuesday, June 9th, the NMR core lab will initiate phase 2 of the reopening plan.  This phase is named the “limited access” stage.  As a reminder, the objective of the NMR lab reopening plan is to:

  • To reduce the possibility that shared lab space in the NMR core lab becomes a transmission hotspot.
  • To protect the health and well-being of the staff of the NMR core lab who must perform essential weekly maintenance on the instruments.

During the “limited access” phase, only one user per PI will be permitted to enter the open-access NMR labs in ISB B143 and SBC 1004.  PIs please designate one graduate student or post-doc for access to the NMR lab by Friday June 5th. This individual will be responsible for running or submitting all samples for his/her group from June 9th to June 22nd

Because of differences in the physical space and capabilities of the open-access instruments, there are slightly different protocols for London, BigSur and Siena.  Please read carefully the protocol below for each instrument.

A note on gloves:  The NMR core lab has ordered (but not yet received) a small supply of gloves.  Given the difficulty in procuring PPE at this time, our supply must be reserved for the NMR lab staff.  Moreover, we are concerned about the potential for chemical contamination of shared keyboards, spinners and the depth gauge if synthetic chemists touch these items with gloves from their lab (to say nothing of any PPE supply issues these groups may be having).  Hence, the NMR core lab workstations will continue to be GLOVE-FREE.  It is strongly recommended that you wash your hands after visiting the NMR core labs.  In ISB there are bathrooms at either ends of the hallway outside the lab.  In SBC there is a bathroom directly across the hall from the lab.  In addition, there are stations with hand sanitizer located in both buildings.

Protocol for BigSur (400 MHz in SBC 1004)

Because there is no card reader, the door will remain unlocked at all times.  Hence, users are on-their-honor to follow the protocol below.  In addition, because there are relatively fewer users on West Campus, relative to the Central District, specific timeslots for subsets of users will not be required.

#1) Look into the lab and make sure no one else is in the room!  Do not enter the room if someone else is present.  Be sure to practice proper social distancing in the hallway outside the lab if there is a queue.

#2) When you are certain the lab is unoccupied, enter and load/unload samples on the BACs using the normal SOP for IconNMR.  The following rule will be implemented keep the queue turning during common working hours so that this instrument will continue to be used for routine characterization in synthetic chemistry:

Between the hours of 10 AM and 5 PM there is a maximum of 5 experiments per group at any given time.  If the number of samples/experiments exceed five, leave a gap on the autosampler greater than or equal to the number of samples you have submitted to allow other groups time to record data.

For example, if you have 10 samples to submit for the “PROTON” experiment, you can put the first five in slots 1 through 5, then you must skip slots 6 through 10 to leave these available for other groups.  You can continue with slots 11 through 15.  If there are not enough slots on the autosampler, do not add any additional samples.  You must submit to Siena (see below).  Do not wait in the lab for slots to open.

Between the hours of 7 AM (when the building opens) to 10 AM and 5 PM to 10 PM (when the building closes) no restrictions will be applied, but it is imperative that experiments do not extend into the 10 AM to 5 PM window!

Note, the lab will also be closed as needed by the staff for cryogen fills and cleaning surfaces.

#3) After leaving the lab, immediately wash your hands in the bathroom across the hall or use the hand sanitizer station adjacent to the bathrooms.

Protocol for London (400 MHz in ISB B143)      

The major challenge with London is that the autosampler ONLY has 24 slots.  Hence, access to London is restricted to time-sensitive experiments required for routine characterization in synthetic chemistry.  All other experiments must be submitted to Siena (see below).  A time limit of 30 minutes per user per day will be enforced by the IconNMR software.

#1) It is difficult to see into the lab from the front doors, but down the main hallway, there are large glass panels that allows you to see the entire lab.  Check these panels and make sure no one is in the lab.  Do not enter if someone else is present!  Be sure to practice proper social distancing in the hallway outside the lab if there is a queue.

#2)  When you are certain the lab is unoccupied, enter and load/unload the samples on the NMRCase autosampler on London using the normal SOP for IconNMR. 

The following rule will be implemented keep the queue turning during the day so that this instrument can continue to be used for routine characterization in synthetic chemistry:

Between the hours of 10 AM to 2 PM and 3 PM to 7 PM there is a maximum of 3 experiments per group at any given time.  If the number of samples/experiments exceed three, leave a gap in the autosampler greater than or equal to the number of samples you have submitted to allow other groups time to record data.

For example, if you have 6 samples to submit for the “PROTON” experiment, you can put the first three in slots 1 through 3, then you must skip slots 4 through 6 to leave these available for other groups.  You can continue with slots 7 through 9 if these are available.  If there are not enough slots on the autosampler, do not add any additional samples.  You must submit to Siena (see below).  Do not wait in the lab for slots to open.

No access to the lab will be allowed between 9-10 AM and 2-3PM to allow NMR lab staff an opportunity to perform cryogen fills, clean surfaces and load Siena.

Between the hours of 7 AM (when the building opens) to 9 AM and 7 PM to 10 PM (when the building closes) no restrictions will be applied at this time, but time used will count against the allotted 30 minute of NMR time.  Also, it is imperative that experiments do not extend into the 10 AM to 6 PM window!

#3) After leaving the lab, immediately wash your hands in the bathroom down the hall or use the hand sanitizer stations.

 

Protocol for Siena (500 MHz with cryoprobe in ISB B143)

The NMR core lab staff highly encourage users to submit all non-time sensitive samples to Siena, the 500 MHz with cryoprobe in the basement of ISB.  The NMR lab staff will control this queue and there will be no restrictions for this instrument. 

To keep the carousel turning, the NMR core lab staff will load Siena twice per day between 9-10 AM and 2-3 PM.  For users from West Campus, there will be two daily pickups of samples from SBC room 1004 (at approximately 8:45 AM and 1:45 PM).     

#1) Whether you submit samples in SBC room 1004 or ISB B143, be sure to look into the lab and make sure no one else is in the room!  Do not enter the room if someone else is present.  Be sure to practice proper social distancing in the hallway outside the lab if there is a queue.

#2)  When you are certain the lab is unoccupied, enter and place the samples in the clearly marked “IN RACK” for Siena.  In ISB B143, this rack is on the shelf to the right of the interior double doors.  In SBC 1004, this rack is roughly eye-high on the shelf to the right, just as you enter.

Use the form at

https://docs.google.com/spreadsheets/d/1zHxpU9IOez84MrX2FfxOGFThqBXBWMiZga20jpAC0m0/edit?usp=sharing   

so that the NMR lab staff has the information necessary to add the sample to the queue.

 

Cleaning and disinfecting of the lab

Though there is evidence to suggest that surfaces are not the major mode of transmission of COVID-19, the NMR lab staff will clean shared items such as the mouse and keyboard of the workstations, spinners, the depth gauges, the desk surface and door knobs approximately once per day with an ethanol and/or bleach solution.


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