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SampleCase Training

For your initial training you MUST read all guidelines and view all videos on this page.

Contents

• Warnings and Requirements
  
  
• SampleCase Overview
  
  
• Functional States of the SampleCase
  
  
• Automatic Sample Insertion
  
  
• Resetting the SampleCase
  
  
• Tube Length Limit
  
  
• Manual Sample Insertion (bypassing the changer)
  
  

Warnings and Requirements

 
   The total length of the NMR tube must NOT exceed 9 inches
  

• Inserting longer tubes is possible with bypassing the SampleCase. See Manual Insertion section below.
  
  
• Ceramic spinners may be used in the automatic mode. To ensure reliable ejection, you must have VTU turned ON with a VT gas flow set to 400 LPH before inserting/ejecting. You may consult Manual Insertion on adjustment of the VT gas flow.

SIDE NOTE: Alternatively, you may use the Bruker 500 MHz system in McCourtney, which does NOT have a limitation on the tube length. However, ejecting ceramic spinners with heavy tubes in McCourtney 500 may still be a challenge. You may consult Manual Insertion on adjustment of the VT gas flow to help ejection.

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SampleCase Overview

The Bruker SampleCase sample changer is installed at Bruker 400 MHz and 800 MHz systems in Stepan Chemistry Hall and Bruker 400 MHz automated system in McCourtney Hall. This overview shows you main parts of the SampleCase system

Youtube link

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Functional States of the SampleCase

The SampleCase has three distinct states indicated by a color of its status lights:

1. Steady YELLOW: the sample in the magnet.
   
   
2. Steady GREEN: the magnet is empty, the sample is in a carousel.
   
   
3. Steady RED: error. The SampleCase needs a reset.

Any FLASHING light means "operation in progress". You must stand by and wait till it switches to a steady light.

Youtube link

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Automatic Sample Insertion

The video shows how to insert the sample in a magnet via a SampleCase.

Youtube link

Summary

To insert your sample:

1. put a sample in a changer
2. type
   1. lock off
   2. ro off
   3. sx [your sample position]
      wait to see a steady yellow light
      
      
   4. rsh bbfo-latest

Proceed with locking/tuning/shimming/etc.

To remove you sample and insert a standard sample:

Type:

1. lock off
2. ro off
3. sx 1
   
   wait to see a steady yellow light  
   
   
4. rsh bbfo-latest
5. lock cdcl3

Now you can retrieve your sample from the carousel

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Resetting the SampleCase

If the changer illuminates a red light, you may be able to reset it to clear the error.

Youtube link

Summary:

To reset the changer

1. Make sure there is no obvious trouble like a broken sample stuck in a shuttle.
   
   IMPORTANT:
   If your sample is broken: STOP!
   Log out and report the changer stuck.
   Place "Out of order" note on a computer keyboard.
   
   
2. If the sample is OK and it seems like just a glitch in a changer: push down the red button
   
   
3. wait five seconds
   
   
4. pull the red button up
   
   
5. wait till the changer goes through self-checks and illuminates a steady light
   
   
6. if the light is yellow or green, acknowledge a warning box on a computer screen and proceed with your experiments.
   
   
7. If the light is red, the changer cannot recover from the error.
   Log out and report the changer stuck.
   Place "Out of order" note on a computer keyboard

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Tube Length Limit

NOTE: You MUST always set the tube depth with a depth gauge!

  If your tube is set deeper than required, it will be broken by a changer and may damage the probe!

If your tube is does NOT exceed 9 inches (including a cap), it WILL safely fit in the SampleCase.

This video shows how SampleCase detects excessively long tubes and how to retrieve on "offender" tube.

Youtube link

If in doubt, after you set the tube to a correct depth in a spinner, you may check the height with a ruler. The changer will stop if the tube exceeds 97.5 mm above the spinner:

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Manual Sample Insertion (bypassing the SampleCase)

IMPORTANT: The manual Insertion in SampleCase is allowed on Bruker 400 MHz system in Stepan Chemistry Hall but not Bruker 800 MHz or automatic 400 MHz systems.

For using the manual insertion mode, you have to request an authorization from the NMR staff.

Long tubes exceeding 9 inches may be inserted manually bypassing the changer. Ceramic spinners may also be difficult to eject in automatic mode, therefore, should be inserted manualy. The video shows you the process:

Youtube link

IMPORTANT: Never touch the shuttle with your hand!   

Summary

To insert your sample manually, do this:

Step 1. Eject current sample

1. ro off
2. lock off
3. sx ej
   
   

Step 2. Switch to manual insert mode

1. Turn the blue valve to a horizontal position.
   
   
2. Open Sample Transporter Control screen:
   
   
   1. Switch Lift Mode to Standard BSMS Lift
   2. Click Set
      
      
3. Increase VT gas flow to use with J Young tubes and/or Ceramic spinners:
   
   
   1. Enter edte screen
   2. Set Target Temperature to the value currently displayed
   3. Set Target Gas Flow to 600 LPH
      
      NOTE: Pay attention not to change the Standby Gas Flow! 
      
      NOTE 2:
      Light samples may need lower Target Gas Flow rate (500-400 LPH), otherwise they may not insert (remain seated in the probe)!
      Heavy samples may need higher Target Gas Flow rate (800+ LPH) for the instrument to be able to eject them!
      
      
   4. Turn VTU system ON.
      
      

Step 3. Insert your sample manually

1. Type ej
2. Place your tube in the bore
3. Type ij

 

Step 4.  Returning to SampleCase configuration

After your experiments are finished, you MUST return the instrument to its standard SampleCase configuration.

To do this:

1. Eject your sample:
   1. ro off
   2. lock off
   3. ej
      
      
2. Pick up your sample and leave the bore empty.
   
   
3. Type ij
   
   
4. Open Sample Transporter Control screen.
   
   
   1. Switch Lift Mode to Sample Transporter.
   2. Click Set
      
      
5. Turn Blue Valve to a vertical position.
   
   
6. Return to a standard VT gas flow:
   
   1. Enter edte screen
   2. Turn VTU system OFF.
   3. Set Target Gas Flow to 200 LPH
      NOTE: Pay attention not to change Standby Gas Flow! 
   
   
7. Insert a standard sample:
   1. sx 1
   2. rsh bbfo-latest
   3. lock cdcl3

You may now log out of your account.

 

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