Sample tubes and caps for magnetically oriented...

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Sample tubes and caps for magnetically oriented samples. 1

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Page 1: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Sample tubes and caps for magnetically oriented

samples.

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Page 2: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Materials for generating sealed bicelle samples for NMR.

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• Our standard bicelle sample is housed in a 5 mm NMR tube.

• New Era NE-RG5-15-FB.

• Samples are capped using a rubber stopper from a syringe.

• BD 1ml Sub-Q Syringe

Page 3: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Syringe components.

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• The component parts of the BD syringe.

• BD 1ml Sub-Q Syringe

Page 4: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Syringe components.

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• The rubber stopper at the end of the syringe plunger is

removed and used as a sample cap.

Page 5: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Sample holder.

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• A pipet tip is used as a sample holder during the capping

process.

Page 6: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Fill the sample.

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• Fill the NMR tube with the sample, water in this example.

The NMR tube is filled with

150 – 180 uL of sample as

desired, leaving space at the

top for the cap to insert

Page 7: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Pierce the cap.

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• With great care, pierce rubber cap with syringe needle, this

will create a perforation through which air will vent during the

capping process. Caution, the syringe needle is sharp!

Page 8: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Insert cap.

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• Insert the cap with the open (hollow) side down. Start

insertion with a pinch and a twist, being careful not to break

the NMR tube.

Page 9: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Insert cap.

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• Push down gently from the edges of the cap in an action that

allows the vent perforation to allow air to escape while the cap

is being pushed down evenly.

Page 10: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Capped sample.

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• Here you can see that the sample is capped with only a very

minimal air bubble trapped in the sample. With care, and

starting with a level meniscus, a sample completely free of

trapped air can be achieved.

Page 11: Sample tubes and caps for magnetically oriented samples.nmrresource.ucsd.edu/probetechnology/CappingSamples.pdf · 2016. 11. 12. · • The rubber stopper at the end of the syringe

Ready for NMR!

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• As a last step, seal off perforation by wrapping over the cap

with parafilm, and/or teflon tape.

• If an air bubble develops over time, it can be removed by

allowing the air to rise into the hollow portion of the cap, then

further inserting the cap as before, effectively driving out the

air through the vent perforation, then re-seal.