Capillaries need to be 0.2-0.7 mm ID, and between 30 - 40 mm in length, as measured from the end of the pin. Larger ID capillaries cannot be sent as they are too fragile. The beam will be centered on the capillary 11 mm from the pin. Capillaries can be purchased from Charles Supper or Hilgenberg.
Ensure
Capillary is completely filled
Material is not loose and moves around inside the capillary
There are no gaps
Capillary is shorter than 40 mm
How to fill and mount a capillaryFill the capillary so that 45 mm of material is in the capillary. Break off the funnel, ensuring the capillary is ~45 mm in length. Insert the broken end of the capillary all the way into the sample pin. Melt a small amount of wax onto the capillary to fix it into position. Wax can be easily melted using a solder iron, or gas stove lighter. Check that the capillary is 30-40 mm, as measured from the end of the pin. The robot will break capillaries longer than 40 mm. Use the cardboard protractor to align the capillary in the pin, and ensure the difference between the sample pin base and capillary is <5°. Capillaries will not align on the diffractometer and be run if the angle is >5°. Ensure that there is sample 11 mm from the end of the pin.
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How to fill and mount a capillaryFill the capillary so that 45 mm of material is in the capillary. Break off the funnel, ensuring the capillary is ~45 mm in length. Insert the broken end of the capillary all the way into the sample pin. Melt a small amount of wax onto the capillary to fix it into position. Wax can be easily melted using a solder iron, or gas stove lighter. Check that the capillary is 30-40 mm, as measured from the end of the pin. The robot will break capillaries longer than 40 mm. Use the cardboard protractor to align the capillary in the pin, and ensure the difference between the sample pin base and capillary is <5°. Capillaries will not align on the diffractometer and be run if the angle is >5°. Ensure that there is sample 11 mm from the end of the pin.
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The PD team can provide information and tips on sample preparation and mounting. We are not responsible for samples that cannot be run due to incorrect mounting, poorly filled capillaries or not enough sample in the capillary.
