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Coastal and Marine Geology Program
Woods Hole Field Center

Geochemical Sediment Analysis Procedures, Open-File Report 02-371


DRYING SAMPLES - Oven or Freeze Dry (preparation)

OVEN DRYING SAMPLES
Materials Required:
  • Oven
  • Sample to be dried
Oven Drying Preparation; link to larger image

Several ovens are available for use:

  • THELCO in XRay Lab for "clean" samples
  • THELCO in Filter Room for desiccant and chemically treated samples
  • Imperial III with N2 in Geochem Lab for samples and some small equipment

Check contents of oven with other users before placing new items in it to avoid cross-contamination to open vessels.

Remove top from sample container.

Inside oven; link to larger image

Place samples in oven at 60 degrees F for at least 24 hours or until cracks appear in sediment.

Check oven door to make sure it latches.

Thermometer for oven; link to larger image

Place samples in desiccator when removed from oven to cool and to avoid getting moisture from the air in your samples.

Weigh samples on a balance to get the dry weight.

Desicato; link to larger imager
FREEZE DRYING PREPARATION
Materials Required:
  • Small Kimwipe
  • Rubberbands
  • Plastic Glove
  • Sample
Freeze Dry preparation for Planar; link to larger image

After core cutting, samples are frozen and put into storage.

When ready to analyse, locate samples in storage and wipe sides of sample container with a Kimwipe so there is no frost.

Wipe frost off container; link to larger image

Place container lid in a plastic glove so there is no contamination of sediment on the lid.

Rip a Kimwipe so 1 layer fits on mouth of sample container.

Place Kimwipe on sample and secure with a rubber band.

Cover sample with Kimwipe; link to larger image
FREEZE DRYING SAMPLES
Materials Required:
  • Samples
  • Freeze Dryer
  • Notebook
  • Sharpie
  • Basin
  • Paper Towels
  • Vacuum Pump Oil
Freeze Drying preparation; link to larger image

Weigh the samples to determine which one is the heaviest and record the weights in a notebook. Mark the heaviest sample with a Sharpie on the Kimwipe to use as a standard to compare the freezing progress of the other samples.

Place a stack of containers in the freeze dryer using the racks provided.

If the heaviest sample is completely freeze dried, then the others will be.

Place samples in rack

Remove attachable jars, or, if necessary, place samples in the jars.

For exterior jars, if removed you must seal the vacuum.
If using jars, make sure the re-seal is good.

Remove jars; link to larger image

Turn the white knob to vent if there is no jar attached.

Turn the white knob to vac if there is a jar attached.

Turn to vent or vacuum; link to larger image

Check the vacuum pump oil level.

Start the machine by pushing the Refrigeration button ON to Man. Vac. (Manual Vacuum). Once the temperature reaches -40 degrees C, turn the vacuum on by pushing the Vacuum button up to the ON position.

You will see the word "HI" for high temperature displayed in the window. Once numbers start appearing, you should check it periodically to make sure the numbers are decreasing. The system is functioning properly when the number drops to 200 millibars or below.

Record the pressure and temperature in the notebook and watch periodically for 3 days until all samples are frozen.

Remove samples from machine and remove the caps immediately so you can weigh the sample immediately.

Turn on; link to larger image

 

 

Record pressure and temperature

To shut down after use:

Push buttons to OFF position, leave the lid open to vent, drain the water out into a basin, and dry the inside coils with paper towels.

Turn the Defrost button ON to help speed the process.

Drainage basin; link to larger image

 

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