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Woods Hole Field Center

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


CHN SAMPLE WEIGHING

Samples can be run for Total Carbon and/or Organic Carbon.

WEIGHING SAMPLES FOR TOTAL CARBON
Materials Required:
  • 4 Place Micro Balance
  • Dried Samples
  • Micro Forceps
  • Micro Spatula
  • Tin Weighing Capsules (8x5mm)
  • Black Plastic Capsule Stand
  • Capsule Tray
  • Kimwipes
  • Methanol Squirt Bottle
  • Sample Weight Data Sheet
Weighing preparation materials; link to larger image

Remove 3 to 5 samples from the drying oven and record their ID's on the sample sheet - sample sheet has rows and columns labeled like the tray so the first empty space in the tray is the first sample ID listed on the sheet.

Close the lids so they are not exposed to the moisture in the air.
*Moisture effects the weighing process.

Record data into notebook; link to larger image


Using the micro forceps, place a clean and empty tin capsule in the capsule stand and tare it on the balance.

 

Tare balance with capsule and stand; link to larger image

Use the micro spatula to remove approximately 10mg of dried sediment sample and place it in the tin capsule.

Spoon sample into tin capsule; link to larger image

Remove the capsule stand and capsule from the balance, and place it on the table.

With micro forceps in each hand, hold onto the capsule stand, pinch the top of the tin capsule closed, and remove it from the stand.

Remove capsule from stand with tweezers; link to larger image



Where you pinched the capsule closed, fold it over into thirds and flatten with the forceps.

 




Turn it 90 degrees and fold it into thirds again.

* Be careful not to tear the capsule.

 

First fold

Second fold

Weigh the finished sample (9.500 to 10.500mg) and place it in the capsule tray.
If the capsule tears during the folding process, you'll need to start over with fresh sample, weigh it, and fold it again.

Clean off the micro spatula with methanol and a Kimwipe and continue with the next sample.

*Non-folded capsules pictured at right.

Capsules open in tray; link to larger image

WEIGHING SAMPLES FOR ORGANIC CARBON
Materials Required:
  • 4 Place Micro Balance
  • Dried Sediment Samples
  • Micro Forceps
  • Micro Spatula
  • Silver Weighing Capsules (12x5mm)
  • Black Plastic Capsule Stand
  • Capsule Tray
  • Kimwipes
  • Methanol Squirt Bottle
  • Sample Weight Data Sheet
  • Sulfurous Acid
  • 50µL pipetter and tip
  • Drying Oven (60°C)
  • Safety Gear - gloves, goggles, lab coat, fume hood
Weighing preparation

Acidification preparation

Remove 3 to 5 samples from the drying oven and record their ID's on the sample sheet - sample sheet has rows and columns labeled like the tray so the first empty space in the tray is the first sample ID listed on the sheet.

Close the lids so they are not exposed to the moisture in the air.
*Moisture effects the weighing process.

Sample recording



Using the micro forceps, place a clean and empty silver capsule in the capsule stand and tare it on the balance.

 

Tare balance with capsule and stand
Use the micro spatula to remove approximately 10mg of dried sediment sample and place it in the silver capsule. Spoon sample into tin capsule; link to larger image

Record the weight (9.500 to 10.500mg), remove the capsule stand from the balance, and place the capsule in the tray.
*Leave capsules open - DO NOT FOLD.

Capsules open in tray; link to larger image

Under a fume hood, add 50µL of Sulfurous Acid to each capsule with a pipette and set tray in drying oven without lid to dry for 20 minutes.
Remove tray from oven, add another 50µL of acid and let dry in oven for 20 minutes.
Remove tray from oven, add a final 50µL of acid and return samples to oven to dry overnight.
*Wear proper safety gear (goggles, gloves, lab coat).

Acidifying samples; link to larger image

On the following day, remove the capsule tray from oven, fold capsules as you would for Total Carbon, return them to the tray, and place them in a desiccator until you are ready to run the analysis.

Samples can remain in the desiccator indefinitely as long as the desiccant is viable.

Folding capsule with tweezers; link to larger image

CLEANING CAPSULES
Materials Required:
  • Capsules to clean (silver or tin)
  • Methanol
  • Acetone
  • 200mL Glass Beaker
  • Waste Container for organic solvents
  • Watch Glass
  • Safety Gear - goggles, gloves, lab coat, fume hood


Preparation Materials for Cleaning Capsules

Empty the jar of capsules into a clean beaker and add enough Methanol to cover the capsules.
*Make sure all capsules are submerged in the Methanol and none are floating.

Sonicate the capsules for 10 minutes.
Take beaker out of sonicator and drain the Methanol into a waste container using a watch glass to keep capsules in the beaker.

Next, add enough Acetone to cover the capsules and sonicate for another 10 minutes making sure all are submerged.

Take beaker out of sonicator and drain the Acetone into the solvent waste container using a watch glass to keep capsules in the beaker.

 

Clean capsules with Methanol

 

Set the beaker of clean capsules in the laminar flow hood to dry.

Let capsules dry in hood; link to larger image

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