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DIGESTION PROCEDURE FOR OILS,
5.
Do not proceed if
sulfuric acid is not visible
Add 10 mL
in the flask.
of 50% hydrogen
peroxide to the charred
sample via the funnel on
the fractionating head.
Note: Visually confirm the
presence of sulfuric acid in
the flask before adding
hydrogen peroxide.
Note: If the digest does not
turn colorless, add 5 mL
increments of peroxide until
the digest becomes clear or
does not change color.
Note: If sample foams
during hydrogen peroxide
addition, stop the peroxide
flow and remove the
digestion flask and
fractionating column (use
finger cots). Cool for
30 seconds and return
apparatus to the heating
block. Start peroxide
addition with 2 mL,
then follow with the
remaining peroxide.
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6.
After addition of
hydrogen peroxide is
complete, boil off excess
hydrogen peroxide by
heating for one more
minute. Do not heat
to dryness.
Note: If the sample goes to
dryness, turn off the
Digesdahl and air cool
completely. Add water
to flask before handling.
Repeat digestion from the
beginning using a new
sample.
continued
7.
Take the hot flask off
the heater and allow the
flask to air cool. Remove
the fractionating column
from the digestion flask.
Note: Use finger cots to
remove the digestion flask.
Place it on a cooling pad
for at least one minute.
Then remove the column.
Do not add water to the
flask until it has cooled.
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8.
Dilute the digest
to approximately 70 mL
with deionized water.
Note: Add demineralized
water slowly at first. Cool
the flask if necessary
for handling.
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