D5453_11 (16e1)
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Obtain a test specimen using the
procedure described in Section
8 of the written standard.
The sulfur concentration
in the test specimen
must be less than the
concentration of the highest
standard and greater
than the concentration
of the lowest standard
used in the calibration.
If required, a dilution can be
performed on either a weight
or volume basis.
Record the mass of
the test specimen
and the total mass of the
test specimen and solvent.
Record the mass of
the test specimen
and the total volume of the
test specimen and solvent.
Measure the response for
the test specimen solution
using one of the procedures
described in 10.2
through 10.4 of the
written standard.
Inspect the combustion tube
and other flow path components
to verify complete oxidation
of the test specimen.
Reduce the sample size or the
rate of injection, or both,
of the specimen into the furnace
if coke or sooting is observed.
Increase the residence time
for the boat in the furnace
if coke or soot is
observed on the boat.
Decrease the boat drive
introduction rate or specimen
sample size, or
both, if coke or soot
is observed on the exit
end of the combustion tube.
Clean any coked or sooted
parts per manufacturer's
instructions.
After any cleaning
or adjustment,
assemble and leak
check the apparatus.
Repeat instrument calibration
prior to re-analysis
of the test specimen.
To obtain one result, measure
each test specimen solution
three times and calculate the
average detector responses.
Density values needed
for calculations
are to be measured using
Test Methods D1298, D4052,
or equivalent, at
the temperature
at which the sample was tested.