D5453_19_11
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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 resident's 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 3 times,
and calculate
the average detector responses.
Determine density values,
gram and milliliter needed for calculations,
by performing a gravimetric weighing
of the test sample into a Class-A volumetric flask.
See, Note 14: C-Section 12.1.
During the various inter-laboratory studies,
see, 15.1:Test Sample Density Values.
Gram and milliliter needed for calculations
are always provided to participants,
and were determined by the ILS distributor
in a variety of ways,
including information
supplied by bulk sample suppliers.
Accompanying information from documentations,
such as safety data sheets,
and gravimetric weighing into a volumetric flask
at ambient laboratory temperatures,
with the gravimetric method
being the most common.
Density values needed for calculations,
may be measured using test methods:
D-1298 and D-4052 or equivalent.
See, Note 15.
Users of the test method, may convert
density measured at standard temperature,
to the temperature
at which the sample was tested,
by using Guide D-1250 and its adjuncts.