D97 17b Spanish CC Test
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Pour the specimen into the
test jar to the level mark.
When necessary, heat
the specimen in a bath
until it is just
sufficiently fluid
to pour into the test jar.
It is known that some materials,
when heated to a temperature
higher than 45 degrees Celsius
during the preceding 24 hours,
do not yield the same
pour point results as when
they are kept at room
temperature for 24 hours prior
to testing.
Examples of materials which
are known to show sensitivity
to thermal history are
residual fuels, black oils,
and cylinder stocks.
Samples of residual
fuels, black oils,
and cylinder stocks which have
been heated to a temperature
higher than 45 degrees Celsius
during the preceding 24 hours,
or when the thermal history
of these sample types
is not known, shall be kept at
room temperature for 24 hours
before testing.
Samples which are
known by the operator
not to be sensitive
to thermal history
need not be kept at room
temperature for 24 hours
before testing.
Experimental evidence
supporting elimination
of the 24-hour waiting
period for some sample types
is contained in a research
report, footnote 6
of the written standard.
In the case of pour
points above 36 degrees
Celsius, use a higher range
temperature measuring device,
such as IP63C, or ASTM 61C, or
a digital contact thermometer.
Close the test jar with a cork
carrying the test temperature
measuring device.
Adjust the position of the
cork and temperature measuring
device so the cork fits tightly,
the temperature measuring
device and the jar are coaxial,
and the temperature measuring
device is immersed
to the correct depth.
For liquid in glass,
the thermometer bulb
should be immersed so the
beginning of the capillary
is 3 millimeters below the
surface of the specimen.
For digital contact
thermometers,
the probe should be immersed
so the end of the probe
is 10 millimeters to 15
millimeters below the surface
of the specimen.
For the measurement
of pour point,
subject the specimen
in the test jar
to the following
preliminary treatment.
Heat the specimen without
stirring to 9 degrees
Celsius above the
expected pour point
but to at least
45 degrees Celsius
in a bath maintained
at 12 degrees
Celsius above the
expected pour point
but at least 48 degrees Celsius.
Transfer the test jar to a
bath maintained at 24 degrees
Celsius plus or minus
1.5 degrees Celsius
and commence observations
for pour point.
When using a liquid bath,
ensure that the liquid level
is between the fill
mark on the test jar
and the top of the test jar.
Heat the specimen without
stirring to at least 45 degrees
Celsius in a bath
maintained at 48 degrees
Celsius plus or minus
1.5 degrees Celsius.
Transfer the test jar
to a bath maintained
at 24 degrees Celsius plus
or minus 1.5 degrees Celsius.
When using a liquid bath,
ensure that the liquid level
is between the fill
mark on the test jar
and the top of the test jar.
When the specimen temperature
reaches 27 degrees Celsius,
and if using liquid
and glass thermometers,
remove the high cloud
and pour thermometer
and place the low cloud and
pour thermometer in position.
Transfer the test jar
to the cooling bath.
See 8.6.1 of the
written standard.
See that the disk, gasket,
and the inside of the jacket
are clean and dry.
Place the disk in the
bottom of the jacket.
Place the gasket
around the test jar
25 millimeters from the bottom.
Insert the test
jar in the jacket.
Never place a jar directly
into the cooling media.
After the specimen
has cooled to allow
the formation of
paraffin wax crystals,
take great care not to
disturb the massive specimen
nor permit the thermometer
to shift in the specimen.
Any disturbance of the spongy
network of wax crystals
will lead to low and
erroneous results.
Pour points are
expressed in integers
that are positive or negative
multiples of 3 degrees Celsius.
Begin to examine the
appearance of the specimen
when the temperature
of the specimen
is 9 degrees Celsius above
the expected pour point
estimated as a multiple
of 3 degrees Celsius.
At each test temperature that
is a multiple of 3 degrees
Celsius below the
starting temperature,
remove the test jar
from the jacket.
To remove condensed moisture
that limits visibility,
wipe the surface with a clean
cloth moistened in alcohol,
ethanol, or methanol.
Tilt the jar just
enough to ascertain
whether there was a movement of
the specimen in the test jar.
If movement of specimen
in the test jar is noted,
then replace the test jar
immediately in the jacket
and repeat a test for a
flow at the next temperature
3 degrees Celsius lower.
Typically, the
complete operation
of removal, wiping,
and replacement
shall require not
more than 3 seconds.
If the specimen has
not ceased to flow
when its temperature has
reached 27 degrees Celsius,
transfer the test
jar to a jacket
in a cooling bath maintained at
0 degrees Celsius plus or minus
1.5 degrees Celsius.
As the specimen
continues to get colder,
transfer the test jar to
a jacket in the next lower
temperature cooling
bath in accordance
with table 2 of the
written standard.
If the specimen in the jar does
not show movement when tilted,
hold the jar in a
horizontal position
for 5 seconds, as noted by
an accurate timing device,
and observe the
specimen carefully.
If the specimen shows
any signs of movement
before 5 seconds has
passed, replace the test jar
immediately in the jacket and
repeated a test for a flow
at the next temperature
3 degrees Celsius lower.
Continue in this
manner until a point
is reached at which the specimen
shows no movement when the test
jar is held in a horizontal
position for 5 seconds.
Record the observed reading
of the test thermometer.
For black specimen, cylinder
stock, and residual fuel
specimen, the result obtained by
the procedure described in 8.1
through 8.7 of the
written standard
is the upper,
maximum pour point.
If required, determine the
lower, minimum pour point
by heating the sample while
stirring to 105 degrees
Celsius, pouring
it into the jar,
and determining
the pour point as
described in 8.4 through
8.7 of the written standard.
Some specifications allow
for a pass fail test or have
pour point limits at
temperatures not divisible
by 3 degrees Celsius.
In these cases, it is
acceptable practice
to conduct the pour point
measurement according
to the following schedule.
Begin to examine the
appearance of the specimen
when the temperature
of the specimen
is 9 degrees Celsius above
the specification pour point.
Continue observations
at 3 degrees
Celsius intervals as
described in 8.6 and 8.7
of the written standard
until the specification
temperature is reached.
Report the sample as
passing or failing
the specification limit.