Parr Instrument 6400 - Manual (Page 18)

2
Quick Start
P a r r I n s t r u m e n t C o m p a n y 16
c
haPter
2
Quick Start
Initial Fill
When you first fill the calorimeter with water the
main reservoir will be filled. There is also a cooling
water reservoir that is filled from the main reservoir.
Once the calorimeter has been filled with water and
all external connections made:
1. Turn on the calorimeter.
2. Once at the Main Menu go to the Calorimeter Op-
eration screen and turn ON the heater and pump.
Water should start to circulate in the tubing.
3. Press Escape to get back to the Main Menu. Then
press Diagnostics and then I/O Diagnostics.
4. Use the side arrow keys(< >) until the description
reads H2O Cool.
5. Unlock and remove the vessel head.
6. Press “1” to turn on the H2O Cool. You should
hear a click and then gurgling coming from the
bomb cylinder.
7. Once the gurgling stops turn off the H2O cool by
pressing “O”.
8. Refill the main reservoir through the elbow at
the back of the calorimeter.
The above procedure will only need to be done
when the calorimeter is first filled with water after
receiving it.
Quick Start
1. Turn on the heater and pump in the Calorimeter
Operation menu. Allow at least 20 minutes for
the calorimeter to warm up.
2. Initiate a pretest to run the calorimeter through
the fill and cool/rinse cycles. This function is
used to pre-condition the calorimeter if it has
been sitting idle for an extended period of time
(greater than 15 minutes).
3. Prepare and weigh the sample to 0.0001g.
4. Gently tap capsules that contain powdered
samples to compact the material. (Pellets are
easier to handle than loose samples and they
burn slower in the bomb, thereby reducing the
chances for incomplete combustion).
5. Carefully place the capsule into the capsule
holder, attach 10 cm of ignition thread and install
the bomb head in the calorimeter.
6. Close the calorimeter cover making sure that the
latch is engaged.
7. Select determination or standardization as ap-
propriate on the Calorimeter Operation page, by
toggling the OPERATING MODE key. Press the
START Key. The calorimeter will now prompt the
operator for sample ID number, Bomb ID num-
ber, sample weight and spike weight in accor-
dance with the instructions set into the operating
controls page.
8. The calorimeter will now take over and conduct
the test. During the time it is establishing the ini-
tial equilibrium, it will display PREPERIOD on the
status bar. Just before it fires the bomb, it will
sound a series of short beeps to warn the user
to move away from the calorimeter. Once the
bomb has been fired, the status bar will display
POSTPERIOD. The calorimeter will check to make
certain that a temperature rise occurs and will
then look for the final equilibrium conditions to
be met. If it fails to meet either the initial or final
equilibrium conditions, or if it fails to detect a
temperature rise within the allotted time, the test
will terminate and advise the user of the error.
9. At the conclusion of the test, the calorimeter will
signal the user.
10. Open the cover and remove the head. Examine
the interior of the bomb for soot or other evi-
dence of incomplete combustion. If such evi-
dence is found, the test will have to be discarded.
If using the optional A1050DD Rinse Container
Assembly:
1. Titrate the bomb washings with a standard
sodium carbonate solution using methyl orange,
red or purple indicator. A 0.0709N sodium car-
bonate solution is recommended for this titra-
tion to simplify the calculation. This is prepared
by dissolving 3.76 grams of Na
2
CO
3
in the water
and diluting to one liter. NaOH or KOH solutions
of the same normality may be used.
2. Analyze the bomb washings to determine the
sulfur content of the sample if it exceeds 0.1%.
Methods for determining sulfur are discussed in
Analytical Methods for Oxygen Bombs, No. 207M.