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Recovering the combustion products, An optional recovery procedure, 1108p oxygen combustion vessels – Parr Instrument 1108P User Manual

Page 7

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1108P Oxygen Combustion Vessels

Fire the charge by pressing the firing button on the
ignition unit, keeping the circuit closed for about 2
seconds. The indicator light will come on when the
button is depressed and will remain on while the
button is depressed.

If the indicator light does not come on when the
firing button is pressed there is either a fault in the
2901 or an open circuit in the system. Check for
voltage between the 10 cm and common termi-
nals of the 2901. Approximately 23 VAC should be
measured. If there is no voltage present, check the
fuse inside the 2901. An open circuit can usually be
located with an ohmmeter. Flex the lead wires dur-
ing any continuity check as the wires may be broken
and making only intermittent contact. If the red indi-
cator light glows during ignition but the bomb fuse
does not burn, check the system for a voltage leak
to ground, most likely in the insulated electrode on
the bomb head. Check the electrode using the high
impedance scale on an ohmmeter and replace the
electrode insulator and seal if leakage is indicated.

Recovering the Combustion Products

Let the bomb stand in the calorimeter or water bath
for at least 3 minutes, then lift it out of the water
and wipe with a clean towel. Open the valve knob
slightly to release all residual gas pressure before
attempting to remove the screw cap.

Caution!
Do NOT have any part of the body in the

exhaust path of the bomb.

Gas release should proceed slowly over a period
of not less than one minute to avoid entrainment
losses. After all pressure has been released, un-
screw the cap; lift the head out of the cylinder and
place it on the support stand. Do not twist the head
during removal. Pull it straight out to avoid sticking.
Examine the interior of the bomb for soot or other
evidence of incomplete combustion. If such is found
the test will have to be discarded. Wash all interior
surfaces of the bomb and the combustion capsule
with a jet of distilled water and collect the washings.
If any precipitate or residue is present, remove it
with a rubber policeman. Do not filter the washings
as this might remove valuable constituents. Titrate
the washings and measure the unburned fuse wire
as required for calorific tests, then analyze the wash-
ings for sulfur and other elements, if required.

An Optional Recovery Procedure

If desired, a luer fitting, 518A, can be attached to the
bomb to provide a means for washing the bomb
and recovering the combustion products with a
syringe without opening the bomb and removing
the bomb head. To use this procedure, remove the
standard A420A valve needle and replace it with an
A420A2 needle to which a syringe, 244C, can be at-
tached.

To recover the combustion products via a luer fit-
ting, let the bomb stand in a cooling bath for at
least 3 minutes after firing to allow for complete
condensation of all residual vapor. Then remove the
bomb from the water and attach only the barrel of a
244C syringe to the luer fitting. Open the valve and
release the pressure at a slow rate, using at least
a full minute to bring the bomb pressure back to
atmospheric. The attached syringe barrel will help to
retain any condensate spray that might be carried
out of the valve during the exhaust period.

Add 30 mL of distilled water to the attached syringe
barrel and use the syringe plunge to force the water
into the bomb, then close the valve while holding
the plunger down. This will develop sufficient pres-
sure within the bomb to seat the inlet check valve
and provide enough positive pressure to help re-
move the washings. Agitate and rotate the bomb in
a horizontal position to wet all inner surfaces, then
turn the bomb upside down over a 600 mL beaker
and open the valve to discharge the washings into
the beaker. Tilt the bomb slightly toward the valve
to get as much of the water out as possible. Repeat
this back-flushing procedure two times, collecting
a total of 90 to 100 mL of washings, then open the
bomb and recover any liquid that may remain in the
cylinder. The three complete back flush and rinse
cycles should recover better than 99 percent of the
combustion products.