Parr Instrument 6300 - Manual (Page 127)

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PPENDIX
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VERVIEW
The A1050DD Bomb Rinse Container Assembly is
provided as an accessory to the 6300 Calorimeter. This
device allows for complete and systematic recovery of
the bomb combustion products.
These combustion products include that portion which
is released during the initial bomb exhaust, followed by
the portion expelled during the bomb rinse cycle.
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ONCEPT OF
O
PERATION
The 6300 Bomb Rinse Container Assembly is connected
to the rear of the calorimeter, in place of the portion of
the waste tube assembly that is connected to the bomb
exhaust fitting. The bomb exhaust and the bomb wash-
ings are collected in the 1053DD, HDPE 500 mL bottle,
provided with the A1050DD. The objective is to capture
and retain all of the combustion products which have
been dissolved in the residual water present in the bomb
prior to combustion as well as any water formed during
the combustion process. The most common examples
of these combustion products include:
Sulfate, derived from any sulfur containing
materials in the original sample.
Chloride, from organic samples containing chlorine.
These combustion products are discharged from the
bomb in two steps. The first step occurs during the
initial rapid release of the residual bomb gases. The
1053DD bottle has sufficient strength and volume to
deal effectively with this sudden pressure release. Gas
is expelled from the four holes on the perimeter of the
1052DD bottle cap, leaving any discharged liquid in
the bottle. As an additional safety measure, the bottle
is supported in a 1054DD acrylic cylinder which serves
to keep the bottle upright and contained in the un-
likely event the bottle ruptures. At the end of the bomb
exhaust step the aqueous combustion products reside
in the bomb, associated tubing as well as the 1053DD
bottle. The bomb rinse step flushes these combus-
tion products from the bomb and the tubing into the
1053DD bottle. The bottle can then be unscrewed from
the assembly and capped, until the sample is to be ana-
lyzed. Some users find it useful to add the contents of
the rinsed combustion capsule to the washings collected
in the bottle. Three 1053DD bottles are provided with
the assembly. Additional bottles may be ordered sepa-
rately from Parr.
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ONNECTION
Break the connection at the rear of the 6300 Calorim-
eter to the bomb exhaust hose. In place of this, connect
the “tube and 3/8” compression fitting provided as part
of the A1050DD.
Adjusting the Bomb Rinse Parameters
The bomb rinse parameters are factory set to provide
approximately 50 ml of bomb washings. This amount
was chosen in order to rinse the bomb as quickly as
possible in order to prepare the calorimeter for the next
test. More quantitative rinsing can be realized, at the
expense of time, by increasing the volume of washings.
Experience has demonstrated that for a bomb of this
volume, wash volumes on the order of 100 ml are
required for quantitative recovery. Doubling either the
# of rinse cycles or the rinse time on the bomb rinse
tank controls menu page of the operating controls menu
from the default value of 3 will provide a volume of
washing better suited for precise analytical work. The
volume of washing can be easily verified by performing
a calorimeter pretest sequence.
O
PERATION
Place the bottle end of the rinse assembly in the
1054DD Bottle Support and orient in such a way to
minimize any undesirable effects by the bomb exhaust
discharge from the four holes in the 1052DD bottle cap.
Analyze the sample in the calorimeter in the usual fash-
ion, using the following guidelines in order to insure
quantitative conversion to the proper ionic form of the
analyte:
Samples containing sulfur should contain no more than
5% sulfur as-burned in the calorimeter and have a heat
of combustion of at least 9000 Btu/lb.