492M

1109A Semi-micro Oxygen Bombs

Operating Instruction Manual
ParrInstrumentCompany
P a r r I n s t r u m e n t C o m p a n y
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1109A
SEMI-MICRO
OXYGEN BOMBS
FIGURES
Figure 1
1109A Semi-micro Oxygen Bomb 3
Figure 2
Binding Fuse to 1109A Bomb 6
Figure 3
1109A Bomb Head Assembly, A530A2 7
Figure 4
1109A Semi-micro Oxygen Bomb, Electrodes 12
Figure 5
1109A Semi-micro Oxygen Bomb, Cut-away View 13
Figure 6
Parts Diagram for the 1109A Manual Valve 14
Parts Key for the 1109A Manual Valve 15
TABLE OF CONTENTS
PURPOSE 3
DESCRIPTION 3
UTILITIES 3
OPERATION 3
Safety 4
Setting the Calorimeter Parameters 4
Installing a Conversion Set 5
Sample Preparation 6
Preparing the Fuse 7
Closing the Bomb 7
Filling the Bomb with Oxygen 8
Filling the Bucket 8
Analyzing the Results 8
Standardization 9
MAINTENANCE 10
PARTS LIST 11
DRAWINGS 12
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1109A
SEMI-MICRO
OXYGEN BOMBS
PURPOSE
The Parr 1109A Semi-micro Oxygen Bomb is designed
for small samples such as marine biology or ecologi-
cal studies. It may also be used when sample size is
limited. These instructions will provide the user with
guidelines for the safe operation and maintenance of
the vessel. These instructions must be supplemented
with manual 205M, Operating Instructions for the 1108
Oxygen Combustion Bomb, which contains information
concerning sample preparation and other application
information relevant to both vessel types. It should
also be supplemented with the appropriate calorimeter
manual.
DESCRIPTION
The semi-micro oxygen bomb is the smallest of the Parr
oxygen bombs. This 22 mL bomb will handle samples
that range from 25 to 200 milligrams, liberating 52
to 1200 calories when burned in oxygen, using initial
pressures up to 35 atmospheres. Outputs of up to 2400
calories can be accommodated if the sample is self-oxi-
dizing, provided it is burned in an inert atmosphere and
does not produce gas.
There are three main components to the semi-micro
oxygen bomb: the cylinder, the screw cap and the head.
UTILITIES
A minimum 99.5% purity oxygen source provid-
ing 420 psig (3 Mpa) of pressure to the bomb is
required.
Distilled water to fill the twin-chambered bucket is
preferred, however, demineralized or tap water with
less than 250 ppm of dissolved solids is acceptable.
To ignite the sample, 10 cm of NiCr fuse wire (P/N
45C10) per test is needed.
OPERATION
Note: The heat unit used in these instructions is the
International Table (IT) Calorie, which is equal to 4.1868
absolute joules. This is the engineering unit commonly
used in the fuel industry. The thermochemical calorie
used in thermochemical studies is equal to 4.1840 absolute
joules.
Note: The calorimeter should be standardized prior to
analyzing a sample.
Figure 1

1109A Semi-micro Oxygen Bomb
P a r r I n s t r u m e n t C o m p a n y
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1109A
SEMI-MICRO
OXYGEN BOMBS
Safety
Samples to be burned in the 1109A bomb may 1.
range in size from 25 to 200 milligrams, depending
upon the combustion characteristics of the material
and the amount of the heat produced.
The total charge must not release more than 1200 2.
calories and this limit must be reduced considerably
if there is any reason to suspect that the test sample
has explosive properties, or that large quantities of
gas will be produced upon ignition.
Use only a fraction of the allowable sample weight 3.
when testing unfamiliar materials, which may burn
either rapidly or explosively.
Do not charge the bomb with more oxygen than is 4.
necessary to obtain complete combustion. Do not
fire the bomb if it is pressurized to more than 35
atmospheres.
Keep all parts of the bomb, especially the insulated 5.
electrode, in good repair at all times. If gas bubbles
escape from the bomb while it is submerged in wa-
ter, do not fire the charge.
Keep away from the top of the calorimeter for 15 6.
seconds after firing. If the bomb should rupture, it
is most likely that the resultant forces will be direct-
ed upward along the vertical axis.
Never use lubricants on valves or fittings in contact 7.
with high-pressure oxygen.
Setting the Calorimeter Parameters
Refer to the following manuals for further instruc- 1.
tions regarding the operation of the calorimeter.
Calorimeter Model Number
Manual
Number
6200 Isoperibol Calorimeter 442M
6100 Compensated Jacket Calorimeter 455M
6725 Semi-micro Calorimeter 457M
When using the 1109A Semi-micro Oxygen Bomb 2.
in a calorimeter, the user must ensure that the
correct User set up ID is set in order to obtain the
appropriate operating parameters.
When using a 6100 or 6200 Calorimeter: 3.
Select Program Info & Control. a.
From Program Info & Control, select User/ b.
Factory Settings.
Select User Setup ID. c.
Press Clear. d.
Enter 62-1107 (or 61-1107). e.
Press Enter. f.
Press Reload User Default Settings and fol- g.
low the instrument prompts.
This will change the jacket temperature of the h.
6200 to 25 C. Any water handling unit in use
should be set at 20 to 22 C.
When using the 6725 Semi-micro Calorimeter with 4.
the 6772 Calorimetric Thermometer:
Select Operating Controls. a.
From the Operating Controls menu, select b.
Method of Operation. This button will toggle
between Solution and Combustion.
Select Combustion. c.
For older models, please contact Parr for the ap- d.
propriate software.
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1109A
SEMI-MICRO
OXYGEN BOMBS
Installing a Conversion Set
In order to use the semi-micro bomb in the larger 1.
Parr calorimeters, a conversion set must be installed.
Contact Parr for the appropriate conversion kit for
your older model calorimeter.
All of the parts needed to operate a semi-micro 2.
bomb in a 6200 or 6100 Calorimeter are provided
in the 6269A Semi-micro Conversion Kit. The kit
consists of the following major parts:
1109A Semi-micro Bomb
A twin-chambered calorimeter bucket
Two Inconel fuel capsules
A sufficient supply of alloy fuse wire
A supply of benzoic acid pellets for standardiz-
ing the calorimeter
A hose assembly for filling the bomb with oxy-
gen from the calorimeter
Install the bucket support 3.
The A604DD twin-chambered bucket for semi- a.
micro operations consists of two cylindrical
chambers with connecting tubes. The larger
chamber holds the semi-micro bomb on a ring
support. The smaller chamber serves as a draft
tube in which the stirrer for the 6200 or 6100
Calorimeter can operate as a pump, circulating
water through the connecting tubes.

Unthread the Delrin feet from the bottom of the b.
air can assembly of the calorimeter.
Install the bucket support and loosely replace c.
the Delrin feet.
Check the position of the support with the d.
twin-chambered bucket installed. The smaller
chamber of the A604DD is positioned toward
the front of the calorimeter and accepts the stir-
rer shaft.
Lower and raise the calorimeter lid slowly to e.
check that the stirrer and temperature probe
do not contact the bucket or bomb. Adjust the
bucket support position as needed and tighten
the Delrin feet to hold the bucket support in
place.
Replace the oxygen filling line and connection for 4.
the 1108 Oxygen Combustion Bomb (part number
A19A16) with the filling line and connection for
the 1109A Semi-micro Oxygen Bomb (part number
A19A14).
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1109A
SEMI-MICRO
OXYGEN BOMBS
Sample Preparation
The precision of calorimetric determinations can be 1.
improved by adherence to several basic practices:
Be consistent in all procedures. Use the same
equilibration periods, pre-periods, post-periods,
weight ranges, temperature ranges, sampling
techniques, etc. for comparable samples.
Standardize the calorimeter with a set of tem-
perature rises nearly identical to the tempera-
ture for the experimental sample. The energy
equivalent is not absolutely constant over a
range of temperature rise value.
Carefully control the purity, moisture content
and homogeneity of the samples.
Weigh samples carefully and keep the analytical
balance in good condition.
Manual 205M, 2. Operating Instructions for the 1108 Oxy-
gen Combustion Bomb, contains valuable information
concerning sample preparation and analysis of the
combustion products.
Some small samples do not burn well unless mixed 3.
with another easily burned material such as benzoic
acid or mineral oil.
Foodstuffs and cellulosic materials are particularly 4.
sensitive to extremes of moisture content.
Very dry samples do not form strong pellets and a.
usually burn too rapidly.
In contrast, samples with too much moisture are b.
difficult to ignite.
Tissue samples may be lyophilized, and then c.
formed into pellets.
Semi-micro samples generally burn best if com- 5.
pressed into inch diameter pellet, which can be
prepared easily with the Parr 2812 Pellet Press. Parr
offers inch diameter benzoic acid pellets for stan-
dardization, P/N 3414.
Place the sample in a tared fuel capsule (208AC) 6.
and weigh it to 0.01 mg, then set the capsule aside
while attaching the fuse to the bomb head.
Some users may desire optional platinum parts a.
as these parts may provide for more complete
combustion when used with samples that liber-
ate less than 600 calories.
The platinum capsule (P/N 169AC) should al- b.
ways be used with a platinum fuse (P/N 45C3)
and the platinum capsule support loop (P/N
165AC2).
Figure 2
Binding Fuse to 1109A Bomb
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1109A
SEMI-MICRO
OXYGEN BOMBS
Preparing the Fuse
Parr offers a stand to support the head of the semi- 1.
micro oxygen bombs while attaching the fuse wire.
The stand, including the ring, is part number A38A
and the semi-micro adapter for holding the head is
part number 533A.
Cut a 10-cm length of fuse wire and bend it to the 2.
hook terminals as shown below in Figure 2.

Catch the wire loop in a small Allen wrench and ro- 3.
tate the wrench to form a five turn helical coil. The
coiled wire will concentrate heat on the sample and
serve also as a rigid support for holding the sample
in place while handling the bomb prior to ignition.
A pair of forceps may be useful for binding and
forming the wire.
After coiling the fuse, set the sample in the capsule 4.
support loop and position the coil so that it bears
against the charge. Some users of the semi-micro
bomb have found it easier to keep the Inconel
capsule (208AC) in place by lodging it between the
turns of the capsule support loop. Quantitative
transfer of the sample from the balance to the cap-
sule becomes important when using this technique.
Closing the Bomb
Moisten the O-ring with distilled water, set the 1.
bomb head in the cup, and then thread on the screw
cap. Some users will find it easier to leave the O-
ring in the cup rather than on the head assembly.
Handle the bomb carefully during this operation so 2.
that the sample will not be disturbed. Unlike other
Parr oxygen bombs, no water is placed inside the
semi-micro bomb prior to ignition.
Figure 3
1109A Bomb Head Assembly, A530A2
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1109A
SEMI-MICRO
OXYGEN BOMBS
Filling the Bomb with Oxygen
Note: Never fire the 1109A Semi-micro Oxygen bomb if it
has been filled with more than 35 atmospheres of oxygen.
Slide the oxygen filling assembly onto the valve cap 1.
assembly (A168AC) until it rests against the valve
cap shoulder.
Insert the pin wrench (10MB3) through the eye of 2.
the valve cap and open the cap one turn from the
closed position. Leave the pin wrench in cap.
Press the O2 Fill key on the calorimeter. After 3.
30 seconds, use the pin wrench to close the manual
valve on the 1109A. The user can then press Re-
set and the residual pressure in the filling hose will
be automatically released.
Remove the pin wrench and lift the filling connec- 4.
tion off the valve cap assembly.
Filling the Bucket
By Weight 1.
Place the semi-micro bomb in the twin-cham- a.
bered bucket and fill the bucket with distilled
water to a level 1/8 above the horizontal tube
with the bomb in place. This amount of water
will then be used in all tests, but the water will
be measured by weight instead of by volume.
Remove the bomb and weigh the bucket and b.
water to 0.05 gram. Record this weight and fill
the bucket to exactly the same weight, +/- 0.05
gram, for each test. Use distilled water, adjusted
to 2 to 5 C below the jacket temperature of the
calorimeter.
By Volume 2.
A 450 mL glass pipet (P/N 167HW3) is offered a.
for use with the 6510 and 1563A Water Han-
dling Systems. Temperature controlled water
flows continuously through the glass delivery
pipet and back to the tank to maintain a con-
stant water temperature in the pipet for filling
the calorimeter bucket with repeatable volumes.
Flow through the pipet stops when the stopcock
is opened to fill the calorimeter bucket. The
pipet refills automatically when the stopcock is
turned back to a closed position.
Alternatively, the bucket may be filled volu- b.
metrically using a bottle top dispenser capable
of delivering 450 ml with sufficient precision
(0.1%).
Transfer the bucket to the calorimeter and set it in 3.
place in the oval air can.
Slide one ignition connector onto the central termi- 4.
nal on the bomb head and push it downward as far
as it will go. Then grasp the bomb with forceps or
with a wire hook and lower it into the bucket. Slide
the other connector onto the terminal inside the
bucket.
Close the calorimeter cover and start the test. The 5.
calorimeter will automatically report the EE value
or heat of combustion, as selected, at the end of the
test.
Analyzing the Results
After obtaining a final reading; open the calorim- 1.
eter, lift the bomb out of the twin-chambered bucket
and remove the ignition cords. Release the bomb
pressure over a period of about one minute.
After all pressure has been released, open the bomb 2.
and examine the inside of the cup and the underside
of the head for any unburned sample or soot.
If evidence of incomplete combustion is found, a.
the test is not valid and will have to be repeated.
(Note: In some cases it may be impossible to get
an absolutely clean combustion without leaving
a slight carbon smear in the bomb.)
If the residue is estimated to weigh less than b.
0.1 milligram, the test may still be acceptable
since the error introduced will be well within the
obtainable precision for the instrument.
Remove all unburned pieces of fuse wire from the 3.
bomb head.
The fuse correction applied by the calorimeter is a.
calculated as:
e3 = (fuse value)(fuse multiplier)
Example:
If the fuse multiplier is set to 1, the fuse value must be
entered in calories.
If the fuse value is to be entered in as length in centimeters
and the Parr 45C10 fuse wire is being used, the fuse multi-
plier must be 2.3 cal / cm.
If platinum wire was used, collect and save the b.
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1109A
SEMI-MICRO
OXYGEN BOMBS
platinum scraps for recycling. Since platinum
does not oxidize under bomb conditions, there
is no calorimeter correction for its combustion,
but there is finite energy input obtained from
the electrical energy used to heat the wire. This
correction amounts to 1 (IT) calorie when using
Parr 45C3 Platinum Wire with a firing current
obtained from the ignition circuit in the calorim-
eter.
Determine the net corrected temperature rise, T, and 4.
calculate the gross heat of combustion by substitu-
tion in the following equation:

Where:
Hg = gross heat of combustion in calories per
gram
W = energy equivalent of the calorimeter in calo-
ries per degree Celsius (determined as described
under Standardization)
f = correction for fuse in calories
Additional corrections for the heat of formation of 5.
nitric and sulfuric acids can be applied as described
in the calorimeter manuals, but they may not be
significant for most semi-micro samples. A typical
value for the nitric acid corrections is 1.5 calories.
Standardization
The energy equivalent, W, of the calorimeter and 1.
its contents is determined by running a series of
tests with a standard material, such as benzoic acid,
which releases a known amount of energy.
The W value can then be calculated by dividing the 2.
known energy input by the corrected temperature
rise, T. A supply of calorific grade benzoic acid in
1/4 diameter pellets is furnished for this purpose.
Additional supplies can be obtained using Parr
Catalog number 3414.
Standardize the calorimeter by running a series of 3.
tests with calorific grade benzoic acid using samples
weighing between 0.18 0.22 grams and following
the procedure described for a calorific determina-
tion. Obtain T and compute the energy equivalent
as follows:

Where:
m = mass of the sample in grams
f = correction for fuse in calories
The value, 6318, in the above equation is the heat of 4.
combustion of calorific grade benzoic acid in (IT)
calories per gram. (Using the thermochemical calo-
rie in thermochemistry, this value would be 6323
calories per gram). The 6200 and 6100 Calorimeter
will perform these calculations for both standardiza-
tions and determinations automatically.
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1109A
SEMI-MICRO
OXYGEN BOMBS
MAINTENANCE
The Parr 1109A Semi-micro Oxygen Bomb will give
long service if handled with reasonable care, but the
user should remember that the bomb is subject to stress
and its mechanical condition must be monitored. Any
parts, which show a sign of deterioration, should be
replaced before failure occurs.
Do not fire the bomb if gas bubbles or other signs of a
possible leak appear when the bomb is submerged in
water. Disassemble the bomb and install new seals im-
mediately.
Note: Never use lubricants on bomb parts or fittings in
contact with high-pressure oxygen.
Tightening the 411A3 Terminal Nut can sometimes
stop a gas leak through the central electrode; however a
leak in this area usually indicates that the 528A insula-
tor has deteriorated and must be replaced. Failure of
this insulator can also result in a short circuit in the igni-
tion system.
Parr offers a clamp which would be placed in a vice to
support the head of the semi-micro oxygen bomb while
servicing the unit. This part number is 534A.
Recommended Parts to Change After 500 Firings
1109A (Manual Check Valve)
Part Number Unit
251AC pk of 12
531AJB pk of 12
659DD pk of 12
663DD ea
528A ea

If there is a leak from the A168AC fitting, replace the
entire fitting which includes the 160AC gasket and
238A O-ring.
Parr 1109A Oxygen Bombs are made from alloys that
will withstand most corrosive gases, but halides in the
presence of moisture are not well tolerated. If samples
yielding appreciable amounts of these elements are
burned in the 1109A bomb, the interior surfaces may
be etched or corroded. This effect can be minimized
by emptying and washing the bomb as soon as possible
after firing. Light corrosion products and foreign matter
can be removed by polishing with an abrasive cloth.
Parr provides oxygen bomb repair services for the
1109A. A factory test is recommended after 5000 fir-
ings. This includes replacing all of the seals, checking
the dimensions of the cylinder, screw cap and head,
hydrostatically testing the seals and proof firing the ves-
sel using benzoic acid.
When returning a bomb to the factory, ship it to:
Parr Instrument Company
Attn: Repair Department
211 53rd Street
Moline, IL 61265-1720
Include a Purchase Order to cover the cost of the repair,
a person to contact (complete with a phone number)
and return shipping information. Individual repair
parts can be ordered from any Parr dealer or direct from
the factory.
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1109A
SEMI-MICRO
OXYGEN BOMBS
PARTS LIST
1109A Oxygen Bomb
Part No. Description
A530A2 Head Assembly w/ Manual Valve
A168AC Manual Valve Cap Assembly
525A Bare Head
532A Cylinder
529A Screw Cap
531AJB O-ring, 1 1/16 ID Buna-N
23AC Electrode Hooks
Accessories
Part No. Description
3414 0.2g benzoic acid (100 count)
45C10 Fuse Wire, 10 cm
A19A14 Fill Connection
357HC O-ring for Fill Connection
208AC Inconel Fuel Capsule
169AC Platinum Capsule
45C3 Platinum Fuse Wire
165AC2 Platinum Capsule Support Loop
165AC2GE Capsule Support Look Ni-Cr
Oxygen Fill Connection
357HC O-ring FKM
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1109A
SEMI-MICRO
OXYGEN BOMBS
DRAWINGS
Figure 4 1109A Semi-micro Oxygen Bomb, Electrodes
Figure 5 1109A Semi-micro Oxygen Bomb, Cut-away View
Figure 6 Parts Diagram for the 1109A Manual Valve
Figure 4
1109A Semi-micro Oxygen Bomb, Electrodes
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1109A
SEMI-MICRO
OXYGEN BOMBS
Figure 5
1109A Semi-micro Oxygen Bomb, Cut-away View
P a r r I n s t r u m e n t C o m p a n y
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1109A
SEMI-MICRO
OXYGEN BOMBS
Figure 6
Parts Diagram for the 1109A Manual Valve
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1109A
SEMI-MICRO
OXYGEN BOMBS
Parts Key for the 1109A Manual Valve
211 53rd Street
Moline, Illinois 61265 USA
Phone: 1-309-762-7716 or 1-800-872-7720
Fax: 1-309-762-9453
E-mail: parr@parrinst.com
http://www.parrinst.com
Parr Instrument Company
Revision 01/29/10