Parr Instrument 1104 User Manual

1104
Oxygen Combustion Vessel
Operating Instruction Manual
209M
1104 Oxygen Combustion Vessel
Table of Contents
Scope — 3
Related Instructions — 3
Purpose — 3
Description — 3
Accessories and Utilities — 3
Sample Preparation
— 3
Operation
Setting the Calorimeter Parameters — 4
Preparing the Fuse When the Combustion Cage is Used — 5
Preparing the Fuse When the Combustion Cage is Not Used — 5
Closing the Bomb — 6
Filling the Bomb Using a Calorimeter — 6
Filling the Bomb Manually — 7
Maintenance
— 7
Parts List
— 8
Drawings
1104 Oxygen Combustion Vessel — 9
1104 Oxygen Combustion Vessel - Head Assembly
— 10
Oxygen Filling Connection for the 1104 Oxygen Combustion Vessel — 11
Note About Nomenclature:
Historically, burning a sample enclosed in a high pressure oxygen environment is known as Oxygen Bomb Calorimetry and the vessel containing the sample is known as an Oxygen Bomb. The terms bomb and vessel are used interchangeably.
Customer Service
Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department:
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
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1104 Oxygen Combustion Vessel
Preface
Scope
These instructions cover the procedures to be fol-
lowed when using a Parr 1104 Oxygen Combustion Vessel (or bomb) to determine caloric values of
solid or liquid combustible material in a Parr calo­rimeter. The user should study these instructions carefully in order to obtain a complete understand­ing of the capabilities and limitations of an 1104
Oxygen Combustion Vessel, and to be well aware
of the precautions to be observed in its operation. Calorimeter operations and the operation of various
oxygen vessel accessories are described in separate instruction manuals listed below, copies of which
are available upon request.
Related Instructions
The following Parr publications are also included to further your understanding of this instrument and its component parts:
No. Description
201M Limited Warranty
205M Operating Instructions for the 1108 Oxy-
gen Combustion Vessel
207M Analytical Methods for Oxygen Bombs
230M Safety Precautions to be observed when
operating Pressure Reaction Equipment
483M Introduction to Bomb Calorimetry
Purpose
The Parr 1104 Oxygen Combustion Vessel is de­signed for combustion tests of explosives and other fast burning, high-energy samples that burn with extreme violence. The bomb is also recommended
for use with materials whose combustion character­istics are unknown or unpredictable. 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 Vessel, which contains information con-
cerning sample preparation and other application information relevant to both vessel types.
Description
The 1104 Oxygen Combustion Vessel is a heavy­walled, 240 mL vessel. It will handle samples liberat-
ing up to 12,000 calories using an oxygen charging pressure up to 45 atm (665 psig). The sample is
contained in a combustion cage that is designed
to mufe the shock forces produced by explosive
samples. The capsule is anchored to the cage so the
explosion will not dislodge it.
Accessories and Utilities
A minimum 99.5% purity oxygen source
providing 420 psig (3 Mpa) of pressure to the bomb is required.
To ignite the sample, 10 cm of NiCr fuse wire
(P/N 45C10) per test is needed.
Sample Preparation
Samples to be burned in the 1104 Oxygen Combus­tion Vessel are held in a thick-walled capsule (P/N 217A) within a heavy combustion cage that serves
to muffle the shock forces produced by high-energy samples. While the combustion cage is essential
for fast burning, high-energy samples, it may not
be necessary to use the cage when testing samples which do not burn violently. In some cases it may be easier to secure complete combustion by substitut-
ing a lighter capsule (P/N 43AS) and omitting the
combustion cage. This substitution is described in the Operation section of these instructions.
Manual 205M, Operating Instructions for the 1108 Oxygen Combustion Vessel, contains valuable infor-
mation concerning sample preparation. As a basic
rule, the 1104 Oxygen Combustion Vessel should
never be charged with a sample that will liberate
more than 12,000 calories when burned in oxygen. Additionally, the oxygen charging pressure should never exceed 45 atm (665 psig). Samples of smoke-
less powder weighing up to 4 grams have been
burned in this bomb, but the requirements for safe
operation vary so widely with different materials that it is difcult to make general statements regard­ing allowable sample size. It is strongly recommend­ed that the user make preliminary combustions with
small samples, then increase the sample size and vary the oxygen pressure carefully to determine the
optimum charge.
Note: Although the high-strength of the bomb is reassuring when working with fast burning or explosive materials, the operator must ALWAYS remember that he is dealing with extreme pres­sure and shock forces that require the exercise of good judgment at all times.
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1104 Oxygen Combustion Vessel
Sample Preparation (continued)
It is not advisable to test true explosives in the presence of oxygen. Some of the end products of the explosion will be combustible in high-pressure oxygen, for example, mixed oxides of nitrogen and carbon monoxide. With high-pressure oxygen avail­able, these will burn to carbon dioxide and release
an undeterminable amount of heat that did not come from the initial reaction of interest. This sec­ondary combustion might give off nearly as much
energy as the preliminary explosion. To eliminate this concern, it is recommended that the user ll the
bomb with nitrogen and then release the valve to
ush the vessel, repeating this process twice. This will reduce the atmospheric oxygen trapped in the bomb to a level that is insignicant, relative to the
primary reaction. It is advisable to leave a residual pressure of at least 5 atmospheres on the bomb in order to seal the inlet check valve.
Operation
Setting the Calorimeter Parameters
When using the 1104 Oxygen Combustion Vessel in a calorimeter, the user must ensure that the correct
User ID is set in order to obtain the appropriate op­erating parameters. For the 6200 Isoperibol Calo-
rimeter, the User ID must be “62-1104”. For the 6100 Compensated Jacket Calorimeter, the User ID must be “61-1104”.
1. From the Main Menu in the 6000 Series calorim-
eter, select “Program Info & Control”
2. From Program Info & Control, select “User Setup ID”
3. Press “Clear”
4. Enter “62-1104” (or “61-1104”)
5. Press “Enter”
6. Press “Reload User Default Settings” and follow the instrument prompts
For older models, please contact Parr for the appro­priate software.
Bomb Head Assembly
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