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204M

Parr Instrument Company

1341 Plain Jacket Calorimeter


Operating Instruction Manual
Parr Instrument Company
TABLE OF CONTENTS

PREFACE  3 MAINTENANCE  12
Scope  3 Calorimeter Maintenance  12
Related Instructions  3 General Cleaning Instructions  12
Important Information  3 Fuse Ratings  12
Intended Usage  3 Electric Ignition Problems  12
Explanation of Symbols  4
Safety Information  4 6772 CALORIMETRIC THERMOMETER  13
General Specifications  4
Environmental Conditions  4
DRAWINGS  14
Provisions for Lifting and Carrying  4
1341 with 6775 & 2901 Electrical Hookup Diagram  14
1341 with 6772 Electrical Hookup Diagram  14
ASSEMBLE THE CALORIMETER  5
Parts for the 1341 Calorimeter  15

OPERATING THE CALORIMETER  6


Operating the 1108 Oxygen Combustion Vessel  6 CUSTOMER SERVICE
Operating the 1341 Calorimeter  6
Questions concerning the installation or operation
CALCULATING THE HEAT OF COMBUSTION  8 of this instrument can be answered by the Parr
Customer Service Department:
Assembly of Data  8
Temperature Rise  8 1-309-762-7716 • 1-800-872-7720
Gross Heat of Combustion  9 parr@parrinst.com • www.parrinst.com
Conversion to Other Bases  9
PRODUCT REGISTRATION & CUSTOMER SATISFACTION
STANDARDIZING THE CALORIMETER  10
The Energy Equivalent Factor  10 Parr’s Product Registration and Customer Satisfaction
Standard Samples  10 Survey can be found by visiting our website at:
www.parrinst.com/support/product-registration
Standardization Procedure  10
Register your equipment with us so you can receive:
DISCUSSION OF CALCULATIONS  11 • Notification of Product Updates
• Free Software Upgrades
Acid Correction  11 • New Product Information
Sulfur Correction  11
Please complete our Customer Satisfaction Survey so
Fuse Wire Correction  11 that we may better serve you. Your feedback helps
Radiation Correction  11 us improve our products and customer service.
Magnitude of Errors  12

2 Parr Instrument Company


1341 Plain Jacket Calorimeter
PREFACE

Scope Important Information


These instructions cover the steps to be taken Your Parr 1341 Plain Jacket Calorimeter has been
in setting up and operating a Parr 1341 Plain designed with function, reliability, and safety in
Jacket Calorimeter. The user should study these mind. It is your responsibility to install it in confor-
instructions carefully before starting to use the mance with local electrical codes.
calorimeter so that they will fully understand the
capabilities of the equipment, and be well aware of This manual contains important operating and safety
the safety precautions to be observed in its opera- information. You must carefully read and understand
tion. Instructions covering the operation of the 1108 the contents of this manual prior to the use of this
Oxygen Combustion Vessel and the use of other re- equipment. For safe operation, please pay attention
lated apparatus are provided in separate instruction to the alert signals throughout the manual.
manuals listed below. The separate manuals which
apply to a particular calorimeter installation should Intended Usage
be added to and made a part of these instructions.
Do not use this equipment for anything other than
its intended usage. Protection provided by the
Note About Nomenclature: Historically, burn- equipment may be impaired if used in a manner
ing a sample enclosed in a high pressure not specified by Parr Instrument Company. This
oxygen environment is known as Oxygen Bomb instrument is to be used indoors.
Calorimetry and the vessel containing the sam-
ple is known as an Oxygen Bomb. The terms
bomb and vessel are used interchangeably.

Related Instructions
No. Description
205M Operating Instructions for the 1108 Series
Oxygen Combustion Vessel
207M Analytical Methods for Oxygen Bombs
545M Operating Instructions for 6775/6775A
Digital Thermometer
201M Limited Warranty

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Parr Instrument Company
PREFACE (CONTINUED)

Explanation of Symbols General Specifications


Electrical Ratings
This CAUTION symbol may be present Plain Jacket Calorimeters:
on the Product Instrumentation and Model 1341EB: 115 VAC, 0.30 Amps, 60 Hz
literature. If present on the product, the Model 1341EE: 230 VAC, 0.15 Amps, 50/60 Hz
user must consult the appropriate part
of the accompanying product literature Ignition Units:
for more information. 2901EB: 115 VAC, 50/60 Hz, 4.0 Amps
2901EE: 230 VAC, 50/60 Hz, 2.0 Amps
Protective Earth (PE) terminal. Provided 2901EU: 230 VAC, 50/60 Hz, 2.0 Amps
for connection of the Protective Earth 2901EX: 230 VAC, 50/60 Hz, 2.0 Amps
(green or green/yellow) supply system 2901EZ: 230 VAC, 50/60 Hz, 2.0 Amps
conductor.
Before connecting the calorimeter to an electrical
outlet, the user must be certain that the electrical
Safety Information outlet has an earth ground connection and that the
To avoid electrical shock, always: line, load and other characteristics of the installa-
1. Use a properly grounded electrical outlet of tion do not exceed the following limits:
correct voltage and current handling capability.
Voltage: Fluctuations in the line voltage should not
2. Ensure that the equipment is connected to exceed 10 % of the rated nominal voltage shown on
electrical service according to local national the data plate.
electrical codes. Failure to properly connect
may create a fire or shock hazard. Frequency: Calorimeters can be operated from
either a 50 Hz or 60 Hz power supply without affect-
3. For continued protection against possible
ing their operation or calibration.
hazard, replace fuses with same type and rating
of fuse. Current: The total current drawn should not exceed
4. Disconnect from the power supply before the rating shown on the data plate on the calorim-
maintenance or servicing. eter by more than 10 %.

To avoid personal injury:


Environmental Conditions
1. Do not use in the presence of flammable or
combustible materials; fire or explosion may Operating: 15 ºC to 40 ºC; maximum relative hu-
result. This device contains components which midity of 80 % non-condensing.
may ignite such material. Installation Category II (over voltage) in accordance
2. Refer servicing to qualified personnel. with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25 ºC to 65 ºC; 10 % to 85 % relative humidity.

Provisions for Lifting and Carrying


Before moving the instrument, disconnect all
connections from the rear of the apparatus. Lift the
instrument by grabbing underneath each corner.

4 Parr Instrument Company


1341 Plain Jacket Calorimeter
ASSEMBLE THE CALORIMETER

1. Unpack the calorimeter carefully and check 5. Check the calorimeter bucket, noting the three
the individual parts against the packing list. If dimples in the bottom of the bucket which rest
shipping damage is discovered, report it im- on supporting pins in the bottom of the jacket.
mediately to the delivering carrier. Unpack The single dimple must always face forward
the jacket first and set it on a sturdy bench or when setting the bucket in the jacket.
table in a location that is reasonably free from
drafts and is protected from sources of radiant 6. Connect the ignition unit. While any electrical
heat, preferably in an air conditioned room. system capable of furnishing approximately
Temperature changes in the room should be 23 V can be used to ignite the fuse in the oxy-
minimal. gen combustion vessel, most users will prefer
to use a Parr 2901 Ignition Unit for this purpose.
There should be convenient access to running This unit operates from any standard electrical
water, to a drain and to an appropriate grounded outlet to provide the proper low voltage firing
electrical outlet. About 0.75 m2 (8 ft2) of work- current, providing also a convenient push
space will be required. Access to a chemical switch, indicating lamp and connecting termi-
balance sensitive to 0.1 mg and to a solution, nals.
trip or torsion balance capable of weighing up to
3.0 kg with 0.1 g sensitivity will be required. The Connect one of the lead wires from the calo-
1341 Calorimeter requires availability of oxygen, rimeter jacket to the terminal labeled “10CM”.
99.5 % purity, with appropriate connection, Connect the second lead to the terminal labeled
2500 psig, maximum. “Common”. Plug the power cord into an appro-
priately grounded electrical outlet. The power
2. Set the cover on the jacket. Remove the two supply cord is the main electrical disconnect
screws from the side of the jacket and attach device for the ignition unit. After the unit has
the stirrer drive motor. Check the stirrer shaft to been plugged into an outlet do not press the
be sure that it turns freely and slip the drive belt firing button unless the lead wires inside the
onto the motor and stirrer pulleys. jacket are connected to the combustion vessel.

3. Assemble the cover support stands. Two


stands are furnished, each consisting of a base, CAUTION! If the bare terminals on
a support rod and ring to be clamped to the these wires happen to be in contact
upper end of the rod. The A37A stand with the with each other or with a metal object
large ring is used to support the calorimeter when the circuit is closed, the result-
cover when it is removed from the jacket, while ing short-circuit may cause serious
the A38A stand with the smaller ring supports damage to the ignition system.
the combustion vessel head when attaching the
fuse wire and arranging the fuel capsule. 7. Attach the oxygen filling connection. Unscrew
the protecting cap from the oxygen tank and in-
4. Install the thermistor by sliding it through the spect the threads on the valve outlet to be sure
opening in the calorimeter cover. Adjust the they are clean and in good condition. Place the
length of the thermistor to match the length of ball end of the 1825 Oxygen Filling Connection
the stirring shaft. Hand tighten the nut to secure into the outlet socket and draw up the union
the thermistor. DO NOT OVER TIGHTEN THE NUT. nut tightly with a wrench, keeping the 0-55 atm
Once installed, the thermistor can remain gauge in an upright position.
attached to the cover during all operations. Do
not lay the cover on the tabletop. Always set Operating instructions for the 1825 Oxygen Filling
it in the supporting ring on the A37A stand to Connection are provided in Instruction Manual
protect the thermistor and stirring shafts. 205M for the 1108 Oxygen Combustion Vessel.

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Parr Instrument Company
OPERATING THE CALORIMETER

Operating the 1108 Oxygen Combustion 5. Let the stirrer run for 5 minutes to reach equi-
Vessel librium before starting a measured run. At the
end of this period record the time on the timer
Detailed instructions for preparing the sample and
of the 6775 Digital Thermometer and read the
charging the 1108 Oxygen Combustion Vessel are
temperature.
given in Instruction Manual, No. 205M. Follow these
instructions carefully, giving particular attention to the 6. Read and record temperatures at one-minute
precautions to be observed in charging and handling intervals for 5 minutes. Then, at the start of the
the oxygen combustion vessel. 6th minute…

7. Stand back from the calorimeter and fire the


Operating the 1341 Calorimeter
combustion vessel by pressing the ignition button
All operations required to test a sample or to stan- and holding it down for 2 s. Normally the indica-
dardize the 1341 Plain Jacket Calorimeter should tor light will glow for only about 0.5 s but release
proceed step-wise in the following manner: the button within 5 s regardless of the light.
1. Prepare the sample and charge the oxygen
CAUTION! Do not have the head,
combustion vessel as described in Instruction
hands or any parts of the body over
Manual No. 205M. the calorimeter when firing the com-
2. Fill the calorimeter bucket by first taring the dry bustion vessel; and continue to stand
bucket on a solution or trip balance; then add clear for 30 seconds after firing.
2 kg ± 0.5 g of water. Distilled water is preferred,
but demineralized or tap water containing less 8. The bucket temperature will start to rise within
than 250 mg/L (250 ppm) of dissolved solid is 20 seconds after firing. This rise will be rapid
satisfactory. The water temperature should be during the first few minutes; then it will become
approximately 1.5 °C below room temperature, slower as the temperature approaches a stable
but this can be varied to suit the operator’s maximum as shown by the typical temperature
preference. It is not necessary to use exactly rise curve below. It is not necessary to plot a
2 kg, but the amount selected must be duplicated similar curve for each test, but accurate time and
within ± 0.5 g for each run. Instead of weighing temperature observations must be recorded to
the bucket it can be filled from an automatic pipet identify certain points needed to calculate the
or from any other volumetric device if the repeat- calorific value of the sample.
ability of the filling system is within ± 0.5 mL and
the water temperature is held within a 1 ºC range. 9. Measure the time required to reach 60 % of the
total rise by estimating the temperature at the
3. Set the bucket in the calorimeter. Attach the 60 % point and observing the time when the
lifting handle to the two holes in the side of the temperature reading reaches that point. If the
screw cap and partially lower the combustion 60 % point cannot be estimated before ignition,
vessel in the water. Handle the vessel carefully take temperature readings at 45, 60, 75, 90 and
during this operation so that the sample will not 105 seconds after firing and interpolate between
be disturbed. Push the two ignition lead wires these readings to identify the 60 % point after the
into the terminal sockets on the vessel head. total rise has been measured.
Orient the wires away from the stirrer shaft
so they do not become tangled in the stirring 10. After the rapid rise period (about 4 or 5 minutes
mechanism. Lower the vessel completely into after ignition) record temperatures at one minute
the water with its feet spanning the circular boss intervals until the difference between successive
in the bottom of the bucket. Remove the lifting readings has been constant for five minutes.
handle and shake any drops of water into the Usually the temperature will reach a maximum;
bucket and check for gas bubbles. then drop very slowly. But this is not always true
since a low starting temperature may result in a
4. Set the cover on the jacket. Turn the stirrer by slow continuous rise without reaching a maxi-
hand to be sure that it runs freely; then slip the mum. As stated above, the difference between
drive belt onto the pulleys and start the motor. successive readings must be noted and the
Turn on the 6775 Digital Thermometer. readings continued at one-minute intervals until

6 Parr Instrument Company


1341 Plain Jacket Calorimeter
OPERATING THE CALORIMETER (CONTINUED)

Graph displaying typical temperature rise curve

the rate of the temperature change becomes 13. Wash all interior surfaces of the combustion
constant over a period of 5 minutes. vessel with a jet of distilled water and collect the
washings in a beaker.
11. After the last temperature reading, stop the mo-
tor, remove the belt and lift the cover from the 14. Remove all unburned pieces of fuse wire from
calorimeter. Wipe the thermistor shaft and stirrer the combustion vessel electrodes; straighten
with a clean cloth and set the cover on the A37A them and measure their combined length in
support stand. Lift the combustion vessel out of centimeters. Subtract this length from the initial
the bucket; remove the ignition leads and wipe length of 10 cm and enter this quantity on the
the vessel with a clean towel. data sheet as the net amount of wire burned.
Alternatively, the correction in calories is located
12. Open the knurled knob on the oxygen combus- on the card of the 45C10 fuse wire.
tion vessel head to release the gas pressure be-
fore attempting to remove the cap. This release 15. Titrate the combustion vessel washings with a
should proceed slowly over a period of not less standard sodium carbonate solution using meth-
than one minute to avoid entrainment losses. yl orange or methyl red indicator. A solution of
After all pressure has been released, unscrew the 0.0709 N sodium carbonate is recommended for
cap; lift the head out of the cylinder and place it this titration to simplify the calculation. This is
on the support stand. Examine the interior of the prepared by dissolving 3.76 g of Na2CO3 in water
vessel for soot or other evidence of incomplete and diluting to 1L. NaOH or KOH solutions of the
combustion. If such evidence is found, the test same normality may be used.
will have to be discarded.
16. Analyze the combustion vessel washings to
determine the sulfur content of the sample if it
CAUTION! Do not have any part of exceeds 0.1 %. Methods for determining sulfur
the body in the pressure relief path. are discussed in Instruction Manual No. 207M.

www.parrinst.com 7
Parr Instrument Company
CALCULATING THE HEAT OF COMBUSTION

Assembly of Data Temperature Rise


The following data should be available at the com- Compute the net corrected temperature rise, t, by
pletion of a test in a 1341 calorimeter: substituting in the following equation:

t = tc - ta - r1 · (b-a) - r2 · (c-b)
a = time of firing, min

b = time (to nearest 0.1 min) when the tem- Thermochemical Corrections
perature reaches 60 % of the total rise, min Compute the following for each test:

c = time at beginning of period (after the tem-


e1 = correction for heat of formation of nitric
perature rise) in which the rate of tempera-
acid (HNO3), cal
ture change has become constant, min
(numerically equal to c1 if 0.0709 N alkali
ta = temperature at time of firing, °C
was used for the titration)
tc = temperature at time c, °C

r1 = rate (temperature units per minute) at e2 = correction for heat of formation of sulfuric
which the temperature was rising during acid (H2SO4), cal
the 5 min period before firing, °C/min
e2 = 13.7 · c2 · m
r2 = rate (temperature units per minute) at which
the temperature was rising during the 5 min
period after time c. If the temperature was e3 = correction for heat of combustion of fuse
falling instead of rising after time c, r is wire, cal
negative and the quantity -r · (c-b) becomes
e3 = 2.3 · c3 when using Parr 45C10 NiCr
positive and must be added when comput-
fuse wire
ing the corrected temperature rise, °C/min
e3 = 2.7 · c3 when using 34 AWG iron fuse
c1 = volume of standard alkali solution used in
wire
the acid titration, mL

c2 = mass fraction of sulfur in the sample, in %

c3 = length of fuse wire consumed in firing, cm

W = energy equivalent of the calorimeter, deter-


mined under standardization, cal/°C

m = mass of sample, g

8 Parr Instrument Company


1341 Plain Jacket Calorimeter
CALCULATING THE HEAT OF COMBUSTION (CONTINUED)

Gross Heat of Combustion Conversion to Other Bases


Compute the gross heat of combustion, Hg, in The calculations described above give the calorific
calories per gram by substituting in the following value of the sample with moisture as it existed
equation: when the sample was weighed. For example, if an
air-dried coal sample was tested, the results will be
in terms of heat units per weight of air-dry sample.
t · W - e1 - e2 - e3
Hg = This can be converted to a moisture free or other
m dry basis by determining the moisture content of
the air-dry sample and using conversion formulae
Example: published in ASTM Method D3180 and in other
a = 1:44:00 references on fuel technology.

b = 1:45:24 The calorific value obtained in a calorimeter test


represents the gross heat of combustion for the
c = 1:52:00 sample. This is the heat produced when the sample
burns, plus the heat given up when the newly
(b-a) = 1:45:24 - 1:44.0 = 1:24 = 1.4 min formed water vapor condenses and cools to the
temperature of the combustion vessel. In nearly
(c-b) = 1:52:00 - 1:45.24 = 6:36 = 6.6 min
all industrial operations this water vapor escapes
ta = 24.432 °C as steam in the flue gases and the latent heat of
vaporization which it contains is not available for
tc = 27.662 °C useful work. The net heat of combustion obtained
by subtracting the latent heat from the gross calo-
r1 = +0.010 °C / 5 min = +0.002 °C/min rific value is therefore an important figure in power
plant calculations. If the percentage of hydrogen, H,
r2 = -0.004 °C / 5 min = -0.001 °C/min in the sample is known, the net heat of combustion,
Hn in BTU/lb can be calculated as follows:
c1 = 23.9 mL

c2 = 1.02 % Sulfur 1.8 · Hg - 91.23 · H (ASTM D240)

c3 = 7.6 cm Parr 45C10 wire

W = 2426 cal/°C

m = 0.9936 g

t = 27.662 - 24.432 - (0.002 · 1.4) - (-0.001 · 6.6)

= 3.234 °C

e1 = 23.9 cal

e2 = 13.7 · 1.02 · 0.9936 = 13.9 cal

e3 = 2.3 · 7.6 = 17.5 cal

3.234 · 2426 - 23.9 - 13.9 - 17.5


Hg =
0.9936

= 7841 cal/g

= 1.8 · 7841 = 14,114 BTU/lb

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Parr Instrument Company
STANDARDIZING THE CALORIMETER

The Energy Equivalent Factor Standardization Procedure


The term “standardization” as used here denotes The procedure for a standardization test is exactly
the operation of the calorimeter with a standard the same as for testing a fuel sample. Use a pellet of
sample from which the energy equivalent or ef- calorific grade benzoic acid weighing not less than
fective heat capacity for the system can be deter- 0.9 g nor more than 1.25 g. Determine the corrected
mined. The energy equivalent factor (W) represents temperature rise, t, from the observed test data, also
the energy required to raise the temperature of titrate the combustion vessel washings to determine
the calorimeter one degree, usually expressed the nitric acid correction and measure the unburned
as calories per degree Celsius. This factor for the fuse wire. Compute the energy equivalent by substi-
1341 calorimeter with an 1108 Oxygen Combus- tuting in the following equation:
tion Vessel will usually fall within a range from
2410 cal/°C to 2430 cal/°C, with the exact value for H · m + e1 + e3
W =
each installation to be determined by the user. This t
requires a series of at least four standardization
tests (and preferably more) from which an average
can be taken to represent the true W value for the W = energy equivalent of the calorimeter,
user’s calorimeter. This will provide a factor which cal/°C
can be used with confidence in subsequent tests H = heat of combustion of the standard
with unknown materials. Standardization tests benzoic acid sample, cal/g
should always be repeated after changing any parts
of the calorimeter, and occasionally as a check on m = mass of the standard benzoic acid
both the calorimeter and the operating technique. sample, g

t = net corrected temperature rise, °C


Standard Samples
A bottle of 100 1 g benzoic acid pellets is furnished e1 = correction for heat of formation of
with each calorimeter for standardization purposes. nitric acid, cal
Additional benzoic acid pellets or powder can be
obtained from Parr. For high precision measure- e3 = correction for heat of combustion of
ments, a primary standard benzoic acid powder can the firing wire, cal
be purchased from the National Institute of Stan-
dards and Technology (NIST). The NIST also offers Example: Standardization with a 0.9998 g benzoic
standard 2,2,4-Trimethylpentane (Isooctane) as a acid sample (6318 cal/g) produced a net corrected
calorific standard for testing volatile fuels. temperature rise of 2.653 °C. The acid titration
required 11.9 mL of standard alkali and 8 cm of fuse
wire were consumed in the firing. Substituting in
CAUTION! Benzoic acid must always the standardization equation:
be compressed into a pellet before it
is burned in an oxygen combustion H = 6318 cal/g
vessel to avoid possible damage from
rapid combustion of the loose powder. m = 0.9998 g

e1 = (11.9 mL) · (1 cal/mL) = 11.9 cal


Compressing benzoic acid into a pellet is best
accomplished by using a Parr 2811 Pellet Press. If e3 = (8 cm) · (2.3 cal/cm) = 18.4 cal
a pellet press is not available, melt the powder into
a lump by heating it carefully to the melting point, t = 2.653 ºC
but do not overheat the powder as this will change
(6318 · 0.9998) + 11.9 + 18.4
the calorific value. W =
2.653

= 2392 cal/°C

10 Parr Instrument Company


1341 Plain Jacket Calorimeter
DISCUSSION OF CALCULATIONS

Acid Correction Fuse Wire Correction


Since combustion in the vessel takes place in an The wire used as a fuse for igniting the sample
atmosphere of nearly pure oxygen at high tempera- is partly consumed in the combustion. Thus the
ture and pressure, several reactions take place which fuse generates heat both by the resistance it offers
would not occur in burning the same material under to the electric firing current, and by the heat of
normal atmospheric conditions. These side reactions combustion of that portion of the wire which is
are important because they generate an appreciable burned. It can be assumed that the heat input from
amount of heat which cannot be credited to the the electric firing current will be the same when
sample, and for which a correction must be made. standardizing the calorimeter as when testing an
unknown sample, and this small amount of energy
For example, in the normal combustion of coal, all therefore requires no correction. However, it will
sulfur is oxidized and liberated as SO2 but nitrogen be found that the amount of wire consumed will
in the material usually is not affected. Likewise, no vary from test to test, therefore a correction must
change occurs in the nitrogen of the air required be made to account for the heat of combustion of
for normal combustion. But, when the same coal is the metal.
burned in the oxygen combustion vessel, oxidation
of the sulfur is carried further to form SO3 which The amount of wire taking part in the combustion
combines with water vapor to form H2SO4; and some is determined by subtracting the length of the re-
of the nitrogen in the combustion vessel is also covered unburned portion from the original length
of 10 cm. The correction is then computed for the
oxidized and combined with water vapor to form
burned portion by assuming a heat of combustion
HNO3. These two side reactions result in acids within
of 2.3 cal/cm for Parr 45C10 (No. 34 B & S gauge
the combustion vessel and require a correction to “Chromel C”) wire, or 2.7 cal/cm for No. 34 B & S
account for the heat liberated in their formation. gauge iron wire.

In computing the correction for acid formation it


is assumed that all of the acid titrated is nitric acid Radiation Correction
(HNO3), and that the heat of formation of 0.1 N HNO3 The method recommended for calculating the
under combustion conditions is -14.1 kcal/mol. correction for heat gain or loss from a plain jacket
Obviously, if sulfuric acid is also present, part of the calorimeter is that specified by the American
correction for H2SO4 is included in the nitric acid cor- Society for Testing and Materials as published
rection. The sulfur correction described below takes under ASTM Designations D240 and D3286. It is
care of the difference between the heats of forma- based upon the work of Dr. H.C. Dickinson at the
tion of nitric and sulfuric acids. National Bureau of Standards who showed that
the amount of heat leak during a test could be
Sulfur Correction approximated by assuming that the calorimeter is
heated by its surroundings during the first 63 % of
A correction of 1.4 kcal must be applied for each the temperature rise at a rate equal to that mea-
gram of sulfur converted to sulfuric acid. This sured during the 5 minute preperiod. The method
is based upon the heat of formation of 0.17 N then assumes that the cooling (or heating) rate
H2SO4 which is -72.2 kcal/mol, but a correction of during the remaining 37 % of the rise is the same
2 · 14.1 kcal/mol of sulfur is included in the nitric as the rate observed during the 5 minute postpe-
acid correction. Therefore the additional correction riod. For most experimental work the dividing
which must be applied for sulfur will be: point between these two periods is taken as that
point in time, b, when the temperature has reached
72.2 - (2 · 14.1) or 44.0 kcal/mol, or 1.37 kcal/g of sulfur six-tenths (instead of 63 %) of the total rise. Note
For convenience, this is expressed as 13.7 cal for that these two time intervals must be expressed in
each percentage point of sulfur per gram of sample. minutes and decimal fractions (Example: 1.4 min
and 6.6 min).

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Parr Instrument Company
DISCUSSION OF CALCULATIONS (CONT.) MAINTENANCE (CONT.)

Magnitude of Errors General Cleaning Instructions


The following examples illustrate the magnitude Wipe exterior surfaces with lightly dampened cloth
of errors which may result from faulty calorimeter containing mild soap solution.
operations. They are based upon an assumed test
in which a 1.0000 g sample produced a 2.800 ºC
Fuse Ratings
temperature rise in a calorimeter having an energy
equivalent of 2400 cal/°C. The replacement of protective fuses should be
performed by qualified personnel.
• An error of 1 mL in making the acid titration will Part No. 139E21 used in Ignition Unit 2901EB:
change the thermal value 1.0 cal. Slow blow, 5.0 Amps, 250 VAC
• An error of 1 cm in measuring the amount of Part No. 139E8 used in Ignition Unit 2901EE:
fuse wire burned will change the thermal value Slow blow, 2.5 Amps, 250 VAC
2.3 cal.

• An error of 1 g in measuring the 2 kg of water Electric Ignition Problems


will change the thermal value 2.8 cal. If the indicator light does not come on when the
firing button is pressed on the ignition unit there
• An error of 1 mg in weighing the sample will is either an open circuit in the system, the light is
change the thermal value 6.7 cal. burned out, or a fault on the A1580E circuit board.
• An error of 0.002 ºC in measuring the tempera- An open circuit can usually be located with an ohm-
ture rise will change the thermal value 4.8 cal. meter. Flex the lead wires during any continuity
check as the wires may be broken and making only
If all of these errors were in the same direction, the intermittent contact. If the red indicator light glows
total error would be 17.6 cal. during ignition but the fuse wire does not burn, check
the system for a voltage leak to ground, most likely
in the insulated electrode on the combustion vessel
head. Check the electrode using the high impedance
MAINTENANCE scale on an ohmmeter and replace the electrode
insulator and seal if leakage is indicated.
Calorimeter Maintenance
The high polished chrome finish on the calorimeter If test methods for hazardous materials require the
bucket is needed to minimize heat transfer. If this operator to stand away from the calorimeter when
finish becomes dull, the bucket should be replaced. firing the combustion vessel, move the ignition unit
Also check the bucket stirrer frequently to be sure to a protected location and add longer wires to the
that it turns freely. Any drag or friction in the stirrer calorimeter. Although remote firing is not neces-
will cause slow and erratic temperature response sary for most samples, the operator should always
in the calorimeter. Add a few drops of machine oil step back from the calorimeter when firing the
annually to the small hole in the top of the stirrer combustion vessel.
assembly. Move the shaft of the assembly up and
down to distribute the oil thoroughly.
CAUTION! Do not have the head,
hands or any parts of the body over
the calorimeter when firing the
combustion vessel; and continue to
stand clear for 30 seconds after firing.

12 Parr Instrument Company


1341 Plain Jacket Calorimeter
6772 CALORIMETRIC THERMOMETER

To improve the precision and simplify the procedure for measuring and recording the temperature
rise in a 1341 Calorimeter, Parr offers the 6772 Calorimetric Thermometer. Readings are taken with
a thermistor sealed in a stainless steel probe. This two-channel precision calorimetric thermometer
features Parr’s newest generation microprocessor control. The thermometer uses a Linux operating
system with communication and file management systems comparable to a PC. A bright, color,
touch screen display and data input system utilizes a graphical interface for easy instrument setup
and operation. A USB port is available for use with a balance, printer, or barcode reader. (For more
information on barcode capability, please contact Parr’s sales staff.) An Ethernet port is available for
data transfer using TCP/IP communications. No additional ignition source is required as the 6772
Calorimetric Thermometer acts as an ignition unit.

Specifications:
• Thermistor Probe
• One Probe – Standard
• Two Probes – Optional
• 0.0001 °C Temperature Resolution
• Absolute Accuracy:
±0.1 °C (without calibration)
±0.05 °C (with calibration)
• Repeatability:
±0.002 °C (Single Point)
• Linearity:
±0.002 °C (10 °C Span)
• Ethernet network communications
• Balance & Printer Port: USB
• Updates via the Internet

Please refer to Parr Bulletin 6700 for complete


details on the 6772 Calorimetric Thermometer.

www.parrinst.com 13
Parr Instrument Company
DRAWINGS

1341 with 6775 & 2901 Electrical Hookup Diagram

1341 1168E2
CALORIMETER THERMISTOR PROBE
(BUCKET)

POWER CORD
34E2 (115V)
1203EEE (10A/220V CONT EU)
2198EEE (10A/250V BRAZIL)
1981EEE (10A/220V CHINA)
1202EEE (13A/250V BS PLUG)

IGNITION LEAD WIRES 2901E SERIES


IGNITION UNIT

POWER CORD
34E2 (115V) 6775
1203EEE (10A/220V) DIGITAL THERMOMETER

1341 with 6772 Electrical Hookup Diagram

1341
CALORIMETER 1168E2 THERMISTOR PROBE (BUCKET)

1759
PRINTER
6772
A2170E USB PORT CALORIMETRIC
PRINTER CABLE THERMOMETER

POWER CORDSET
A719E (115V)
ETHERNET 1200EEE (250V, CONT EU)
PORT 1456EEE (220V)
2121EEE (250V, BRAZIL)

IGNITION LEAD WIRES

EXTENSION CORD
A1877E (115V)
A1877E2 (230V)
A1877E3 (230V EURO)

14 Parr Instrument Company


1341 Plain Jacket Calorimeter
DRAWINGS (CONTINUED)

Parts for the 1341 Calorimeter


Key No. Part No. Description
A50MEB Motor Assembly with Pulley, 115V 60 Hz
1
A50MEE Motor Assembly with Pulley, 230V 50/60 Hz
2 355C Motor Pulley
3 37M2 Stirrer Drive Belt
4 A27A Stirrer Bearing Assembly with Stirrer Pulley
5 A468E Ignition Wire
6 A30A3 Stirrer Shaft with Impeller
7 A391DD Oval Bucket
8 A1100DD Calorimeter Jacket with Cover
9 1108 Oxygen Combustion Vessel 11
10 182VBAD Male Connector
11 1168E2 Thermistor

3 4
2 10
5
1

7 9

www.parrinst.com 15
204M R10 10/08/2021

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