FREQUENTLY ASKED QUESTIONS:
1. What does ChemiSens mean when they
refer to true zero-line and true measurement?
2. Automated chemistry. What is it according
to ChemiSens opinion?
3. Why does the CPA202 look different from most
other reaction calorimeters?
4. How do I determine Cp with the CPA202?
5. ChemiSens offers three different types of
reaction calorimeter systems. Why?
6. Can I operate differnt CPA systems with the
dynamic correction included on-line?
7. What are the special features of the ChemiSens
Heat-Balance systems?
8. The CPA202 is pre-calibrated once and for all.
Why do you then deliver it with a calibration heater?
9. Why is a small reactor volume important for
a reaction calorimeter?
10. Is a torque transducer really necessary
in a reaction calorimeter?
11. What are the special benefits of the CPA202
compared to traditional reaction calorimeters?
12. Can you point out some particular areas of
use where the CPA is really beneficial?
13. Is it complicated to operate the CPA202?
14. Is it time efficient to work with the CPA
systems?
15. Why is it important to get the result directly
on line in real time?
1. What does ChemiSens mean with true
zero-line and true measurement?
Answer:
The output from a true reaction calorimeter is a signal given in true
power units (watts) and directly describing the ongoing thermal activity
inside the reaction calorimeter. Without any activity the signal is always
zero, that’s a true zero-line. If the studied reaction generates
a power of XX watts, then the result presented on line should be exactly
XX watts, that’s true measurement.
2. Automated chemistry. What is it according
to ChemiSens opinion?
Answer:
ChemiSens systems and most other commercial reaction calorimeters include
automatic facilities for auxiliary sensors and multi line dosing capability.
According to ChemiSens automated chemistry means operations where all
necessary process steps can be fully pre-programmed and performed by the
system.
The necessity of stable dosing to a reaction calorimeter must always
be considered.
Most experiments in a reaction calorimeter are performed as semi-batch
operations. One or more reactants are continuously fed to the reactor.
With a high-resolution reaction calorimeter any irregular or unstable
dosing will be reflected in the measurements. The calorimeter system must
be able to handle any necessary dosing of reactants or sampling from the
reactor in an automatically controlled way that will not disturb any of
the measurements.
3. Why does the CPA202 look different from
most other reaction calorimeters?
Answer:
The CPA202 is from the beginning built as a reaction calorimeter with
all considerations to be a precision instrument. The reactor itself looks
very much like an ordinary small jacketed reactor. The sophisticated measuring
devices are located within the base part of the reactor vessel. When the
reactor is operating it must be submerged into the CPA thermostatting
unit. The thermostatting unit is necessary to establish a uniform thermal
surrounding for the reactor. Note that many traditional reaction calorimeters
look very different when they are used. They are wrapped in layers of
insulation or covered by a box or modified in other ways to improve the
measuring capability.
4. How do I determine Cp with the CPA202?
Answer:
There are principally two different ways. Either through a temperature
scanning experiment or through a stepwise change of the reactor temperature.
In both cases we recommend for the best results to run the experiment
with different amounts in the reactor and make a differential calculation.
For simple determinations a single experiment is sufficient.
5. ChemiSens offers three different types
of reaction calorimeter systems. Why?
Answer:
Our prime system, the CPA202 can solve most problems within reaction calorimetry.
For small-scale production or where larger product quantities are required
for further testing, the volume capacity of the CPA202 reactor might be
insufficient.
For these situations our complement is the CPA122 system.
Some routine tests might not require the sophisticated CPA202. In
these cases our CPA102 is a natural choice. The CPA102 is thermostatted
by circulating liquid in its jacket. The reactor, when it is operating,
is surrounded by air while a liquid surrounds the CPA reactor. In some
rare cases the “dry” surrounding of the RM200S reactor might
be favorable compared to the CPA102.
6. Can I operate different CPA systems
with the dynamic correction included on-line?
Answer:
Yes, it is possible. The dynamic correction compensates for the heat accumulated
in the reaction mass and strongly reduces the system time lag.
The heat-balance equation for any reaction calorimeter includes a
term q(acc) that describes the heat flow corresponding to the heat accumulated
in the reaction mass. In reality the heat balance equation for the whole
calorimeter must also include accumulation terms for the different inert
thermal masses of the reactor vessel. The CPA systems automatically corrects
for the heat accumulation in the known inert reactor masses. The reactor
temperature derivative is always calculated. If a value for the heat capacity
of the reaction mass is given, this value is multiplied by the temperature
derivative and used as the dynamic correction.
7. What are the special features with
the ChemiSens Heat-Balance systems?
Answer
ChemiSens offers two different heat-balance systems CPA122 and CPA102
as complement to the CPA202 system. The general problem with the heat-balance
technique is to measure the small temperature difference between the outlet
and inlet flow of the thermostatting liquid into the reactor jacket. ChemiSens
has solved this problem without lowering the flow rate of the thermostatting
media. A low flow rate promotes the measurement of the temperature difference
but also lowers the control capability of the reactor and might cause
reactor instability.
Another problem associated with the heat balance technique is its
sensitivity to disturbances from the surroundings. ChemiSens has included
separate sensors to measure and correct for these disturbances. The reactor
cover is separately heated to avoid internal reflux and uncontrolled heat
losses.
8. The CPA202 is pre-calibrated once and for
all. Why do you then deliver it with a calibration heater?
Answer:
The calibration heater is used for the regular system validation. The
heater is also used for the determination of the heat transfer properties
in non-reacting systems.
9. Why is a small reactor volume important
for a reaction calorimeter?
Answer:
In most cases the output from a reaction calorimeter is just information.
For that reason and the fact that the consumption of sometimes expensive
chemicals normally must be considered, the vessel volume should be as
small as possible. The minimum size is set by practical considerations.
The small volume of our reactor takes into account the space necessary
for all of the sensors, both standard and optional, that may be incorporated
into the system. The small volume also allows for scaled down reactor
conditions such as sampling, dosing of solids, handling of heterogeneous
systems, etc.
When studying reactions where energetic compounds are involved it
is obvious that the reactor size should be as small as possible.
10. Is it really necessary with a torque
transducer in a reaction calorimeter?
Answer:
Mostly yes. Besides being used as a correction in the measurement of the
total reaction power , the torque measurements also carry separate information.
Analyzing the torque graph gives valuable information about viscosity
changes due to fouling, precipitation, agglomeration, phase inversions
etc. This is important information for the understanding of the complete
process.
11. What are the special benefits with
the CPA202 compared to the traditional reaction calorimeters?
Answer:
The CPA202 presents both the true heat flow and the total reaction power
on line and in the real time. You get the true picture of the process
with all the details. No time has to be spent on calibration procedures.
There is no risk for hiding reactions below misinterpreted baselines.
12. Can you point on some particular areas
of use where the CPA202 is really beneficial?
Answer:
The CPA202 is really beneficial for studies of complicated systems. We
are then talking about reactions in media’s with changing viscosity
due to agglomeration, crystallization, fouling, polymerization, phase
inversions etc. Mass transfer controlled reactions can easily be examined
by changing the stirring intensity and watch the true result directly
on the screen.
13. Is it complicated to operate the CPA
systems?
Answer:
The menu system is user-friendly and self-instructing. The reactor is
a robust and reliable piece of hardware, easy to lift into or out from
the thermostatting unit. The open CPA102 and CPA122 reactor vessels can
be placed directly on the bench balance for charging initial material
for the experiment.
The reactor armature is easily reconfigured to meet the actual experimental
needs. The lid ports and the rest of the armature are compatible with
the Swagelok system from Crawford Fittings USA.
14. Is it time efficient to work with the
CPA202?
Answer:
Yes it is. You start your experiment directly, run it until you have got
the result and then interrupt. You have the true result on the screen
and in your log directly. There is no need for electrical calibration
pulses before the experiment, each time you change the temperature or
the stirring intensity and finally afterwards, when you think the reaction
is completed.
15. Why is it important to get the result
directly on line in the real time?
Answer:
It’s very time efficient. You get directly the correct response
to your changes of the experimental conditions. This is especially beneficial
for screening tests. The result/response from an addition or from a change
of experimental parameters can be used directly for planning the next
experimental step.
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