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Sponsor: Ken James

Advisor: Nate Cloud

CO2 Bulk Delivery System


Courtney Barkey, R. Chris Jones, D.J. Lee, Dennis McBrearty, Merrill Myers

Executive Summary
Supercritical Fluids Technologies, Inc. designs, manufactures, and implements supercritical fluid
extractors that serve to extract pure oils. SFT provides a full range of services in order to meet
the specific needs in supercritical fluid extraction and reaction science. The company currently
uses CO2 drawn from cylinders that contain 40 L of useable CO2 in the liquid phase. Issues have
been brought up due to the cost of the tank and the space occupied by cumbersome liquid
tanks. The approach to this problem is to use a vapor draw Dewar tank of CO2, which contains
300 L of CO2 mixture, at a fraction the cost of liquid tanks. In order to use the Dewar tank, CO2
will be drawn into a distillation system that will precede the SFT machinery. The primary
function of this design is to condense the CO2 to a liquid of high purity. Considerations for
safety and delivery conditions will shape the other aspects of the design. When completed, SFT
will be delivered a working prototype for use in their lab, with the potential for future
commercialization.

Team Supercritical Fluids


MEEG 401

Table of Contents
Executive Summary

Table of Contents

Introduction/Background

Project Scope

Refined Metrics

Concept Generation & Selection

Concept Overview

Methods

Subsystem Engineering

Design Specifications

Design Layout

Proof of Concept Test

Test Procedure

Results

10

Butane Condensation Test Results

10

Butane Condensation with Pumping Test Results

10

Post Heater Test Results

11

Conclusions

11

Path Forward

12

Future Testing

12

Prototype vs. Commercial Product

12

Appendices

13
2

Team Supercritical Fluids


MEEG 401
Introduction: Supercritical Fluid Technologies, Inc. (SFT) specializes in developing innovative solutions for
supercritical fluid extraction and reaction processes. A supercritical fluid exists when a substance is
pressurized and heated above its critical point. This unique phase allows for dual-property existence.
The supercritical fluid will experience the solvating property of a liquid while at the same time exhibiting
the diffusive property of a gas, making it an excellent candidate for extraction media. Some common
applications of supercritical fluid extraction can be seen in pharmaceuticals, neutraceuticals, polymers,
and reaction chemistry. Liquid CO2 is the extraction media used by Supercritical Fluid Technologies. This
team has been assigned to develop a CO2 delivery system that will provide CO2 from a bulk storage tank
to downstream SFT machinery at specified conditions.
SFT currently pulls pure liquid CO2 via a dip tube from 20 liter tanks (750 psi, 22C) and delivers directly
to their machinery. The liquid tanks must be of high purity, making them expensive. Large extraction
experiments may require up to 50 of the 20 L liquid CO2 tanks to fill the extraction machine.
Additionally, the 20 L capacity per tank means that they must be renewed often, creating a pile-up of
empty tanks in the lab.
SFT would like to use CO2 from a Dewar tank (250 psi, -20C) that contains 300 L of CO2 mixture. SFT
extraction machines require a 99.99% CO2 purity level, meaning that the CO2 cannot be directly fed into
SFT machinery. By drawing vapor CO2 from the Dewar tank, pure liquid can be produced via a distillation
process. The CO2 gas will be converted to pure liquid at a temperature and pressure of 10-22C and 1160
psi, respectively, to be accepted by and fed to SFT machinery. A working prototype will be designed and
implemented to carry out the aforementioned condensing and pressurizing process for the CO2 bulk
delivery system.
Project Scope: To design system that will condense and pressurize CO2 vapor output from a Dewar tank
and deliver it to downstream SFT machinery, eliminating the need for expensive and cumbersome liquid
tanks. A useable prototype will be constructed for proof of concept and commercial realization.
Refined Metrics: Top metrics considered for the system and their target values given in Table 1 below.
Rank
1
2
3
4
5
6
7

Metric
Delivery Temperature
Delivery Pressure
Cost of System
CO2 Delivery Time
Flow Rate
Size of System (Volume)
Weight of System

Target Value
10C - 22C
>80 bar
$20,000.00 $5,000.00
<30 min
Variable up to 250 ml/min
< 3ft x 3ft x 6ft
Can move on wheels

Table 1 Refined design metrics, ranked in order of importance.

Metrics were based upon the wants and constraints dictated by the sponsor as well as competitive
benchmarked products in the market. Downstream machinery was also considered. For example, the
CO2 delivery temperature and pressure were given a specified range for which the SFT machinery will
accept. Metrics will be validated following completion of proof of concept
3

Team Supercritical Fluids


MEEG 401
Concept Generation & Selection: The goal of this project is to enable Supercritical Fluid Technologies to
use a larger, less expensive Dewar tank instead of a liquid tank to feed the extraction machinery. The
main functions involved in the purification process are condensing and pressurizing. Design concepts
were generated to meet the following specifications: 10-22C, 1160 psi and flow rate up to 250mL/min.
Two significant differences arose between the various concepts. The first involved raising the pressure
by the use of a pump or a compressor. The second involved the use of an intermediate holding tank.
The CO2 gas can be pressurized and then condensed or vice versa. By first using a condenser, the CO2
will maintain near constant pressure of 250 psi while being cooled to the saturation temperature of
-25C. As soon as the saturation temperature is
crossed, the CO2 will be in liquid phase and can be
pumped up to the desired pressure of 1160 psi.
During the pumping stage, isentropic paths are
followed which run nearly parallel to isothermal
lines, allowing for a very efficient process (Figure
1). The alternative to the pumping system is a
compressor. If a compressor is first used to
increase pressure, isentropic lines run almost
perpendicular to the lines of constant
temperature and the path of the compressor
Figure 1 P-h diagram depicting the two process
must be longer to ensure exit from the saturation
options of the design: use of a pump versus
compressor.
phase.
Once the compression process is
completed, a condenser must be used to drop the temperature, but this line of enthalpy will be larger
than before (Figure 1). Therefore, it is more thermodynamically efficient to use a pumping system.
To provide a flow rate up to 250mL/min, a holding tank was considered following the pump. Overnight
storage arose as the main concern for implementing a holding tank. In adverse temperature conditions,
vapor expansion in the tank could become hazardous when left unattended, creating a safety hazard. To
combat this, an intricate control system would have to be used. Running a process time calculation, it
was determined that an intermediate holding tank would not be necessary to deliver at 250mL/min
since the process could be completed in under 30 seconds (see Appendix).
Concept Overview: The selected concept is shown as a schematic in Figure 2 below. For this concept,
vapor CO2 is 1) output from the Dewar tank, 2) goes through a chiller/condenser system which cools the
CO2 below saturation temperature
Figure 2 Process diagram of the
causing a phase change, 3) is sent
Dewar
chosen concept, identifying changes
Chiller/
through a pump which brings the
of state.
T k
Condenser
liquid to critical pressure, 4)
Liquid CO to SCF
machinery at: 10-22C, 80
passes through a pulse dampener
bar (critical pressure)
to smooth flow and finally 5)
Pulse Damper
warmed up to desired output
Pump
temperature.
Vapor CO2
17 bar, -20C

Liquid CO2
17 bar, -30C

Liquid CO2
80 bar, -30C

Team Supercritical Fluids


MEEG 401
Subsystem Engineering
Chiller/Condenser
The purpose of the chiller and condenser system is to cool the vapor CO2 to below saturation
temperature (-25C at pressure of 250 psi as supplied by the Dewar tank) and ultimately condense it into
liquid form. This operation is completed by the
chiller, which runs an internal refrigeration cycle to
cool an intermediary fluid. This fluid is output from
the chiller and circulated through the condenser.

Figure 3 Flow rate possible for a given


cooling power, valid for CO2 at -30C.

The chiller must provide 1.4 kW of cooling power at


-30C to fully condense CO2 at 250 mL/min, which is
the potential maximum flow rate of this application.
An appropriately sized chiller may be selected for
future applications by use of Figure 3. A lower flow
rate was deemed acceptable in exchange for a lower
chiller cost in the interest of this project. The FTS
RC210 was specified as the chiller for this
application, allowing for a liquid CO2 flow rate of 210
mL/min.

The intermediary fluid to be used between the chiller and condenser is a 75Wt.% Ethylene Glycol/
25Wt.% Water mixture. With a freezing point of -50C, this fluid will remain a liquid at the low
temperatures being reached by the chiller. The flow rate of this fluid is 6 gallons per minute, as dictated
by the recirculation of the chiller.
The condenser to be used should be a heat exchanger with a transfer area of at least 0.34 m2 (3.7 ft2).
The CO2 will run through the inner side, and the chilled intermediary fluid through the outer side. This
transfer area was calculated for a heat transfer of 1.4 kW between the two fluids, assuming the CO2 is
running at 250 mL/min for maximum demand. A conservative estimate of 230 was used for the Heat
Transfer value (U). A sample cooler from Madden has been specified as the condenser with a transfer
area of 0.35m2 (3.8 ft2).
Pump
The pump to be used should increase pressure from 250 psi to 1160 psi, and deliver at variable flow
rates up to 250 mL/min. It is necessary to reach the critical pressure of CO2 (1160 psi), so that
vaporization will not occur in the downstream heater. The SSI Prep250 VFR Diaphragm pump meets
these needs and is specified for this application.
Pulse Dampener
Immediately following the pump, a pulse dampener will serve to smooth out the fluid delivery and
reduce the fluid pulse caused by the pump. This dampener will be made by using an oversized section
of tubing. Given a stroke volume of 0.4525 mL (from pump specifications) and a recommended
dampener volume to stroke factor of 350, a stainless steel, 1 diameter, 1 ft, schedule 10 was specified.
Heater
Final output of the delivery system must be at a temperature in the range of C
10to 22C (room
temperature) to be accepted by the downstream SFT machinery. 500 W of power is required to heat the
5

Team Supercritical Fluids


MEEG 401
-30C CO2 to acceptable output temperature. Self regulating heat tape provides protection against
overheating and adjustable process output temperature. A helical coil of tubing provides increased
efficiency through a secondary fluid flow. 20W/ft self-regulating heat tape will be wrapped over a coil of
copper alloy tubing and insulated with a vapor sealed fiberglass wrap to ensure that the CO2 receives all
of the heat from the heat tape and prevent corrosion of the tubing.
Tubing
All subsystems will be connected via 1/8 stainless steel tubing. Friction losses and pressure drops will
not significantly affect the system for CO2 flow rates up to 250 ml/min. Stainless steel was chosen for its
corrosion resistance as the sub-freezing CO2 will create condensation on the outside of the tubing.
Gauges/Valves
Gauges placed throughout the system will ensure that the temperature and pressure of fluid is
compatible with the processing capabilities of each subsequent component. Pressure relief, throttling,
and purge valves were selected to keep system pressure well within the pressure rating of each
component. The most important locations for these relief valves are immediately downstream of the
pump, where the system pressure will be highest, and immediately before the system feeds to SFT
equipment, where unacceptably high pressure could cause damage to instruments. Figure 3 below
shows the system in terms process and instrumentation.

Figure 4 Process and Instrumentation diagram of the design concept. This drawing represents a critical
piece of the drawing package and is a key deliverable. The P&I diagram specifies technical aspects of the
design and provides a basis for design replication.

Team Supercritical Fluids


MEEG 401
Design Specifications: Table 2 below outlines the specified components and costs of the selected CO2
condenser concept. These costs reflect the prototype build. These specifications will reflect the
commercial unit as well, pending prototype testing. Additionally, it is important to consider the cost of
time that the team has put into the project. For instance, assuming a cost of 50 dollars per hour per
person, where every team member works 20 hours a week, an extra $75,000 in cost can be included for
the prototype(not seen it table).
Component

Quantity

Manufacturer/Description

Model Number

Cost

Chiller

FTS Systems - ULT Series RC210

RC210C0

$14,575.00

Condenser

Madden Manufacturing - Sample Cooler

SC106

$835.00

Pump

SSI - Prep 250 Diaphragm Pump

Prep-250

$4,100.00

Chiller Tubing

15 ft

McMaster Carr - Poly Tubing

5545K14

$12.15

Ethelyne Glycol Coolant

McMaster Carr - 5 Gallons

8673T22

$127.33

Pressure Gauge

WIKA Series 213.53-Liquid Filled

Stock # 36287

$94.82

Temperature Gauge

Omega - RTD Pipe Plug

RTD-NPT-72-E-DUAL-1/4-MTP

$230.00

Alarm

Omega - 1/16 DIN Temperature Controller

CN1A-RTD-230VAC

$168.00

SS 1/4 in Pipe

20 ft

Swagelok

SS-T4-S-04-20, 5.69/ft +2CutChge

$123.80

SS 1 in Pipe

1 ft

Swagelok

SS-T16-S-083-20, 26.37/ft+2CutChge

$273.70

Dewar Fitting

Cramer Decker - CGA320 x .25 NPT female

N832A

$17.80

Dewar & SC Fitting

Swagelok

SS-400-1-4

$20.70

Chiller Fitting

Swagelok

SS-600-1-4

$19.00

SC Fitting

Swagelok

SS-600-1-6

$22.00

Gauge Attachments

Swagelok

SS-400-3-4TTF

$94.20

Pump Fitting

Swagelok

SS-400-1-2

$6.60

Pulse Dampener Fitting

Swagelok

SS-1610-6-4

$167.40

SFT Machinery Fitting

Swagelok

SS-400-6-2

$11.00

Relief Valve

McMaster Carr - 900-2000psi Relief Valve

5026K51

$61.85

T-Fitting

Swagelok

SS-400-3-4TTF

$31.40

20W/ft Heat Tape w/ Jacket

25ft

Chromalox

SRM/E 20-1CT

$230.00

Power Connection

Chromalox

RTPC

$56.10

Line Sensing Thermostat

Chromalox

RTBC

$194.70

End Seal

Chromalox

RTES

$6.05

Copper Tubing

50ft Coil

McMaster Carr - Copper Tubing

8955K26

$156.38

Heater Fittings

Swagelok

S-600-6-4

$9.50

Fiberglass Wrap

McMaster Carr - Insulation

4478K1

$16.59

PolyU. Insulation

McMaster Carr - Insulation

5431K15

$8.93

Alarm

Omega - 1/16 DIN Temperature Controller

CN1A-RTD-230VAC

$168.00
Total:

$21,838.00

Table 2 Bill of Materials indicating the total design cost as well as individual component
specifications and purchasing information.

Team Supercritical Fluids


MEEG 401
Design Layout:
A schematic of how the major subsystems will be put together can be seen below (Figure 3). The scale is
relative, where each component is drawn to the appropriate size based on the others.

Figure 5 Preliminary design layouts, showing spatial relations and basis for future
commercialization of housing design.

Proof of Concept Test:


Though the system is designed to condense and pressurize carbon dioxide to a specified output
condition, the concept must be proved using a different substance. The specified chiller was unavailable
for the scope of this project due to a 10 week lead time. The FTS RC210 has the ultra-low temperature
capability needed to condense CO2 at a flow rate of 210 mL/min. It reaches -35C, the temperature
needed to condense CO2, and also provides 1 kW of cooling power at this temperature, which permits
the flow rate of 210 mL/min.
A proof of concept prototype will be tested as a
contingency for not having the specified chiller
available for the scope of this project. A Polyscience Series
6706, which has a 500 W capacity at -10C was made
available for testing purposes. Since this temperature is
not suitable for condensing CO2, a different substance was
selected for the proof of concept. The chiller and test
bench setup used is pictured in Figure 6 at right.

Figure 6 Lab bench setup for testing


purposes. The condenser is the large upright
cylinder. The chiller used is under the bench.

Vapor butane, a common supercritical extraction medium,


will be tested in the system in place of CO2. Butane has a
higher saturation temperature than CO2 of 7C at the
Butane tank pressure of 19.5 psi. By running butane, the
concept can be verified without the use of a low
temperature chiller. The tests will prove the various
functions of the design including condensing, pressurizing,
damping, and heat conditioning to the appropriate
delivery temperate. Because each of the functions can be
tested with the butane system, results can be obtained for
the metrics of the project.
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Team Supercritical Fluids


MEEG 401
Test Procedure:
Each test should be performed in a fume hood when indoors. Connect all system components except
gas feed, then start the chiller. When chiller reaches temperature, connect the gas feed. Connect system
in accordance with assembly procedure for each test. The following tests will first be performed using
butane gas in order to prove the concept. The tests may be repeated using carbon dioxide gas.
Condensing Test
1. Connect chiller to in/out feeds of the condenser and set
to -5C. Allow to drop to temperature. This is among the
lowest temperatures reached by conventional chiller
units.
2. At the outlet of the condenser, connect temperature and
pressure gauges, followed by a viewing glass, then a
throttling valve. See Figure 7 at right.
3. Ensure digital temperature gauge is working correctly and
throttling valve is cracked open. Use compressed air to
pressurize the system, ensuring it is free of leaks.
4. When chiller reaches temperature, open the butane
flow to the inlet of the condenser.
5. Monitor the pressure gauge to ensure that pressure does
not exceed 50 psi. Adjust the throttling valve accordingly.
6. Watch the viewing glass for traces of liquid butane,
indicating that it is successfully condensing. See Figure 8
at right.
7. If the butane appears to be flashing as it enters the
viewing glass, adjust the throttling valve towards the
closed position.
8. To perform a mass flow calculation, place the butane
tank on a scale and measure the time for the mass to
drop by 0.05 kg; this should occur in about 1 minute.

Figure 7 Close up of the condenser


test setup.

Figure 8 Typical sight glass used for


visual verification of condensate.

Pressure Test
1. This test must be performed using CO2 because the tank pressure of butane is not great enough
to open the check valves on the pump. Connect chiller to in/out feeds of the condenser and set
to -35C. Allow to drop to temperature.
2. At the outlet of the condenser, connect temperature and pressure gauges, followed the pump.
After the pump, the second pressure gauge and a temperature sensor should be in place.
3. Ensure digital temperature gauge is working correctly. Use compressed air to pressurize the
system, ensuring it is free of leaks.
4. When chiller reaches temperature, open the CO2 flow to the inlet of the condenser.
5. Monitor the temperature gauge following the condenser. When temperature and pressure
indicate saturation, turn on the pump.
6. Monitor the downstream pressure gauge to ensure that the pump is reaching the specified
pressure. Also monitor the downstream temperature gauge to determine if there is a significant
temperature change across the pump.

Team Supercritical Fluids


MEEG 401
Heater Test
1. Connect chiller to in/out feeds of the condenser and set to -5C. Allow to drop to temperature.
This is most likely the lowest temperature reached by conventional chiller units. Plug in the selfregulating heat tape to power the heater. Allow heater to rise to temperature.
2. At the outlet of the condenser, connect temperature and pressure gauges, followed the pump.
After the pump, the second pressure gauge and a temperature sensor should be in place. Install
the post heater assembly. A final temperature sensor should be in place after the heater.
3. Ensure digital temperature gauge is working correctly. Use compressed air to pressurize the
system, ensuring it is free of leaks.
4. When chiller reaches temperature, open the butane flow to the inlet of the condenser.
5. Monitor the temperature gauge following the condenser. When temperature and pressure
indicate saturation, turn on the pump.
6. Monitor the temperature gauge downstream of the heater to ensure that the proper
temperature is being reached.
Assembly Guidelines:
1. The condenser should be mounted so that it is inverted, allowing the condensed liquid product
to easily drain. The condenser must be securely fastened to its mounting point so that its weight
is sufficiently supported.
2. Outlet of the condenser should be connected to downstream instrumentation. See P&I diagram
for process order.
3. The pump should be mounted or placed on a flat surface, at least 3 feet off the ground to allow
for ease of use.
4. The pulse damper should be mounted vertically, with the inlet at the bottom.
5. All heater components should be assembled in accordance with the final prototype design
supplied.
Proof of Concept Test Results:
The system was successfully able to condense butane gas to a liquid. As stated above, condensing of
butane proves that the system is also capable of condensing CO2. Results of the condensation test can
be seen in Figure 9 below; the sight glass is filled with condensate. Temperature data and pressure data
collected during the condensation experiment also indicated conditions for condensing butane. A mass
flow experiment was also performed by measuring
the elapsed time for a mass loss of 0.05 kg by the
butane tank. The elapsed time was approximately
1 minute, giving a flow rate of about 80 mL/min of
butane. Using the temperature, pressure, and
state observations collected during the
experiment, the required cooling power of the
chiller at 22F (-5C) was back-calculated to be 340
Watts This value is in agreement with the available
cooling capacity offered by the Polyscience 6706
Series chiller. Therefore, this test proves the
experimental calculations were correct to a close
approximation.
Figure 9 Close up of the sight glass showing
condensate inside.

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Team Supercritical Fluids


MEEG 401
The other goals of the system are to pressurize the CO2 condensate to 1160 psi, then heat the
condensate to room temperature. The function of the pump and heater components can be verified
using the test procedures listed above; however their performance is much more guaranteed than that
of the condenser. So, testing of these components is not required to prove the concept. Additionally,
the pump performance was tested by manufacturer, SSI. Positive results from this test were sufficient to
prove the performance of the pump for use in the design. The heater uses self-regulating heat wire, and
has been designed with a safety margin to allow for a flow rate of 300 mL/min, almost double the flow
required by SFT extraction experiments, making testing unnecessary.
Conclusions:
In conclusion, it has been shown that the chosen concept is a valid solution for the CO2 bulk delivery
system. With the results of the experiment, Supercritical Fluid Technologies will be able to begin using
high-volume, vapor draw Dewar tanks for their CO2 supply. The use of vapor draw Dewar tanks will
replace expensive, low-quantity, liquid drawn CO2 tanks. The benefit to the sponsor is a cost savings, a
conservation of space, and increased convenience. The cost benefit of a Dewar tank as the CO2 source
comes from the Dewar costing 3 times more than the liquid tank, $150 compared to $50, but containing
300 L of useable CO2 versus 40 L with the liquid tank. That is 7.5 times more CO2 for only 3 times the
price. Space will be conserved since CO2 gas consumes less volume than CO2 in a liquid state. This is
beneficial in smaller scale facilities, like SFTs laboratory. Convenience is difficult to quantify. Speaking in
terms of number of tanks, it can be measured. Companies that run large capacity supercritical fluid
extraction experiments, such as Accudyne, could use up to fifty 40 L liquid draw CO2 containers to fill
one of their extraction machines. These medium to large sized companies would see benefit by
requiring only 7 Dewar tanks of CO2 to complete their experiments versus 50 liquid tanks. By nature,
Dewar tanks are wheel-mounted, making them more mobile than a heavy liquid tank without wheels,
adding to the convenience benefit.
In agreement with the sponsor, the key metrics were sufficiently met by the design. While the ability to
condense is the primary goal of this effort, the desired delivery conditions in terms of temperature and
pressure are the metrics of highest importance. These metrics were met by the design. Cost falls within
the anticipated bounds. Flow rate suffered a noticeable departure from the initial goal of 250 mL/min,
however the tradeoff was understood by the sponsor and 210 mL/min became an agreeable solution.
The concept has been proven successful in terms of the metrics.
Delivery Temperature
Delivery Pressure
Cost of System
Delivery Time
Flow Rate
Size of System (Volume)
Weight of System

10C - 22C
>80 bar
$20,000.00 $5,000.00
<30 min
Variable up to 250 ml/min
< 3ft x 3ft x 6ft
Can move on wheels

22C
80 bar
$21,838
1 min
210 ml/min
3 x 4 x 5 ft
Yes

Table 3 Refined design metrics, ranked in order of importance, with measured results at right.

The final deliverables of the project were sufficiently completed in accordance with SFT. The primary
function of the system, the condenser capability, has been validated using proof of concept tests. The
other deliverable expected as a result of this project is a functional prototype that SFT will be able to use
in their lab for supercritical extractions. Accommodations for complete system assembly will be made so
that this deliverable will be completed in the scope of this project. The pump, framing, and remaining
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Team Supercritical Fluids


MEEG 401
heater components will most likely arrive within the week following submission of this report. At that
time, the prototype will be fully completed and delivered to SFT. Once the specified chiller is made
available, it can easily be integrated, enabling the system to perform at its full design capacity. The final
benefits to the sponsor, Supercritical Fluid Technologies, will be the use of the CO2 bulk delivery system
in their laboratory over a timeframe of about a year and the opportunity to replicate the concept for
commercialization.
Path Forward: The future of the CO2 bulk delivery concept will begin with rigorous use of the prototype
in Supercritical Fluid Technologies laboratory. The specified chiller should be available in January 2009,
permitting regular use of the system to begin. As the CO2 bulk delivery system prototype is used over
the next year to two years, any pitfalls will be discovered. Most attention will be paid to fine-tuning the
heater load, accounting for the heat of compression and piping friction losses. After full capacity testing
by SFT, the system will be ready for commercialization. A new, more compact enclosure will be
produced to match the SFT product line and the unit may be made commercially available.
Prototype vs. Commercial Product: It is important to distinguish between the prototype (scope of this
project) and future commercial system. Main differences will occur in the realm of functions and cost
between the two systems. A comparison of this can be seen in Table 4, below. The prototype served to
validate the theory and prove the core concept. The prototype enables SFT to move from liquid tanks to
Dewar tanks, meeting their business goal of cost savings. Additionally, the prototype provides a
functional basis for the sponsor to create a professional grade product which can be added to his
current product line.

Prototype

Commercial Product

Function
Detail thermodynamics of process and determine
Optimized process parameters after seeing
cost of system
performance
Define most inefficient aspects of process
Minimize excess at each instrument
Reduce sponsors costs in liquid CO2 tanks
Eliminate sponsors need to buy purified CO2 and
sell to others
Cost
Buying all instruments at single item list price
Negotiation of bulk or repeat discount possible
Each process not necessarily optimized

Trim down unused performance of parts

Can only buy what is available today

More appropriate instruments to be released in


future

Table 4 Differences between the prototype and the future commercial product,
outlined in terms of function and cost.

12

Appendix A: Concept Generation


Concept 1
Concept 2
Concept 3
Concept 4

13

14

15

Appendix B: Concept Selection


Compressor vs. Pump
Relative Ranking

16

Compressor vs. Pump

17

18

19

Appendix C: Initial Calculations


Cooling capacity
Process Time

20

21

22

Appendix D: Chiller Selection


Chiller Vendors
Flow Rate Possible for Given Chiller
Cost
FTS Chiller Information

23

Final Chiller Selection Flow Rate vs. Cost Trade-off


The premier manufacturers in the chiller field were contacted for price quotes on a chiller to meet our needs. The
chiller selection is limited by cost, temperature and power. We require a temperature of -35C, which was
confirmed to be uncommon in the chiller industry, falling into a grey area between conventional machines and
cryogenic machines. To run at the desired flow rate of 250 mL/min, 1.4 kW of power is required at -35C. It seems
that the only chillers capable of this are more expensive than we would like. A trade-off between flow rate and
cost must be made.
Cooling
Temperature
(Celsius)
-40
-30
-35
-35
-40
-40
-40
Approx. -90

Power (W) at
Cooling Temp.
60
400
1200
2000
600
2700
1000
3000

Approx. Flow
Rate Possible
(mL/min)
20
40
210
250
150
350
250
650

Manufacturer
Model
FTS Systems
RS33LT
FTS Systems
MC100LT
FTS Systems
RC210
FTS Systems
UC500LT1
Julabo
FP52-SL
FTS Systems
RC311
Julabo
FPW55-SL
Brooks/Polycold
n/a
Notes:
1. Costs may be approximate.
2. Cooling Temperature is given because cooling power may not be available for 35C exactly.
3. For flow rate greater than 100mL/min, an additional $700 is added to the Total
System
Cost to accommodate an electrical post-heater.

Chiller
Cost ($)
$4,700
$9,500
$15,000
$20,000
$23,600
$25,000
$25,600
$35,000

Approx. Total
System Cost ($)
$11,500
$16,300
$22,500
$27,500
$31,100
$32,500
$33,100
$42,800

Flow Rate Possible for Given Chiller Cost


700

Flow Rate (mL/min)

600
500
400
300
200
Largest Jump
in
Performance

100
0
$0

$5,000 $10,000$15,000$20,000$25,000$30,000$35,000$40,000
Chiller Cost ($)

24

This page includes an expanded summary of all findings on chiller vendors, pricing, and
performance. Links to the respective websites and contact information are also included.
FTS Systems 845.687.5359 Terry
o RS - http://www.ftssystems.com/rschillerback.htm
RS33LT does 195W at -30C, 60W at -40C. $4700
o Maxi-cool Series - http://www.ftssystems.com/maxicool.htm
100LT does 400W at -30C. $9500
o Ultra-cool - http://www.ftssystems.com/ultracool.htm
UC500LT1 does 3600W at -30C, 2000W at -35C, 1100W at -40C. $19,500
o ULT - http://www.ftssystems.com/ultseries.htm
RC311 does 2700W at -40C. $22k-25k
RC210 does 1200W at -35C. $15000
o Note: LT model numbers indicate Low-Temp
o Terry confirmed that chillers in the range we are looking for are uncommon, but that is
really FTS niche.

Polyscience 215.541.1181 (home business line) Mike Gallagher


o May have a chiller than can do 150W at -35C. This low temp not shown on website.
o http://www.polyscience.com/lab/chill.html
o Estimated that 1.35kW at -40C would cost above $30k and use cascade cooling.
o Recommended Julabo FP90-SL.

Julabo 845.612.5772 Terry Mclaughlin (terrym@julabo.com)


o Cooling calculation and cost request sent. Quote received for two appropriate models.
o

FPW55-SL does 1kW at -40C. $25,600

http://www.julabo.com/us/p_datasheet.asp?Produkt=FPW55-SL
o

FP52-SL does 600W at -$40C. $23,600

http://www.julabo.com/us/p_datasheet.asp?Produkt=FP52-SL

Brooks Automation: Polycold Chillers 707.769.7050 Kim Lorence, Chris Beckey


o

http://www.brooks.com/pages/2149_polycold%C2%AE_systems_cryogenic_refrigeration.cfm

For our application (chiller cooling a heat exchanger/condenser), the appropriate Polycold
chiller is in the $35k range.
Polycold is in the cryogenics business. Their recirculating chillers have temperature ranges of
-30 or -40 to -150, and can produce around 3 kW at these low temps.
Chris Beckey confirmed that there is a gap between the common chiller industry (temps of 10C) and the cryogenics industry (typically -100C). Estimated that a chiller didnt exist that
would provide 1.4 kW at -35C without being a cryogenic chiller, however, said he has limited
knowledge of the non-cryogenic chiller field.

o
o

25

26

Appendix E: Condenser
Condenser calculations and selection

27

28

Appendix F: Pump Selection


Pump Vendors

29

30

Appendix G: Pulse Dampener Selection


Pulse Dampener Calculations

31

32

Appendix H: Heater Selection


Heater Calculations

33

34

Appendix I: Electrical
Electrical Diagram

35

36

Appendix J: Piping
Friction Loss Calculations

37

38

Appendix K: Testing Contingency Plan


CO2 vs. Butane system layout by
processes

39

40

Appendix L: Path Forward


Gantt Chart

41

42

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