co2 bulk delivery system

8/13/2019 CO2 Bulk Delivery System

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Sponsor: Ken JamesAdvisor: 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 CO 2 drawn from cylinders that contain 40 L of useable CO 2 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 CO 2, which contains

300 L of CO2 mixture, at a fraction the cost of liquid tanks. In order to use the Dewar tank, CO 2

will be drawn into a distillation system that will precede the SFT machinery. The primary

function of this design is to condense the CO 2 to a liquid of high purity. Considerations forsafety 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.


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Team Supercritical FluidsMEEG 401

2

Table of Contents

Executive Summary

Table of Contents

1

Introduction/Background2

Project Scope

3

Refined Metrics

3

Concept Generation & Selection

3

Concept Overview

4

Methods

4

Subsystem Engineering

5

Design Specifications

5

Design Layout

7

Proof of Concept Test

8

Test Procedure

8

Results

9

Butane Condensation Test Results

10

Butane Condensation with Pumping Test Results

10

Post Heater Test Results

10

Conclusions

11

Path Forward

11

Future Testing

12

Prototype vs. Commercial Product

12

Appendices

12

13


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Introduction:

SFT currently pulls pure liquid CO 2 via a dip tube from 20 liter tanks (750 psi, 22 C) and delivers directlyto their machinery. The liquid tanks must be of high purity, making them expensive. Large extractionexperiments may require up to 50 of the 20 L liquid CO 2 tanks to fill the extraction machine.Additionally, the 20 L capacity per tank means that they must be renewed often, creating a pile-up ofempty tanks in the lab.

Supercritical Fluid Technologies, Inc. (SFT) specializes in developing innovative solutions forsupercritical fluid extraction and reaction processes. A supercritical fluid exists when a substance ispressurized 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 exhibitingthe 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 CO 2 is the extraction media used by Supercritical Fluid Technologies. Thisteam has been assigned to develop a CO 2 delivery system that will provide CO 2 from a bulk storage tankto downstream SFT machinery at specified conditions.

SFT would like to use CO 2 from a Dewar tank (250 psi, -20 C) that contains 300 L of CO 2 mixture. SFTextraction machines require a 99.99% CO 2 purity level, meaning that the CO 2 cannot be directly fed intoSFT machinery. By drawing vapor CO 2 from the Dewar tank, pure liquid can be produced via a distillationprocess. The CO 2 gas will be converted to pure liquid at a temperature and pressure of 10-22 C and 1160psi, respectively, to be accepted by and fed to SFT machinery. A working prototype will be designed andimplemented to carry out the aforementioned condensing and pressurizing process for the CO 2 bulkdelivery system.

Project Scope: To design system that will condense and pressurize CO 2 vapor output from a Dewar tankand deliver it to downstream SFT machinery, eliminating the need for expensive and cumbersome liquidtanks. 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 Metric Target Value1 Delivery Temperature 10 C - 22 C2 Delivery Pressure >80 bar3 Cost of System $20,000.00 $5,000.004 CO2 Delivery Time


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Figure 1 P-h diagram depicting the two process

options of the design: use of a pump versus

compressor.

Figure 2 Process diagram of the

chosen concept, identifying changesof state.

Concept Generation & Selection

The CO2 gas can be pressurized and then condensed or vice versa. By first using a condenser, the CO 2 will maintain near constant pressure of 250 psi while being cooled to the saturation temperature of-25 C. As soon as the saturation temperature iscrossed, the CO 2 will be in liquid phase and can bepumped up to the desired pressure of 1160 psi.During the pumping stage, isentropic paths arefollowed which run nearly parallel to isothermallines, allowing for a very efficient process (Figure

1). The alternative to the pumping system is acompressor. If a compressor is first used toincrease pressure, isentropic lines run almostperpendicular to the lines of constanttemperature and the path of the compressormust be longer to ensure exit from the saturationphase. Once the compression process iscompleted, a condenser must be used to drop the temperature, but this line of enthalpy will be largerthan 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. Overnightstorage 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. Tocombat this, an intricate control system would have to be used. Running a process time calculation, itwas determined that an intermediate holding tank would not be necessary to deliver at 250mL/minsince the process could be completed in under 30 seconds (see Appendix).

: The goal of this project is to enable Supercritical Fluid Technologies touse a larger, less expensive Dewar tank instead of a liquid tank to feed the extraction machinery. Themain functions involved in the purification process are condensing and pressurizing. Design conceptswere generated to meet the following specifications: 10-22 C, 1160 psi and flow rate up to 250mL/min.Two significant differences arose between the various concepts. The first involved raising the pressureby the use of a pump or a compressor. The second involved the use of an intermediate holding tank.

Concept Overview: The selected concept is shown as a schematic in Figure 2 below. For this concept,vapor CO 2 is 1) output from the Dewar tank, 2) goes through a chiller/condenser system which cools the

CO2 below saturation temperaturecausing a phase change, 3) is sentthrough a pump which brings theliquid to critical pressure, 4)passes through a pulse dampenerto smooth flow and finally 5)warmed up to desired outputtemperature.

Pump

Dewar Chiller/

Condenser

Pulse Damper

Vapor CO217 bar, -20 C

Liquid CO217 bar, -30 C

Liquid CO280 bar, -30 C

Liquid CO 2 to SCFmachinery at: 10-22C, 80bar (critical pressure)


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Figure 3 Flow rate possible for a given

cooling power, valid for CO 2 at -30C.

The purpose of the chiller and condenser system is to cool the vapor CO 2 to below saturationtemperature (-25 C at pre ssure of 250 psi as supplied by the Dewar tank) and ultimately condense it into

liquid form. This operation is completed by thechiller, which runs an internal refrigeration cycle tocool an intermediary fluid. This fluid is output fromthe chiller and circulated through the condenser.

Subsystem Engineering

Chiller/Condenser

The chiller must provide 1.4 kW of cooling power at-30C to fully condense CO 2 at 250 mL/min, which isthe potential maximum flow rate of this application.An appropriately sized chiller may be selected forfuture applications by use of Figure 3. A lower flowrate was deemed acceptable in exchange for a lowerchiller cost in the interest of this project. The FTS

RC210 was specified as the chiller for thisapplication, allowing for a liquid CO 2 flow rate of 210mL/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 -50 C, this fluid will remain a liquid at the lowtemperatures being reached by the chiller. The flow rate of this fluid is 6 gallons per minute, as dictatedby the recirculation of the chiller.

The condenser to be used should be a heat exchanger with a transfer area of at least 0.34 m 2 (3.7 ft 2).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 CO 2 isrunning at 250 mL/min for maximum demand. A conservative estimate of 230 was used for the HeatTransfer value (U). A sample cooler from Madden has been specified as the condenser with a transferarea of 0.35m 2 (3.8 ft 2).

PumpThe pump to be used should increase pressure from 250 psi to 1160 psi, and deliver at variable flowrates up to 250 mL/min. It is necessary to reach the critical pressure of CO 2 (1160 psi), so thatvaporization will not occur in the downstream heater. The SSI Prep250 VFR Diaphragm pump meetsthese needs and is specified for this application.

Pulse DampenerImmediately following the pump, a pulse dampener will serve to smooth out the fluid delivery andreduce the fluid pulse caused by the pump. This dampener will be made by using an oversized sectionof tubing. Given a stroke volume of 0.4525 mL (from pump specifications) and a recommendeddampener volume to stroke factor of 350, a stainless steel, 1 diameter, 1 ft, schedule 10 was specified.

HeaterFinal output of the delivery system must be at a temperature in the range of 10 C to 22C (roomtemperature) to be accepted by the downstream SFT machinery. 500 W of power is required to heat the


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-30C CO2 to acceptable output temperature. Self regulating heat tape provides protection againstoverheating and adjustable process output temperature. A helical coil of tubing provides increasedefficiency through a secondary fluid flow. 20W/ft self-regulating heat tape will be wrapped over a coil ofcopper alloy tubing and insulated with a vapor sealed fiberglass wrap to ensure that the CO 2 receives allof the heat from the heat tape and prevent corrosion of the tubing.

TubingAll subsystems will be connected via 1/8 stainless steel tubing. Friction losses and pressure drops willnot significantly affect the system for CO 2 flow rates up to 250 ml/min. Stainless steel was chosen for itscorrosion resistance as the sub-freezing CO 2 will create condensation on the outside of the tubing.

Gauges/ValvesGauges placed throughout the system will ensure that the temperature and pressure of fluid iscompatible 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 eachcomponent. The most important locations for these relief valves are immediately downstream of thepump, 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 belowshows 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.


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Design Specifications:

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

Component Quantity Manufacturer/Description Model Number Cost

Chiller 1 FTS Systems - ULT Series RC210 RC210C0 $14,575.00

Condenser 1 Madden Manufacturing - Sample Cooler SC106 $835.00

Pump 1 SSI - Prep 250 Diaphragm Pump Prep-250 $4,100.00

Chiller Tubing 15 ft McMaster Carr - Poly Tubing 5545K14 $12.15

Ethelyne Glycol Coolant 1 McMaster Carr - 5 Gallons 8673T22 $127.33

Pressure Gauge 2 WIKA Series 213.53-Liquid Filled Stock # 36287 $94.82

Temperature Gauge 2 Omega - RTD Pipe Plug RTD-NPT-72-E-DUAL-1/4-MTP $230.00

Alarm 1 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 1 Cramer Decker - CGA320 x .25 NPT female N832A $17.80

Dewar & SC Fitting 3 Swagelok SS-400-1-4 $20.70

Chiller Fitting 2 Swagelok SS-600-1-4 $19.00

SC Fitting 2 Swagelok SS-600-1-6 $22.00

Gauge Attachments 3 Swagelok SS-400-3-4TTF $94.20

Pump Fitting 2 Swagelok SS-400-1-2 $6.60

Pulse Dampener Fitting 2 Swagelok SS-1610-6-4 $167.40

SFT Machinery Fitting 1 Swagelok SS-400-6-2 $11.00

Relief Valve 1 McMaster Carr - 900-2000psi Relief Valve 5026K51 $61.85

T-Fitting 2 Swagelok SS-400-3-4TTF $31.40

20W/ft Heat Tape w/ Jacket 25ft Chromalox SRM/E 20-1CT $230.00

Power Connection 1 Chromalox RTPC $56.10

Line Sensing Thermostat 1 Chromalox RTBC $194.70

End Seal 1 Chromalox RTES $6.05

Copper Tubing 50ft Coil McMaster Carr - Copper Tubing 8955K26 $156.38

Heater Fittings 2 Swagelok S-600-6-4 $9.50

Fiberglass Wrap 3 McMaster Carr - Insulation 4478K1 $16.59

PolyU. Insulation 1 McMaster Carr - Insulation 5431K15 $8.93

Alarm 2 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 componentspecifications and purchasing information.
http://www.mcmaster.com/param/asp/psearch.asp?FAM=tubing&FT_138=154264&FT_3501=157161&FT_813=31329&FT_3877=173673&FT_663=176969&FT_3513=228982&FT_167=154272&FT_505=130193&FT_2967=158149&FT_136=1009&ppe=4&session=tubing;3501=157161;138=154264;813=31329;3877=173673;M;Ihttp://www.mcmaster.com/param/asp/psearch.asp?FAM=tubing&FT_138=154264&FT_3501=157161&FT_813=31329&FT_3877=173673&FT_663=176969&FT_3513=228982&FT_167=154272&FT_505=130193&FT_2967=158149&FT_136=1009&ppe=4&session=tubing;3501=157161;138=154264;813=31329;3877=173673;M;I


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

Though the system is designed to condense and pressurize carbon dioxide to a specified outputcondition, the concept must be proved using a different substance. The specified chiller was unavailablefor the scope of this project due to a 10 week lead time. The FTS RC210 has the ultra-low temperaturecapability needed to condense CO 2 at a flow rate of 210 mL/min. It reaches -35 C, the temperatureneeded to condense CO 2, and also provides 1 kW of cooling power at this temperature, which permitsthe flow rate of 210 mL/min.

Proof of Concept Test:

A proof of concept prototype will be tested as acontingency for not having the specified chilleravailable for the scope of this project. A Polyscience Series6706, which has a 500 W capacity at -10 C was madeavailable for testing purposes. Since this temperature isnot suitable for condensing CO 2, a different substance wasselected for the proof of concept. The chiller and testbench setup used is pictured in Figure 6 at right.

Vapor butane, a common supercritical extraction medium,will be tested in the system in place of CO 2. Butane has ahigher saturation temperature than CO 2 of 7 C at the

Butane tank pressure of 19.5 psi. By running butane, theconcept can be verified without the use of a lowtemperature chiller. The tests will prove the variousfunctions of the design including condensing, pressurizing,damping, and heat conditioning to the appropriatedelivery temperate. Because each of the functions can betested with the butane system, results can be obtained forthe metrics of the project.

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

Figure 6 Lab bench setup for testing

purposes. The condenser is the large upright

c linder. The chiller used is under the bench.


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1. Connect chiller to in/out feeds of the condenser and setto -5 C. Allow to drop to temperature. This is among thelowest temperatures reached by conventional chillerunits.

Test Procedure:Each test should be performed in a fume hood when indoors. Connect all system components exceptgas feed, then start the chiller. When chiller reaches temperature, connect the gas feed. Connect systemin accordance with assembly procedure for each test. The following tests will first be performed usingbutane gas in order to prove the concept. The tests may be repeated using carbon dioxide gas.

Condensing Test

2. At the outlet of the condenser, connect temperature andpressure gauges, followed by a viewing glass, then athrottling valve. See Figure 7 at right.

3. Ensure digital temperature gauge is working correctly andthrottling valve is cracked open. Use compressed air topressurize the system, ensuring it is free of leaks.

4. When chiller reaches temperature, open the butaneflow to the inlet of the condenser.

5. Monitor the pressure gauge to ensure that pressure doesnot 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 8at right.

7. If the butane appears to be flashing as it enters theviewing glass, adjust the throttling valve towards theclosed position.

8. To perform a mass flow calculation, place the butane

tank on a scale and measure the time for the mass todrop by 0.05 kg; this should occur in about 1 minute.

Pressure Test1. This test must be performed using CO 2 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 setto -35 C. 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 thesystem, ensuring it is free of leaks.

4. When chiller reaches temperature, open the CO 2 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 significanttemperature change across the pump.

Figure 7 Close up of the condenser

test setup.

Figure 8 Typical sight glass used for

visual verification of condensate.


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Heater Test1. Connect chiller to in/out feeds of the condenser and set to -5 C. Allow to drop to temperature.

This is most likely the lowest temperature reached by conventional chiller units. Plug in the self-regulating 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. Installthe 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 thesystem, 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.

1. The condenser should be mounted so that it is inverted, allowing the condensed liquid productto easily drain. The condenser must be securely fastened to its mounting point so that its weightis sufficiently supported.

Assembly Guidelines:

2. Outlet of the condenser should be connected to downstream instrumentation. See P&I diagramfor process order.

3. The pump should be mounted or placed on a flat surface, at least 3 feet off the ground to allowfor 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.

The system was successfully able to condense butane gas to a liquid. As stated above, condensing ofbutane proves that the system is also capable of condensing CO 2. Results of the condensation test canbe seen in Figure 9 below; the sight glass is filled with condensate. Temperature data and pressure datacollected during the condensation experiment also indicated conditions for condensing butane. A mass

flow experiment was also performed by measuringthe elapsed time for a mass loss of 0.05 kg by thebutane tank. The elapsed time was approximately1 minute, giving a flow rate of about 80 mL/min ofbutane. Using the temperature, pressure, andstate observations collected during theexperiment, the required cooling power of thechiller at 22F (-5C) was back-calculated to be 340Watts This value is in agreement with the availablecooling capacity offered by the Polyscience 6706Series chiller. Therefore, this test proves theexperimental calculations were correct to a closeapproximation.

Proof of Concept Test Results:

Figure 9 Close up of the sight glass showing

condensate inside.


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The other goals of the system are to pressurize the CO 2 condensate to 1160 psi, then heat thecondensate to room temperature. The function of the pump and heater components can be verifiedusing the test procedures listed above; however their performance is much more guaranteed than thatof 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 toprove the performance of the pump for use in the design. The heater uses self-regulating heat wire, andhas been designed with a safety margin to allow for a flow rate of 300 mL/min, almost double the flowrequired by SFT extraction experiments, making testing unnecessary.

In conclusion, it has been shown that the chosen concept is a valid solution for the CO 2 bulk deliverysystem. With the results of the experiment, Supercritical Fluid Technologies will be able to begin usinghigh-volume, vapor draw Dewar tanks for their CO 2 supply. The use of vapor draw Dewar tanks willreplace expensive, low-quantity, liquid drawn CO 2 tanks. The benefit to the sponsor is a cost savings, aconservation of space, and increased convenience. The cost benefit of a Dewar tank as the CO 2 sourcecomes from the Dewar costing 3 times more than the liquid tank, $150 compared to $50, but containing300 L of useable CO 2 versus 40 L with the liquid tank. That is 7.5 times more CO 2 for only 3 times the

price. Space will be conserved since CO 2 gas consumes less volume than CO 2 in a liquid state. This isbeneficial in smaller scale facilities, like SFTs laboratory. Convenience is difficult to quantify. Speaking interms of number of tanks, it can be measured. Companies that run large capacity supercritical fluidextraction experiments, such as Accudyne, could use up to fifty 40 L liquid draw CO 2 containers to fillone of their extraction machines. These medium to large sized companies would see benefit byrequiring only 7 Dewar tanks of CO 2 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.

Conclusions:

In agreement with the sponsor, the key metrics were sufficiently met by the design. While the ability tocondense 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 withinthe 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 10 C - 22 C 22 CDelivery Pressure >80 bar 80 barCost of System $20,000.00 $5,000.00 $21,838Delivery Time


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heater components will most likely arrive within the week following submission of this report. At thattime, the prototype will be fully completed and delivered to SFT. Once the specified chiller is madeavailable, it can easily be integrated, enabling the system to perform at its full design capacity. The finalbenefits to the sponsor, Supercritical Fluid Technologies, will be the use of the CO 2 bulk delivery systemin their laboratory over a timeframe of about a year and the opportunity to replicate the concept forcommercialization.

Path Forward:

The future of the CO 2 bulk delivery concept will begin with rigorous use of the prototypein Supercritical Fluid Technologies laboratory. The specified chiller should be available in January 2009,permitting regular use of the system to begin. As the CO 2 bulk delivery system prototype is used overthe next year to two years, any pitfalls will be discovered. Most attention will be paid to fine-tuning theheater load, accounting for the heat of compression and piping friction losses. After full capacity testingby SFT, the system will be ready for commercialization. A new, more compact enclosure will beproduced 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 thisproject) 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 tovalidate the theory and prove the core concept. The prototype enables SFT to move from liquid tanks toDewar tanks, meeting their business goal of cost savings. Additionally, the prototype provides afunctional basis for the sponsor to create a professional grade product which can be added to hiscurrent product line.

Prototype Commercial ProductFunction

Detail thermodynamics of process and determinecost of system

Optimized process parameters after seeingperformance

Define most inefficient aspects of process Minimize excess at each instrument

Reduce sponsors costs in liquid CO 2 tanks Eliminate sponsors need to buy purified CO 2 andsell to others

CostBuying 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 infuture

Table 4 Differences between the prototype and the future commercial product,

outlined in terms of function and cost.


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Concept 1

Appendix A: Concept Generation

Concept 2 Concept 3 Concept 4


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Compressor vs. Pump

Appendix B: Concept Selection

Relative Ranking


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Compressor vs. Pump


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Cooling capacity

Appendix C: Initial Calculations

Process Time


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Chiller Vendors

Appendix D: Chiller Selection

Flow Rate Possible for Given ChillerCost

FTS Chiller Information


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The premier manufacturers in the chiller field were contacted for price quotes on a chiller to meet our needs. Thechiller 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 andcryogenic machines. To run at the desired flow rate of 250 mL/min, 1.4 kW of power is required at -35C. It seemsthat the only chillers capable of this are more expensive than we would like. A trade-off between flow rate and

cost must be made.

Final Chiller Selection Flow Rate vs. Cost Trade-off

Manufacturer Model

CoolingTemperature

(Celsius)Power (W) atCooling Temp.

Approx. FlowRate Possible

(mL/min)Chiller

Cost ($)Approx. Total

System Cost ($)FTS Systems RS33LT -40 60 20 $4,700 $11,500FTS Systems MC100LT -30 400 40 $9,500 $16,300FTS Systems RC210 -35 1200 210 $15,000 $22,500FTS Systems UC500LT1 -35 2000 250 $20,000 $27,500Julabo FP52-SL -40 600 150 $23,600 $31,100

FTS Systems RC311 -40 2700 350 $25,000 $32,500Julabo FPW55-SL -40 1000 250 $25,600 $33,100Brooks/Polycold n/a Approx. -90 3000 650 $35,000 $42,800Notes: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 TotalSystem

Cost to accommodate an electrical post-heater.

0

100

200

300

400

500

600

700

$0 $5,000 $10,000$15,000$20,000$25,000$30,000$35,000$40,000

F l o w R a t e

( m L / m i n

)

Chiller Cost ($)

Flow Rate Possible for Given Chiller Cost

Largest Jumpin

Performance


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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 Terryo RS - http://www.ftssystems.com/rschillerback.htm

RS33LT does 195W at -30C, 60W at -40C. $4700o Maxi-cool Series - http://www.ftssystems.com/maxicool.htm

100LT does 400W at -30C. $9500o Ultra-cool - http://www.ftssystems.com/ultracool.htm

UC500LT1 does 3600W at -30C, 2000W at -35C, 1100W at -40C. $19,500o 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-Tempo 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 Gallaghero 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 ([email protected])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 Beckeyo http://www.brooks.com/pages/2149_polycold%C2%AE_systems_cryogenic_refrigeration.cfm o For our application (chiller cooling a heat exchanger/condenser), the appropriate Polycold

chiller is in the $35k range.o 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.o 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 thatwould provide 1.4 kW at -35C without being a cryogenic chiller, however, said he has limitedknowledge of the non-cryogenic chiller field.
http://www.ftssystems.com/rschillerback.htmhttp://www.ftssystems.com/rschillerback.htmhttp://www.ftssystems.com/rschillerback.htmhttp://www.ftssystems.com/maxicool.htmhttp://www.ftssystems.com/maxicool.htmhttp://www.ftssystems.com/maxicool.htmhttp://www.ftssystems.com/ultracool.htmhttp://www.ftssystems.com/ultracool.htmhttp://www.ftssystems.com/ultracool.htmhttp://www.ftssystems.com/ultseries.htmhttp://www.ftssystems.com/ultseries.htmhttp://www.ftssystems.com/ultseries.htmhttp://www.polyscience.com/lab/chill.htmlhttp://www.polyscience.com/lab/chill.htmlhttps://ms4.nss.udel.edu/wm/mail/fetch.html?urlid=22f396339d5f4f1259a664fdf9ba41cf6&url=http%3A%2F%2Fwww.julabo.com%2Fus%2Fp_datasheet.asp%3FProdukt%3DFPW55-SLhttps://ms4.nss.udel.edu/wm/mail/fetch.html?urlid=22f396339d5f4f1259a664fdf9ba41cf6&url=http%3A%2F%2Fwww.julabo.com%2Fus%2Fp_datasheet.asp%3FProdukt%3DFP52-SLhttps://ms4.nss.udel.edu/wm/mail/fetch.html?urlid=22f396339d5f4f1259a664fdf9ba41cf6&url=http%3A%2F%2Fwww.julabo.com%2Fus%2Fp_datasheet.asp%3FProdukt%3DFP52-SLhttp://www.brooks.com/pages/2149_polycold%C2%AE_systems_cryogenic_refrigeration.cfmhttp://www.brooks.com/pages/2149_polycold%C2%AE_systems_cryogenic_refrigeration.cfmhttp://www.brooks.com/pages/2149_polycold%C2%AE_systems_cryogenic_refrigeration.cfmhttps://ms4.nss.udel.edu/wm/mail/fetch.html?urlid=22f396339d5f4f1259a664fdf9ba41cf6&url=http%3A%2F%2Fwww.julabo.com%2Fus%2Fp_datasheet.asp%3FProdukt%3DFP52-SLhttps://ms4.nss.udel.edu/wm/mail/fetch.html?urlid=22f396339d5f4f1259a664fdf9ba41cf6&url=http%3A%2F%2Fwww.julabo.com%2Fus%2Fp_datasheet.asp%3FProdukt%3DFPW55-SLhttp://www.polyscience.com/lab/chill.htmlhttp://www.ftssystems.com/ultseries.htmhttp://www.ftssystems.com/ultracool.htmhttp://www.ftssystems.com/maxicool.htmhttp://www.ftssystems.com/rschillerback.htm


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Condenser calculations and selection

Appendix E: Condenser


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Pump Vendors

Appendix F: Pump Selection


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Pulse Dampener Calculations

Appendix G: Pulse Dampener Selection


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Heater Calculations

Appendix H: Heater Selection


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Electrical Diagram

Appendix I: Electrical


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Friction Loss Calculations

Appendix J: Piping


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CO2 vs. Butane system layout byprocesses

Appendix K: Testing Contingency Plan


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Gantt Chart

Appendix L: Path Forward


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co2 bulk delivery system

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