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 3 3 4 4

1 2 3

Methods
Subsystem Engineering Design Specifications Design Layout Proof of Concept Test Test Procedure 5 7 8 8 9

Results
Butane Condensation Test Results Butane Condensation with Pumping Test Results Post Heater Test Results 10 10 11

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Conclusions Path Forward

Future Testing Prototype vs. Commercial Product 12 12

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Appendices

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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
2

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. 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.

Figure 3 Flow rate possible for a given cooling power, valid for CO2 at -30C.

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 Chiller Condenser Pump Chiller Tubing Ethelyne Glycol Coolant Pressure Gauge Temperature Gauge Alarm SS 1/4 in Pipe SS 1 in Pipe Dewar Fitting Dewar & SC Fitting Chiller Fitting SC Fitting Gauge Attachments Pump Fitting Pulse Dampener Fitting SFT Machinery Fitting Relief Valve T-Fitting 20W/ft Heat Tape w/ Jacket Power Connection Line Sensing Thermostat End Seal Copper Tubing Heater Fittings Fiberglass Wrap PolyU. Insulation Alarm Quantity 1 1 1 15 ft 1 2 2 1 20 ft 1 ft 1 3 2 2 3 2 2 1 1 2 25ft 1 1 1 50ft Coil 2 3 1 2 Manufacturer/Description FTS Systems - ULT Series RC210 Madden Manufacturing - Sample Cooler SSI - Prep 250 Diaphragm Pump McMaster Carr - Poly Tubing McMaster Carr - 5 Gallons WIKA Series 213.53-Liquid Filled Omega - RTD Pipe Plug Omega - 1/16 DIN Temperature Controller Swagelok Swagelok Cramer Decker - CGA320 x .25 NPT female Swagelok Swagelok Swagelok Swagelok Swagelok Swagelok Swagelok McMaster Carr - 900-2000psi Relief Valve Swagelok Chromalox Chromalox Chromalox Chromalox McMaster Carr - Copper Tubing Swagelok McMaster Carr - Insulation McMaster Carr - Insulation Omega - 1/16 DIN Temperature Controller Model Number RC210C0 SC106 Prep-250 5545K14 8673T22 Stock # 36287 RTD-NPT-72-E-DUAL-1/4-MTP CN1A-RTD-230VAC SS-T4-S-04-20, 5.69/ft +2CutChge SS-T16-S-083-20, 26.37/ft+2CutChge N832A SS-400-1-4 SS-600-1-4 SS-600-1-6 SS-400-3-4TTF SS-400-1-2 SS-1610-6-4 SS-400-6-2 5026K51 SS-400-3-4TTF SRM/E 20-1CT RTPC RTBC RTES 8955K26 S-600-6-4 4478K1 5431K15 CN1A-RTD-230VAC Total: Cost $14,575.00 $835.00 $4,100.00 $12.15 $127.33 $94.82 $230.00 $168.00 $123.80 $273.70 $17.80 $20.70 $19.00 $22.00 $94.20 $6.60 $167.40 $11.00 $61.85 $31.40 $230.00 $56.10 $194.70 $6.05 $156.38 $9.50 $16.59 $8.93 $168.00 $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. 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. 8
Figure 6 Lab bench setup for testing purposes. The condenser is the large upright cylinder. The chiller used is under the bench.

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 11

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 Can only buy what is available today Trim down unused performance of parts 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.

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Appendix A: Concept Generation Concept 1 Concept 2 Concept 3 Concept 4

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Appendix B: Concept Selection Compressor vs. Pump Relative Ranking

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Compressor vs. Pump

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Appendix C: Initial Calculations Cooling capacity Process Time

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Appendix D: Chiller Selection Chiller Vendors Flow Rate Possible for Given Chiller Cost FTS Chiller Information

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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 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.

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

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

700 600 Flow Rate (mL/min) 500 400 300 200 100 0 $0 Largest Jump in Performance $5,000 $10,000$15,000$20,000$25,000$30,000$35,000$40,000 Chiller Cost ($)

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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 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

o o o

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.

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Appendix E: Condenser Condenser calculations and selection

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Appendix F: Pump Selection Pump Vendors

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Appendix G: Pulse Dampener Selection Pulse Dampener Calculations

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Appendix H: Heater Selection Heater Calculations

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Appendix I: Electrical Electrical Diagram

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Appendix J: Piping Friction Loss Calculations

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Appendix K: Testing Contingency Plan CO2 vs. Butane system layout by processes

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Appendix L: Path Forward Gantt Chart

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