Apeks Supercritical
Setup and Operating Instructions
for
1500-5L and 1500-20L with Automatic CO2 Makeup
Recirculating Subcritical/Supercritical CO2 Extraction Systems
Apeks Fabrication
14381 Blamer Rd
Johnstown OH 43031
www.apekssupercritical.com
Updated 6-17-14
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Copyright Apeks Fabrication 2014
Operating Instructions for CO2 Extraction Systems
Throughout these instructions, this symbol is used to indicate that high
pressure is in the system and failure to follow the instructions as written can
result in a rapid release of pressure potentially causing equipment or personnel
damage.
DANGER – Subcritical and Supercritical CO2 systems operate under high
pressure. Operators must be fully trained and familiar with the system. Failure to
operate the system properly can result in equipment damage and/or bodily injury.
DANGER – Opening a vessel under pressure can result in a rapid release of
pressure and ejection of the material inside the vessel. DO NOT ATTEMPT TO
OPEN A VESSEL UNDER PRESSURE! Always make sure a vent path for the
vessel is opened and the corresponding pressure gage reads zero prior to loosening
the vessel closure bolts.
1. System Setup and Installation
The Apeks Fabrication 1500-5L and 1500-20L subcritical/supercritical CO2 systems
come fully assembled and require only facility hookup and installation.
1.1.
System Requirements and Connections for Installation
The following instructions are recommended for connecting the 1500-5L or 1500-20L
subcritical/supercritical CO2 systems to your facility. Variations in utilities and available
space may require modifications to these recommendations. Contact Apeks Supercritical
to insure installation modifications will not be detrimental to the system.
1.1.1. Location
 CAUTION - The system stores CO2 during use. A suitable location with
adequate ventilation is required to prevent buildup of CO2 which can
cause asphyxiation. Use of a CO2 monitor is recommended for indoor or
low lying applications.
 CAUTION – The 1500-5L system weighs approximately 550 pounds, and
the 1500-20L system weighs approximately 750 pounds. Appropriate
rigging equipment and methods should be used to move the system.
 Use the supplied leveling feet to provide adequate clearance below the
system and to keep the system from sliding when being operated. Use
caution to ensure the leveling feet bolts are not touching the frame. There
should be at least 1/8” clearance between the top of the leveling feet bolt
and the bottom of the frame.
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1.1.2. Electrical
 CAUTION - Do not modify the power connections or attempt to use a
higher or lower voltage than is specified.
 Electrical connections are to be made using the supplied power cords.
 CO2 system control box – 110V, 15A, 50-60Hz, 1 phase. Plug is NEMA
5-15 male.
 Chiller/heater unit – 220V, 15A, 60Hz, 1 phase. Plug is NEMA 6-15
male.
1.1.3. Air
 Compressed air must be non-lubricated and should be filtered to between
5μ and 40μ and have a dew point between 0°F and 50°F
 Max pressure – 150psi. No regulator or lubricator is required.
 Minimum pressure – 100psi.
 Minimum flow – 30 SCFM
 Maximum flow – 120 SCFM
 NOTE: CO2 flowrate (and subsequently extraction time) is proportional to
air flow
 CO2 system air connection is ½” NPT female. Connection to facility
compressed air should be made through a minimum ½” inner diameter
pipe or flexible hose. Runs longer than 50 feet should be ¾” minimum
inner diameter.
 Always follow the air compressor manufacturer’s operating instructions to
insure proper performance of the compressed air system.
1.1.4. Water Chiller/Heater
 Chiller/heater unit is designed for use in an area where room temperature
is less than 85F. Higher temperatures will adversely affect the cooling
capacity of the chiller.
 Circulating fluid - Recirculating chiller/heater fluid should be a mixture of
50/50 water and propylene glycol to prevent freezing and improve heat
transfer. Plain distilled water can be used for temperatures above 32F if
propylene glycol is not available. – DO NOT USE DEIONIZED WATER.
 Volume – Total volume of fluid in the cooling/heating water jackets on the
vessels and chiller/heater reservoir is approximately 4 gallons for the
1500-5L, and 12 gallons for the 1500-20L.
 Outlet connection - Connect the chiller/heater “OUTLET” to the back
connection (inlet) of the temperature control heat exchanger.
 Inlet connection – Connect the chiller/heater “INLET” to the top (outlet)
of the 2nd separator jacket.
 Remote Probe - With the chiller/heater power off, connect remote
temperature sensor to the “REMOTE PROBE” connection on the back of
the chiller. CAUTION – DO NOT CONNECT/DISCONNECT THE
TEMPERATURE PROBE WHILE THE CHILLER IS UNDER POWER.
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It may be necessary to adjust the chiller settings for Remote Probe Control mode:
1. To verify chiller is in Remote Probe Control mode, press
“Menu” button until the left display shows “P1” or “P2”
2. If left display shows “P1”, then chiller is in Remote Probe
Control mode and no other adjustments are necessary. Press
menu 1 time so the left display shows water pressure in “psi”.
NOTE: When “P1” is displayed on the left screen, the chiller’s
internal temperature probe reading is displayed on the right
screen.
3.


If left display shows “P2”, then press and hold menu button for
3 seconds, press menu button until “rP” is displayed on the left,
and use the temperature control knob to adjust the right setting
to “rPC”. Wait for 10 seconds for the chiller to reset out of the
menu mode, then repeat step 1 and 2 to verify changes.
Circulating fluid is added to the system through the reservoir cap on the
top of the chiller/heater while the chiller/heater is running. Maintain a
visible level of fluid in the chiller/heater reservoir during operation.
More detailed operating instructions for the heater/chiller can be found in
the manufacturer’s operating instructions.
1.1.5. CO2
 CO2 should be beverage grade or better for operations that come in
contact with food product.
 1500-5L system holds 8-12# of liquid CO2 while operating. A minimum
50# CO2 cylinder is recommended for this system
 1500-20L holds approximately 30-40# of liquid CO2 while operating. A
minimum 75# CO2 cylinder is recommended for this system
 CO2 system connection is CGA-320.
 The supplied hose should be connected directly to the CO2 bottle valve.
No regulator is required. A supplied CGA-320 plastic gasket is required
to seal the connection between the hose and the CO2 bottle.
 CO2 cylinder should be high pressure gas feed with no check valves.
Siphon tube or dip tube bottles can cause system blockages during startup
and should not be used.
 NOTE: a liquid CO2 dewar is not recommended due to the limited amount
of CO2 lost during the extraction process.
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2. Theory of Operation
The 1500-5L and 1500-20L systems perform botanical oil extractions using CO2 as a
solvent. When CO2 is a supercritical fluid or a subcritical liquid it has the ability to
dissolve and carry certain oils, waxes and other soluble compounds from botanical plant
materials. When the supercritical/liquid CO2 with suspended oils and waxes is
subsequently decompressed, the CO2 loses its ability to hold the suspended oils and
waxes in solution and drops them out of solution at the point of decompression. In
addition to the oil and wax extraction, the 1500-5L and 1500-20L systems also recirculate
the CO2 during operation and recover the CO2 at the end of the extraction to minimize
CO2 loss.
The extraction process begins in the Extraction Vessel. CO2 in either a liquid state
(Figure 2) or supercritical state (Figure 3) enters the Extraction Vessel where it will
dissolve oils/waxes from the botanical plant material and carry it over to the Valveless
Expansion Technology (VET) mechanism in the separator vessel. The
supercritical/liquid CO2 is decompressed through the VET mechanism which causes it to
change phase into a gas and subsequently drop the suspended oil/wax into the separator
vessel. The heavier oil and wax will collect in the bottom of the separator vessel.
After oil and wax separation, the cold, gaseous CO2 is directed to the inlet of the pump
where it is recompressed. The pump discharge is cooled in the regenerative heat
exchanger by the water cooling circuit, and then is cooled/heated to the appropriate
temperature by the temperature control heat exchanger and water chiller/heater. The
liquid or supercritical CO2 then enters the Extraction Vessel to extract more oils and
waxes again.
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Figure 1 – Subcritical CO2 System Dynamics During Operation
Figure 2 - Supercritical CO2 System Dynamics During Operation
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3. System Operation
These operating instructions are for 1500-5L and 1500-20L systems with Valveless
Expansion Technology mechanism and automatic CO2 makeup installed.
3.1.
Orifice Selection
The size of the orifice must be chosen such that the flow of CO2 into the separators
matches the flow of CO2 from the gas booster. The following are recommended settings
for choosing the correct orifice:
3.1.1. Supercritical CO2
NOTE: external cooling for the CO2 pump must be applied for supercritical parameters
Chiller/heater temperature – 110F to 120F
Extraction pressure – 1200-1300psi
Orifice size:
 30CFM air flow (~7.5 HP air compressor) – #15 orifice
 60CFM air flow (~15 HP air compressor) – #20 orifice
 100CFM air flow (~25 HP air compressor) – #25 orifice
Weight of CO2 in system – 6-8 pounds for the 5L systems, 20-25 pounds
for the 20L systems
Separator pressure – 250-300psi
Separator temperature – 50F to 80F
3.1.2. Subcritical CO2
Chiller/heater temperature – 60F to 65F
Extraction pressure – 1200-1300psi
Orifice size:
 30CFM air flow (~7.5 HP air compressor) – #10 orifice
 60CFM air flow (~15 HP air compressor) – #15 orifice
 100CFM air flow (~25 HP air compressor) – #20 orifice
Weight of CO2 in system – 8-12 pounds for the 5L systems, 30-40 pounds
for the 20L systems
Separator pressure – 250psi to 300psi
Separator temperature – 20F to 30F
3.2.
Loading Material into the Extraction Vessel
DANGER – Opening a vessel under pressure can result in a rapid release of
pressure and ejection of the material inside the vessel. DO NOT ATTEMPT TO
OPEN A VESSEL UNDER PRESSURE! Always make sure a vent path for the
vessel is opened and the corresponding pressure gage reads zero prior to loosening
the vessel closure bolts.
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3.2.1. Opening the Extraction Vessel
NOTE: This operation cannot be performed during an extraction. The
extraction must be stopped prior to opening the Extraction vessel
 Shut valves 1 and 2.
 Open valves 3 and 4.
 Remove the bolts on the top of the vessel using a 1.5” impact socket and
impact wrench.
 Lift the flange and allow it to rest in the open position on the stops.
 Use caution not to scratch or otherwise damage the o-ring sealing surfaces
on the flanges.
3.2.2. Loading the Extraction Vessel
 The system scale can be used to weigh the amount of material loaded.
Tare the scale by pushing the “tare/reset” key.
 Media to be extracted can be loaded directly into the Extraction Vessel.
The supplied funnel can help minimize spillage. Media can be ground to a
particle size as small as 50 micron, but particles about the size of coffee
grounds generally works well.
 Any amount of material can be loaded into the Extraction Vessel – it does
not have to be full in order to operate correctly
 Gentle compression can be used to increase the amount of material loaded
in the vessel, however heavy compaction should be avoided to prevent
CO2 channeling through the material upon startup.
3.2.3. Sealing the Extraction Vessel
 Once the desired amount of material is loaded into the Extraction Vessel
the vessel can be closed and sealed
 Ensure all sealing surfaces are clean and free of debris
 Check the o-ring for any visible damage or defects. Replace as necessary
 The o-ring does not require any lubrication
 Close the vessel flange and install each of the closure bolts hand tight
 Using the supplied impact wrench and socket, tighten the bolts in a star
pattern. Use the supplied impact wrench with 1-2 second bursts to
deliver approximately 50 ft-lbs of torque to each bolt. Heavy
torqueing of the bolts is not required.
3.3.
Evacuating entire system
To remove any moisture from the system the entire system must be evacuated. Evacuate
using these steps:
3.3.1. Open all valves on system except CO2 bottle valve and valve 4.
3.3.2. Connect vacuum pump to valve 10, open valve 10, and turn vacuum
pump on to vacuum system down to 20-25 in.Hg.
3.3.3. Hold vacuum for several minutes to ensure no gross leaks and to remove
moisture.
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3.3.4.
3.4.
Shut all valves and disconnect vacuum pump and vacuum gage from
valve 10.
Fill system with CO2 and start extraction
Filling the system with CO2 is accomplished with the following steps:
3.4.1. Tare the scale by pushing the “tare/reset” key.
3.4.2. Open CO2 bottle valve.
3.4.3. Open valves 1, 3, 5, and 7.
3.4.4. Pressurize and fill Extractor by slowly opening valve 13. Allow
Extractor pressure to equalize with the CO2 bottle pressure.
3.4.5. Once Extractor pressure has equalized with the CO2 bottle pressure, shut
valves 5 and 13.
3.4.6. Pressurize separators to 300psi by opening valves 11 and 12. Adjustment
of the green handled regulating valve may be necessary to set the
separators to approximately 300psi.
3.4.7. Close valve 11.
3.4.8. Open valve 14.
3.4.9. Turn the start/stop switch on control panel to “START” to start the CO2
pump.
3.4.10. Once Extractor pressure has reached approximately 1200psi, close valve
14, and open valves 6 and 11.
3.4.11. If necessary, adjust the green handled regulating valve to maintain 300psi
in the separators and a corresponding1200psi in the extraction vessel.
NOTE: changes may take several minutes to stabilize – make changes in
small increments and allow at least 5 minutes between changes.
3.5.
Removing CO2 to Maintain Pressure
The system is now circulating CO2 and extracting. In the event that the system is
overfilled with CO2 due to ambient temperature variations the system may shut down on
Extractor over pressure. Decrease the Extractor pressure as follows:
3.5.1. Turn the green handled regulating valve in the “decrease” direction
approximately ¼ turn to avoid overloading the CO2 again.
3.5.2. Shut valves 1 and 5 (or check that they are both shut) and QUICKLY
open and shut valve 13, then QUICKLY reopen valve 1 or 5 (whichever
was previously opened).
3.5.3. Allow system to stabilize for 5 minutes and repeat as necessary
3.6.
Setting extraction timer
The control system is equipped with a timer that will automatically shut down the system
after a set amount of time has elapsed. The timer can be adjusted at any time during the
extraction. Actual time elapsed is displayed as red text.
To set the timer:
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


3.7.
Use the up or down arrow keys on the timer controller to set the desired run time
(green text)
Use the left arrow to adjust the place setting (HH:MM)
Press “MODE” to lock in the new time
Flow Reversal
It may be necessary to reverse the flow in the Extraction Vessel during operation to either
back flush a clogged filter, to prevent channeling through the media, or both.
The Extractor vessel filter may need back flushed if a differential pressure greater than
300 psi exists between the Extractor pressure and either the inlet or outlet pressure for the
Extractor.
Note: these instructions assume the valves are in the original positions. If a reversal has
already been performed, use the valves in parenthesis
3.7.1. Extractor Flow Reversal
3.7.1.1.
Open valve 5 (valve 1)
3.7.1.2.
Open valve 2 (valve 6)
3.7.1.3.
Shut valve 1 (valve 5)
3.7.1.4.
Shut valve 6 (valve 2).
3.8.
Orifice clog
On rare occasions it may be necessary to clean the orifice during operation. The orifice is
clogged when separation pressure continually decreases with a corresponding increase in
extraction pressure.
To clear a clogged orifice filter:
3.8.1.
Shut valve 2 and valve 6 (only one of them will be open).
3.8.2.
Shut valve 12.
3.8.3.
Allow the pump to draw the CO2 out of the separators and transfer the
CO2 to the Extraction vessel.
3.8.4.
When Extraction Vessel pressure reaches 1400psi, shut valves 1 and 5
(only one of them will be open), then quickly open valve 13 to direct the
remaining CO2 in the separators back to the storage bottle.
3.8.5.
When the separators reach approximately 70 psi, the pump will
automatically turn off.
3.8.6.
Shut valve 13
3.8.7.
Open valve 1 or 5 (whichever was previously opened).
3.8.8.
Shut valve 11.
3.8.9.
Open valve 10 to relieve any residual pressure in the separators. Leave
valve 10 open to allow any residual pressure to vent.
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3.8.10.
3.8.11.
3.8.12.
3.8.13.
3.8.14.
3.9.
Remove the 1st separator cap and remove the orifice. Clean the orifice by
removing it and soaking it in acetone or ethanol and blowing it out with
compressed air. Verify the orifice is clear by looking through it.
Reassemble the orifice using the provided Teflon tape. Use caution to
prevent excess Teflon tape from getting into the orifice. Tighten the
orifice assembly such that the orifice points toward the separator wall.
Replace the 1st separator cap and tighten the clamp bolts to 20 ft-lbs
Shut valve 10
Open valve 11, valve 12 and valve 2 or 6 (whichever was previously
open). The pump will automatically re-start when separator pressure
reaches 70psi.
CO2 Recovery
Once the extraction is complete, recover the CO2 as follows. NOTE: if the system shut
down with the timer, it will be necessary to switch the system to “STOP” to reset the
timer, then returning the system to “START” to start the pump.
3.9.1. To recover the CO2 from the system:
3.9.1.1. Increase the temperature of the chiller/heater to 110F.
3.9.1.2. Open valve 6 and shut valve 2 (they may already be in this position).
3.9.1.3. Shut valves 1 and valve 5 (only one of them will be open).
3.9.1.4. Quickly open valve 13 to allow flow into the CO2 bottle.
3.9.1.5. Shut valve 12
3.9.1.6. When Extractor pressure is below 700psi, shut valve 6 and open valves 2
and 8.
3.9.1.7. The pump will shut down automatically when separator pressure reaches
70psi.
3.9.1.8. Shut CO2 bottle valve.
3.9.1.9. Vent remaining CO2 in system by opening valves 10, 1 and 4.
NOTE: LEAVE VALVES 10, 3 and 4 OPEN TO ALLOW ANY
RESIDUAL PRESSURE IN THE SYSTEM TO VENT
The system can now be powered down, or new extraction media can be reloaded and the
extraction process and be started again.
4. System Error Messages
The 1500-5L and 1500-20L control system will monitor and attempt to protect the system
in the event of an overpressure or underpressure condition. There are 4 system errors:
High Separator Pressure - Pressure in the Separator Vessels is higher than 500psi.
High Extractor Pressure – Pressure in the Extraction Vessel is higher than 1500psi.
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Low Separator Pressure – Pressure in the Separator Vessels is less than 70psi.
Air Pressure Fault – Air Pressure is greater than 140psi or less than 40psi.
5. System Maintenance
Maintenance on the system is critical to proper operation. Failure to follow these
maintenance items can cause premature system failure. The maintenance items below
pertain to the CO2 system only. Follow the manufacturer’s recommended maintenance
plan for the chiller/heater unit and the compressed air system.
This maintenance schedule assumes an 8 hour daily operating schedule. More frequent
operation will require more frequent maintenance operations.
Frequency
After Each
Extraction
Weekly
Bi-Weekly
Updated 6-17-14
Maintenance Item
 Extraction vessel – remove spent material from the extraction
vessel by either vacuuming it out through the top flange, or by
opening the bottom flange and catching the material in a receptacle.
 Verify the extractor filters are clear and free of debris
 Check extraction vessel oring and oring groove sealing surfaces for
damage – replace if necessary
 Separator vessels – remove extracted oil from separator vessels
and clean with alcohol or other acceptable solvent. Remove any oil
carryover from the flow line between the separators with alcohol
and compressed air.
 Check separator vessel gaskets for damage – replace if necessary
Pump Inlet Line
 Disconnect the flexible line connecting the outlet of Separator #2 to
the CO2 pump and disconnect the stainless tubing from the inlet
side of the CO2 pump. Open valve 11, clean flexible line and
tubing with acetone or alcohol, then blow out with compressed air.
 Lubricate CO2 pump spool valve orings. Replace if necessary.
 Clean CO2 flow lines from separator #2 to the CO2 pump with
alcohol and compressed air. Disassembly of the flowlines may be
necessary.
 Check chiller/heater water level is between min and max
 Check CO2 pump seals for wear - While system is operating,
remove piston vent filters (4 total) and verify no flow for
compressed air piston vents (point toward front of system), and
intermittent suction/pressure for CO2 piston vents (point toward
back of system)
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Monthly
Updated 6-17-14
 Check air operated safety valve operation – during operation, turn
start/stop switch to stop and verify valve coupling rotates 90
degrees quickly and without hesitation. “Ext Out” gage reading
should drop to match separator pressure. Restart process and verify
valve coupling rotates 90 degrees in the opposite direction. Contact
Apeks immediately if valve is not operating properly.
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Figure 4 - PID drawing for 1500-5L and 1500-20L CO2 systems.
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Figure 5 – Extraction Vessel for 1500-20L Supercritical CO2 system.
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Figure 6 – Extraction Vessel for 1500-5L Supercritical CO2 system.
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Figure 7 – Separator Vessels for 1500-20L and 1500-5L Supercritical CO2 system.
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