Apeks Supercritical

Setup and Operating Instructions

for

1500-5L and 1500-20L

Recirculating Subcritical/Supercritical CO2 Extraction Systems

Apeks Fabrication
14381 Blamer Rd
Johnstown OH 43031
www.apekssupercritical.com

Updated 6-12-2013 1 Copyright Apeks Fabrication, 2013

 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 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 clearance between the top of the leveling feet bolt and the
bottom of the frame.

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 made using the supplied power cords.
Updated 6-12-2013 2 Copyright Apeks Fabrication, 2013
 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
5 and 40 and have a dew point between 0F and 50F
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 NPT female. Connection to facility
compressed air should be made through a minimum inner diameter
pipe or flexible hose. Runs longer than 50 feet should be minimum
inner diameter.
Always follow the air compressor manufacturers operating instructions to
insure proper performance of the compressed air system.

1.1.4. Water Chiller/Heater

Circulating fluid - Recirculating chiller/heater fluid should be a mixture of
50/50 water and propylene glycol to prevent freezing for operating
temperatures below 32F. Plain distilled water can be used for
temperatures above 32F if glycol cannot be used. 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 3 gallons.
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.

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 5 times 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.

Updated 6-12-2013 3 Copyright Apeks Fabrication, 2013

 NOTE: When P1 is displayed on the left screen, the chillers
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 6 times 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.

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 manufacturers 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 approximately 12# of liquid CO2 while operating
1500-20L holds approximately 35# of liquid CO2 while operating
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 storage bottle should be high pressure liquid (siphon or dip tube) or
gas feed with no check valves. Siphon tube bottles will fill the system
faster on startup, but are only recommended for use by experienced
operators due to the rapid changes in pressure that occur during system
startup.
NOTE: a liquid CO2 dewar is not recommended due to the limited amount
of CO2 lost during the extraction process.

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 liquid it has the ability to dissolve and
carry certain oils, waxes and other compounds from botanical plant materials. When the
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 usage.

Updated 6-12-2013 4 Copyright Apeks Fabrication, 2013

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) orifice 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 heated in the regenerative heat
exchanger by heat from the pump discharge, and is directed to the inlet of the pump
where it is compressed to 1100-1200 psi. The pump discharge is cooled in the
regenerative heat exchanger by the gaseous CO2 from the separator, 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.

Figure 1 Subcritical CO2 System Dynamics During Operation

Updated 6-12-2013 5 Copyright Apeks Fabrication, 2013

 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 Technlogy orifice installed.

3.1. Cleaning the system

The 1500-5L and 1500-20L systems are constructed from 304 or 316 stainless steel and
can be cleaned with any cleaner that is compatible with both stainless steel and your
extracted product. Simple Green cleaner works well for most applications.

Apeks Fabrication takes great care to ensure all manufacturing oils and fluids are cleaned
from the system prior to shipping, however the user should verify the system is cleaned to
the appropriate level prior to processing any materials.

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.

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
Close valves 1 and 2.
Open valves 3 and 4.
Remove the bolts on the top of the vessel using a 1-1/2 impact socket and
supplied 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 using your hand can be used to increase the amount of
material loaded in the vessel, however heavy compaction should be
avoided to prevent compaction of the material upon initial loading.
Updated 6-12-2013 7 Copyright Apeks Fabrication, 2013
 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 air and moisture the entire system must be evacuated:
3.3.1. Open all valves on system except CO2 bottle valve and valve 4.
3.3.2. Connect vacuum pump to valve 10 and pump system down to 20-25
in.Hg.
3.3.3. Hold vacuum for several minutes to ensure no gross leaks and to remove
all moisture.
3.3.4. Close all valves and disconnect vacuum pump from valve 10.

3.4. Fill system with CO2 and start extraction

The steps below assume the following conditions exist:

Compressed air is available at ~125psi and 30 CFM minimum.

Chiller/heater is operating and circulating in the temperature control heat
exchanger and the vessel jackets at the desired temperature.
Control panel is connected to 115VAC and is powered on.
CO2 cylinder is connected to the system and has at least 20# of liquid available
(1500-5L) or 40# (1500-20L).

Fill the system with CO2:

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 and
the weight scale is no longer increasing, shut valves 5 and 13.
3.4.6. Pressurize separators to 300psi by opening valve 12 and throttling valve
11. Close valve 11 when separator pressure is approximately 300 psi. DO
NOT OVERPRESSURIZE SEPARATORS.

Updated 6-12-2013 8 Copyright Apeks Fabrication, 2013

 3.4.7. Turn the switch to START on control panel. When Extractor pressure
reaches approximately 1200psi, QUICKLY open valve 6, shut valve 12,
and open valve 11.
3.4.8. Allow system to stabilize for approximately 5 minutes.

3.5. Adding or Removing CO2 to Maintain Pressure

The system is now circulating CO2 and extracting. It may be necessary to adjust the
amount of CO2 in the system to maintain the desired extraction pressure:

3.5.1. To increase Extractor pressure

3.5.1.1. Shut valve 11 and open valve 12 until Extractor reaches 1400psi or
the separators reach 450 psi (whichever happens first), then shut
valve 12 and open valve 11.
3.5.1.2. Allow system to stabilize for 5 minutes and repeat as necessary.

3.5.2. To decrease Extractor pressure

3.5.2.1. Shut valve 1 or 5 (only one valve will be open) and QUICKLY
open and shut valve 13, then QUICKLY reopen valve 1 or 5
(whichever was previously opened).
3.5.2.2. 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:

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

3.7. 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 backflushed if a differential pressure greater than
300 psi exists between the Extractor pressure and either the inlet or outlet pressure for the
Extractor.

To reverse flow through 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):

Updated 6-12-2013 9 Copyright Apeks Fabrication, 2013

 3.7.1. Open valve 5 (valve 1)
3.7.2. Open valve 2 (valve 6)
3.7.3. Shut valve 1 (valve 5)
3.7.4. 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:

3.8.1. Shut valve 2 or valve 6 (only one of them will be open).
3.8.2. Allow the pump to draw the CO2 out of the separators and transfer the
CO2 to the Extraction vessel.
3.8.3. When Extraction Vessel pressure reaches 1400psi, shut valve 1 or 5 (only
one of them will be open) and QUICKLY open valve 13.
3.8.4. When the separators reach approximately 70 psi, the pump will
automatically turn off.
3.8.5. Shut valve 13, open valve 1 or 5 (whichever was opened previously).
3.8.6. Shut valve 11.
3.8.7. Open valve 10 to relieve any residual pressure in the separators. Leave
valve 10 open to allow any residual pressure to vent.
3.8.8. Remove the 1st separator cap and remove the orifice. Clean the orifice by
soaking it in acetone or methanol and blowing it out with compressed air.
Verify the orifice is clear by looking through it.
3.8.9. 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.
3.8.10. Replace the 1st separator cap and tighten the clamp bolts to 20 ft-lbs
3.8.11. Close valve 10
3.8.12. Open valve 11
3.8.13. Restart the CO2 pump by slowly throttling valve 12. Close valve 12
when the pump automatically re-starts. DO NOT OVERPRESSURIZE
SEPARATORS.
3.8.14. Open valve 2 or valve 6 (whichever valve was previously opened)
3.8.15. Increase or decrease Extractor pressure per section 2.5.

3.9. 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.

To recover the CO2 from the system:

Updated 6-12-2013 10 Copyright Apeks Fabrication, 2013

 3.9.1. Increase the temperature of the chiller/heater to 110F.
3.9.2. Open valve 6 and shut valve 2 (they may already be in this position).
3.9.3. Shut valve 1 or valve 5 (only one of them will be open) and QUICKLY
open valve 13 to allow flow into the CO2 bottle.
3.9.4. When separator pressure is less than 150psi, shut valve 6 and open valve
2 and valve 8.
3.9.5. The pump will shut down automatically when separator pressure reaches
70psi.
3.9.6. Close CO2 bottle valve.
3.9.7. 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. Orifice Selection and Recommended Parameters

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:

4.1. Supercritical CO2

Chiller/heater temperature 110F to 120F

Extraction pressure 1200psi
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 approximately 10 pounds for the 5L systems, 25 pounds for
the 20L systems
Separator pressure - 300psi to 350psi
Separator temperature 70F to 80F

4.2. Subcritical CO2

Chiller/heater temperature 60F to 70F

Extraction pressure 1100psi
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

Updated 6-12-2013 11 Copyright Apeks Fabrication, 2013

Weight of CO2 in system approximately 12 pounds for the 5L systems, 35 pounds for
the 20L systems
Separator pressure 250psi to 300psi
Separator temperature 20F to 30F

NOTE: Subcritical CO2 operation requires the Extraction Vessel be completely full of
liquid CO2. It may be necessary to add CO2 to the system several times per section 2.5
to maintain the desired extraction pressure.

5. 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.

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.

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4.

Figure 1 - PID drawing for 1500-20L Supercritical CO2 system.

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Figure 2 - PID drawing for 1500-5L Supercritical CO2 system.

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Figure 3 Extraction Vessel for 1500-20L Supercritical CO2 system.

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Figure 4 Extraction Vessel for 1500-5L Supercritical CO2 system.

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Figure 5 Separator Vessels for 1500-20L and 1500-5L Supercritical CO2 system.

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 Apeks Supercritical 1500-5L/20L Extraction System Operating Log
Run #
Date

Pre-extraction Post-extraction
Time Started Time Stopped
Weight of material loaded in vessel (g) Weight of oil collectd (g)
Weight of material loaded in vessel (lbs) Room Temperature (F)
CO2 bottle #1 pressure at start (psi)
CO2 bottle #1 pressure after filling (psi)
CO2 bottle #2 pressure at start (psi)
CO2 bottle #2 pressure after filling (psi)
Total weight of CO2 added to system (lbs)
Room Temperature (F)

Extractor Pump Extractor

Timer Pump Out Extractor Out Separator Separator Water Extractor Separator Air Cycling Scale Flow
Reading Pressure A pressure Pressure #1 Press #2 Press Temp (P1) Temp (P2) #1 Temp Pressure Rate Reading Direction Comments
HH:mm psi psi psi psi psi F F F psi sec lbs up/down

Version 1.0. Copyright Apeks Fabrication 2013

Updated 6-12-2013 Copyright Apeks

18 Fabrication, 2013