Applied Separations Spe-ed SFE-2 User manual

Applied Separations · 930 Hamilton Street · Allentown, PA 18101
www.appliedseparations.com
SFE Manual
Disclaimer of Documentation Warranty
This publication is provided “as is” without warranty of any kind, express or implied. Applied
Separations does not warrant, guarantee, or make any representations regarding the use, or the
results of the use, of this publication in terms of correctness, accuracy, reliability, correctness, or
otherwise. Further, Applied Separations reserves the right to revise this publication and to make
changes from time to time in content herein without obligation of Applied Separations to notify any
person or organization of such revision or changes.

Applied Separations · 930 Hamilton Street · Allentown, PA 18101
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TABLE OF CONTENTS
INTRODUCTION Section 1
Purpose of Spe-ed™ SFE 1.1
Specifications 1.2
Site Preparations 1.3
Pre-Installation 1.4
Overview of Features 1.5
REQUIRED UTILITIES Section 2
Liquid Carbon Dioxide 2.1
Electricity 2.2
Compressed Air 2.3
Recirculating Coolant 2.4
ASSEMBLY AND SET-UP Section 3
Front/Rear Views 3.1
Attaching the Liquid CO2Tank 3.2
Power 3.3
Compressed Air 3.4
CO2Outlet Port
(Oven/Pump Module Connection) 3.5
CO2Safety Head Outlet 3.6
Connecting Recirculating Coolant 3.7
Connecting the Flow Meter 3.8
EXTRACTOR VESSEL PACKING Section 4
Extractor Vessel Packing 4.1
In-Line Analyte Trapping 4.2
Vessel Packing Example 4.3
SYSTEM OPERATIONS Section 5
Setting Oven and Control and Collection
(C&C)Modules 5.1
Inlet, Outlet, Vent, Micro-metering,
and Fluid Delivery Valves 5.2
Operating the Spe-ed SFE 5.3
Pressurization of the SFE Plumbing System 5.31
Depressurizing the SFE via Vent Valves 5.32
Flushing the Transfer Lines 5.33
Overview of Off-line Extraction Procedure 5.4

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OPTIONS Section 6
Spe-ed SFE Modifier Pump Module 6.1
MAINTENANCE Section 7
Cleaning 7.1
Preventive Maintenance 7.2
TROUBLESHOOTING Section 8
Emergency Operating Procedures
ACCESSORIES Section 9
APPENDIX A
Calibrating the Pressure Monitor Display
APPENDIX B
Specifics of the Keypad and the Temperature Control
APPENDIX C
Spe-ed SFE Configurations
APPENDIX D
Example Applications
APPENDIX E
Extractor Vessel Information
APPENDIX F
Spe-ed SFE Electric CO2 Pump Set-up / Operation

Applied Separations · 930 Hamilton Street · Allentown, PA 18101
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INTRODUCTION Section 1
Although most references and figures refer to the Spe-ed SFE model 7070 (SFE-2, 120VAC), 7071
(SFE-2, 240VAC) the information in this manual applied equally to our models 7011 (SFE-NP,
120VAC), 7013 (SFE-NP, 240VAC), 7072 (SFE-4, 120VAC), 7073 (SFE-4, 240VAC).
When using this manual in conjunction with the 7072 or 7073, the user must be aware that these
units have the capacity to support 4 vessels; figures showing 2 vessels should be reinterpreted for the
appropriate number.
Warranty
This manual provides basic information for the user to install and operate the Spe-ed SFE, the
maintenance required, and how to obtain necessary service or parts. WARNINGS, CAUTIONS and
NOTES are used throughout this manual to emphasize pertinent or critical instructions to the user
according to the following definitions.
Warning A procedure, that if not followed properly, can prove to be extremely
hazardous to the operator, the environment, or both.
Caution Emphasizes a procedure that must be followed to avoid possible damage to
the instrument.
Note Highlights important information about the instrument or procedures associated with
the operation of the instrument.
Several internationally accepted symbols are used to label certain parts of the system and
throughout this Operator Manual as required for CE Mark Safety Certification. These
symbols are defined below.
Caution Risk of Electric Shock- High voltage exists within enclosures. Allow access
to qualified personal only.
Easily Touched Higher Temperature Parts Surface is normally hot
during operation. Exercise caution when operating in this area.
Caution (refer to accompanying documents)- Read Operators Manual before
applying power or operating system.

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Purpose of the Spe-ed SFE 1.1
The Spe-ed SFE allows an analyst to perform supercritical fluid extractions simply and efficiently.
Developed in conjunction with the USDA, the Spe-ed SFE has achieved simple sophistication in
design and use. With its flexibility of both dynamic (continuous flow) and static (where supercritical
CO2is pressurized in a sealed extraction vessel for a specific period of time) modes, the Spe-ed SFE
offers precise, repeatable performances for a variety of laboratory procedures including, but not
limited to:
•Extracting pesticides and PAHs from soil samples
•Extracting antibiotics and steroids from veterinary products
•Extracting natural products
•Extracting monomers from polymeric compounds
•Extracting fat from food products
(For specific application procedures, please see Appendix D.)
Specifications 1.2
Physical Dimensions
Oven (including Controller)
Outside: 13”w x 20 1/2” D (115v Circulating Fan Motor) x 28” H
13”w x 21 3/4” D (240v Circulating Fan Motor) x 28” H
Inside: 10”w x 9” D x 19” H
Pump Module
Outside: 16”w x 18” D x 8 1/2” H
Electrical
Oven Module
120 VAC/ 60Hz @ 17A 220-240VAC/[email protected]
Use 20A TimeDelay 1/4”X11/4” Use 10A Time Lag 5X20mm Fuse
Pump Module
120 VAC/ 60Hz @ .5A 220-240VAC/[email protected] max.
Use.5A TimeDelay 5x20mm Fuse Use .25A Time Lag 5X20mm Fuse
Warning To avoid fire hazard, replace fuses only with the same type and rating as
specified in Operator Manual and labeled on back of system.
Caution High Voltage exists within enclosure. Allow access to qualified personal
only.

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Warning The Spe-ed SFE instrument may be pressurized to10,000 psi (690 Bar) at
temperatures up to 240C. Check with the extractor vessel manufacturer to determine
whether vessels used can withstand the pressures and temperatures that the Spe-ed SFE is
capable of delivering. Do not operate the Spe-ed SFE beyond the MAWP (Maximum
Allowable Working Pressure) of the vessel. No warranties are given on the extraction
vessels beyond those provided by the manufacturers.
Caution The Spe-ed SFE was designed to use CO2 or CO2containing organic
solvent modifiers only. The use of any other fluid will render all warranties void.
Caution This instrument is not intended for use with Nitrous Oxide, or with
corrosive compounds such as ammonia or sulfur hexafluoride, which can form an
explosive mixture with organic compounds.
Site Preparation 1.3
Location Bench Space Required
Width
Oven Module 22”
Pump Module 22”
Depth
Oven Module 22”
Pump Module 22”*
Height
Oven Module 28”
Pump Module 9”
Weight
Oven Module 100 lb.
Pump Module 55 lb.
*Rear access occasionally required to drain air filter or replace broken rupture disc.
If you are setting up the Spe-ed SFE in a stacked configuration, you may want to keep the height of
the table less than 33” (84cm) high so that an operator can reach all parts of the instrument. The Spe-
ed SFE can also be set up in a side-by-side configuration.
Compressed Air Line
The Spe-ed SFE requires a compressed air line (or cylinder) with a minimum delivered pressure of
100 psig (6.9 BAR) and capacity of 6.2 actual cfm (cubic ft./min.) or 48 standard cfm. The
compressor should be set to turn on at 95 psig (6.6 BAR) and turn off at 125 psig (8.6 BAR)
Electricity
The Spe-ed SFE will need a dedicated electrical outlet of 120VAC, 20 amps or 240VAC, 10 amps.

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Vial Venting
Accessory connections and tubing are available for venting into collection vials and flow meter
hookup.
Pressure Relief Connections
A 3/8” female NPT fitting can be connected to a CO2safely head outlet. This connection may be
used to direct emergency venting to a remote location in the event of a rupture disc failure.
Cylinder Safety Requirement
Provisions should be made for clamping the CO2cylinder to either a permanent table edge or wall by
using the appropriate cylinder bracket.

Applied Separations · 930 Hamilton Street · Allentown, PA 18101
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Pre-Installation 1.4
The following items are included with your Spe-ed SFE. If any are missing, please contact Applied
Separations.
• Spe-ed SFE Oven Module, P/N 7700/7260/7760, 120 VAC; 7701/7761/7761, 240 VAC
• Spe-ed SFE Pump Module, P/N 7102, 120 VAC; 7103, 240 VAC
• Spe-ed SFE Control & Collection Module (Micrometering Valves)
• Power cord (for oven), P/N 7759, 120 VAC; 7763, 240 VAC
• Power cord (for oven to pump), P/N 7105
• Solvent collection rack, P/N 7798
• Extractor vessel oven brackets (2), P/N 7932
• Discharge tube for collection in solvents (1), P/N 7713
• Sample of polypropylene wool, P/N 7952
• SPE Vent Adaptor, P/N 7732
• Collection Tube Vent Assembly, P/N 7733
• Flow meter Kit, P/N 7928
Note Other necessary parts and accessories may have been on your order and are included
in the shipment. Check your packing slip and invoice.
Save the Spe-ed SFE boxes and packing materials for use if it becomes necessary to return the Spe-
ed SFE for service.
Tools needed for assembly:
Wrenches: 5/16”, 1/2”, 9/16” and 5/8” sizes
OR
8mm, 13mm, 15mm, and 16mm
Extractor vessels are required for operation (See “Accessories” section of this manual).
If you have additional questions about the assembly or operation of the instrument, contact Applied
Separations Engineering Services Office at [phone].
• Sample of polypropylene frits, P/N 7956

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REQUIRED UTILITIES SECTION 2
Liquid Carbon Dioxide (CO2) 2.1
Most analyses will require SFE grade CO2or CO2passed through a CO2clean-up column. (See the
“Accessories” section of this manual.) A dip tube will be required in the CO2cylinder.
Caution The CO2cylinder must contain a dip tube to ensure that liquid CO2is
delivered to the pump module.
Note The CO2tank shut-off valve controlling the carbon dioxide must be opened before the
pump module system can be pressurized.
Note Refer to section 3 for operating instructions with a refrigerated cooling bath (RCB).
Note Prior to operating Spe-ed RCB, it is important to pressurize the SFE pump to a
minimum CO2Pressure. After opening the CO2tank, slowly increase pressure to avoid pump
cavitation, and then turn on RCB. When RCB reaches the desired cooling temperature, operating
pressure may be increased of decreased to its optimum setting.
Electricity 2.2
The Spe-ed SFE will operate with a dedicated circuit on either:
120 VAC / 60Hz, 20 amps
OR
240 VAC / 50Hz, 10 amps
For use outside the United States, the power cord will require an appropriate adaptor. Your dealer
will be able to assist you in the necessary adaptation for your specific power supply.
Caution High Voltage exists within enclosure. Allow access to qualified personal
only.
CompressedAir 2.3
Compressed air is necessary to drive the pump. Maximum air pressure should be 125 psig (8.6 BAR)
the minimum is 100 psig (6.9 BAR). The air supply may be obtained from an air compressor or from
air cylinders, although it is recommended that an air compressor be used. If it is necessary to use gas
cylinders, use a technical grade of air.
Recirculating Coolant 2.4
Recirculating Coolant is required by the Pump Module for CO2pressurization. The recirculating
coolant should be maintained at a controlled temperature of 0°C.

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ASSEMBLY AND SET-UP SECTION 3
Figures 2 and 3
Front View of Spe-ed SFE 3.1

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Rear Panel of Spe-ed SFE

Note For use with optional electric CO
2
pump.
Refer to Appendix F

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CO2Outlet Port (Oven /Pump Module Connection) 3.5
Figure 6
SFE-2, SFE-4:
Connect the 1/16”OD high pressure
tubing from the rear of the oven
module to the CO2outlet port on
the pump module. Tighten fitting
with a 5/16” wrench.
SFE-NP:
Connect the 1/8”OD high pressure
tubing from the rear of the oven
module to the CO2outlet port on
the pump module. Tighten fitting
with a 7/16” wrench.
CO2Safety Head Outlet 3.6
The safety head (shown in Figure 6) on the rear panel of the pump module, contains a rupture disc
that will burst if the CO2outlet pressure exceeds 12,500 psi (862 BAR). In the event of a ruptured
disc, the CO2will vent from the safety head outlet until the pressure in the system is relieved.
Note This outlet has a 3/8” female NPT pipe thread fitting. This fitting allows the user to
vent, if desired, the discharging gas to a housing ventilation system.
Note In the event of a burst rupture disc, a new disc must be installed to seal the port. The
system cannot be pressurized unless a new rupture disc has been installed. (Please see the
“Accessories” section of this manual.)

Note For use with optional electric CO
2
pump. Refer to Appendix F

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Connecting the Flow meter 3.8
The flow meter is attached to the right side of the oven module. It is calibrated for gaseous CO2.
Instructions for using the flow meter for SPE collection and for solvent collection follow.
For SPE Collection
Slide the 6mL SPE cartridge onto the cartridge adaptor (interfaced to the C&C Module) and connect
the tubing adaptor to the 6mL cartridge. Affix a length of tygon tubing to the ends of both the tubing
adaptor and to the flow meter (Figure 7). The micro-adjustment valve at the outlet of the flow meter
should be full open. If the balls in the flow meter oscillate during use, slightly close the valve until
the oscillations stop.

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For Solvent Collection
Perforate the septum on the collection vial with the collector vessel vent. Affix the tubing adaptor to
the flow meter (Figure 8).
Note If a solvent is used in the collection vial, the vial must be positioned so that the
solvent level is below the tip of the vent needle.

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EXTRACTOR VESSEL PACKING SECTION 4
Packing the Extractor Vessel 4.1
1. Choose an appropriate sized vessel rated at the pressure
required for your application.
Note The following instructions describe the use of the
analytical scale extraction vessels available from Applied
Separations. Vessels obtained from other suppliers may
vary slightly in design.
2. Remove one of the end-fittings and push a plug of glass
or polypropylene wool or a polypropylene frit (P/N 7956) to
the closed end of the vessel with a tamping rod.
Caution In the end-fittings of the extractor
vessels are metal frits that hold the sample in
place and prevent particulate matter from
entering the fluid transfer lines. Since the frits
can be easily clogged by the sample matrix, it is
important to place some kind of coarse
filtration material such as polypropylene wool
in the vessel to protect the frits from fine
particulate matter. The metal frits are available
in pore sizes from 2 - 20 microns.
3. Fill the vessel with the sample and tamp the bed. (See the
“Accessories” section of this manual for tamping rods.) Be
sure to pack the sample bed firmly to ensure that the
supercritical fluid diffuses uniformly through the sample
matrix.
4. Add a second plug of polypropylene wool or a frit to the top of the sample bed (Figure 9). If a
large void remains, fill the additional space in the vessel with Spe-ed Matrix (P/N 7950).
5. Add a final plug of polypropylene wool or a frit and tighten the end-fitting.
6. Set the vessel aside or refrigerate until ready to perform the extraction. (See Section 5.3 for details
on mounting the vessel in the oven.)
Warning Make sure that the Seals are properly installed and the end caps are
properly tightened.

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Note For many samples, packing the tube in this manner would result in a sample bed that
would not permit even diffusion of the supercritical fluid. In such instances, some materials must be
used to disperse the original sample. Among the materials which have been used are glass and metal
beads, sand, silica gel, sodium sulfate, and Spe-ed Matrix (P/N 7950).
Note Extraction vessels usually have recessed seals at each end. During cleaning of the
vessels after the extraction, the seal may become dislodged. The vessel will not fully pressurize
unless the seal is replaced in the vessel.