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Applied Separations Spe-ed SFE-Basic Operation Manual

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S p e - e d S F E - B a s i c
Op e r a t i o n s Ma n u a l
V e r s i o n 1 . 0
R e a d Op e r a t i o n s Ma n u a l f o r I n s t r u c t i o n s
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9 3 0 H a mi l t o n S t .
A l l e n t o w n , P A 1 8 1 0 1
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  • Page 1 S p e - e d S F E - B a s i c Op e r a t i o n s Ma n u a l V e r s i o n 1 . 0 R e a d Op e r a t i o n s Ma n u a l f o r I n s t r u c t i o n s B E F OR E S e t t i n g U p o r R u n n i n g S y s t e m 9 3 0 H a mi l t o n S t .
  • Page 2 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.

  • Page 3: Table Of Contents

    TABLE OF CONTENTS INTRODUCTION Section 1 Purpose of Spe-ed™ SFE Basic Specifications Site Preparations Pre-Installation Overview of Features REQUIRED UTILITIES Section 2 Liquid Carbon Dioxide Electricity Compressed Air Recirculating Coolant ASSEMBLY AND SET-UP Section 3 Front/Rear Views Attaching the Liquid CO Tank Power Compressed Air...
  • Page 4 OPTIONS Section 6 Spe-ed™ SFE Basic Modifier Pump Module MAINTENANCE Section 7 Cleaning Preventive Maintenance TROUBLESHOOTING Section 8 Emergency Operating Procedures ACCESSORIES Section 9 APPENDIX A Example Applications...

  • Page 5: Introduction

    INTRODUCTION Section 1 Warranty This manual provides basic information for the user to install and operate the Spe-ed™ SFE Basic, 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.

  • Page 6: Purpose Of Spe-Ed™ Sfe Basic

    Spe-ed Purpose of the ™ SFE Basic The Spe-ed™ SFE Basic allows an analyst to perform supercritical fluid extractions simply and efficiently. Developed in conjunction with the USDA, the Spe-ed™ SFE Basic has achieved simple sophistication in design and use. With its flexibility of both dynamic (continuous flow) and static (where supercritical CO is pressurized in a sealed extraction vessel for a specific period of time) modes, the Spe-ed™...

  • Page 7: Site Preparations

    Caution The Spe-ed™ SFE Basic was designed to use CO or CO containing 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.

  • Page 8: Pre-Installation

    6mL SPE discharge fitting (2), P/N 7712 • Discharge tube for collection of solvents (1), P/N 7713 • Samples of Applied Separations Spe-ed™ SPE 1g/6mL cartridges (1 box), P/N 7965 • Sample of polypropylene wool, P/N 7952 • Polypropylene frits, P/N 7956 •...

  • Page 9: Overview Of Features

    Overview or Features The Spe-ed™ SFE Basic is capable of pressures up to 10,000 psig and oven temperature up to 240° C. Within this range of pressures and temperatures the analyst can accomplish a wide range of extractions. Several unique features are incorporated into the Spe-ed™ SFE Basic that overcome many of the problems researchers currently encounter with other designs.

  • Page 10: Required Utilities

    REQUIRED UTILITIES SECTION 2 Liquid Carbon Dioxide (CO Most analyses will require Instrument grade CO or CO passed through a CO clean-up column. (See the “Accessories” section of this manual.) A dip/eductor tube will be required in the CO cylinder. Caution The CO cylinder must contain a dip/eductor tube to ensure that...

  • Page 11: Assembly And Set-Up

    ASSEMBLY AND SET-UP SECTION 3 Spe-ed Front View of the ™ SFE Basic Figure 1...
  • Page 12 Spe-ed Rear View of the ™ SFE Basic Figure 2...

  • Page 13: Power

    Cylinder to the Spe-ed ™ SFE Basic Connecting the CO Attach the flex hose with a CGA fitting (P/N 7118) from the CO2 cylinder to the CO2 inlet port on rear panel (Figure 3). Tighten the nut on the rear panel connection with a 9/16”...

  • Page 14: Compressed Air

    Compressed Air Connect 1/4”OD nylon tubing (P/N 7115) from the compressed air source (compressed air cylinder or house air supply) to the air filter on the back of the unit (Figure 4). Press the tubing into the fitting port firmly until secure.

  • Page 15: Connecting Recirculating Coolant

    Connecting Recirculating Coolant Set-up and Use 1. Attach the flexible tubing fluid lines to the inlet and outlet adaptors on the rear of the SFE Basic (Figure 6) to the Spe-ed™ RCB Refrigerated Circulating Bath (P/N 7025, 120VAC or P/N 7027, 240VAC). 2.

  • Page 16: Connecting The Flow Meter

    Connecting the Flow meter The flow meter is attached to the right side of the unit. It is calibrated for gaseous CO 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 located on the Flow Control Module and connect the tubing adaptor to the 6mL cartridge.

  • Page 17: Extractor Vessel Packing

    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.
  • Page 18 Warning Make sure that the Seals or O-Rings/Backup Rings are properly installed and the end caps are properly tightened. 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.

  • Page 19: In-Line Analyte Trapping

    Packing the Extraction Vessel for In-line Analyte Trapping Below is a procedure for packing an extractor vessel with SPE columns (in a Teflon sleeve) to perform in-line SFE applications. 1. Attach the top end cap to the vessel and 2. Carefully tighten.

  • Page 20: Vessel Packing Example

    8. Attach the bottom end cap to the extractor vessel and tighten (Figure 14). 9. Set the vessel aside or refrigerate until ready to perform the extraction. Caution At the ends of the extractor vessels are metal frits that hold the sample in place and prevent particulate matter from entering the fluid transfer lines.
  • Page 21 NOTE Figure 15 shows a sample matrix compressed with a tamping rod. NOTE Figure 16 depicts the vessel from Figure 15 mounted on the SFE Basic using an upward vertical flow of supercritical fluid. Observe that the end marked “TOP” (Figure 15) during the packing process was at the bottom;...

  • Page 22: System Operations

    SYSTEM OPERATIONS SECTION 5 Inlet, Outlet, Vent, Micro-metering, and Fluid Delivery Valves Outlet Valve The outlet valve is a shut-off valve that supplies supercritical CO from the extraction vessel to the metering valve on the Flow Control Module. Turn the handle clockwise to close and counter-clockwise to open (Figure 17).
  • Page 23 Vent Valve The vent valve is a shut-off valve that is used to vent the supercritical CO from the extractor vessel to the atmosphere. Turn the handle clockwise to close and counter-clockwise to open (Figure 18). Note The vent valves must be closed to perform an extraction.
  • Page 24 Caution Do not over tighten the micro-metering valve below the zero setting when reducing flow. Over-tightening may score the valve seat and result in erratic flow control. Outlet valve should be used to shut off the flow. Note Before opening the outlet valve during the extraction process, the micro-metering valve should be preset at a minimum flow rate of approx.

  • Page 25: Operating The Spe-Ed™ Sfe Basic

    Spe-ed Operating the ™ SFE Basic The Spe-ed™ SFE Basic is easy to operate. Mastering the controls requires little training. In this section, a basic procedure for conducting SFE experiments is outlined. The steps below are only generalizations since each user’s requirements will vary depending on the experiment.
  • Page 26 Figure 20 – Vessel inlet Figure 21 – Vessel outlet Caution Firm pressure is only needed when tightening the compression nut and only mild pressure is needed for tightening the locking cap. Strong force can crack the black sealing ferrule which can cause CO leakage.
  • Page 27 Caution Make sure that the “air pressure regulator” is closed before introducing the to the system or the pump module could over-pressurize. Turn the “air pressure regulator” knob fully counter-clockwise to close. 5. Open the inlet valve and begin to pressurize the system to half the desired operating pressure by slowly turning the knob labeled “air pressure regulator”...
  • Page 28 Collecting with SPE Mount a Spe-ed™ SPE cartridge to the FC module by sliding it onto the SPE adaptor (P/N 7712). This will collect the off-line extract. Connect the Spe-ed™ SPE cartridge to the flow meter. (Refer to Section 3.8) Collecting “Neat”...
  • Page 29 Pressurization of the SFE Plumbing System 5.21 11. Ensure that the micro-metering valves are nearly closed (but not completely). (Refer to the discussion on micro-metering valves in Section 5.31.) Caution Make sure that the “air pressure regulator” is closed before introducing the CO to the system or the pump module could over-pressurize.

  • Page 30: Depressurizing The Spe-Ed™ Sfe Via Vent Valves

    14. Adjust the micro-metering valve to the desired flow rate by observing the flow meter. Continue the flow of CO until the desired number of liters of expanded gas has been recorded. As the extraction continues it is normal for the pressure to decrease slightly when the pump strokes.

  • Page 31: Flushing The Transfer Lines

    Flushing the Transfer Lines 5.23 for Residual Analyte Recovery 19. Ensure that both the valve is closed, and fully open both outlet and micro-metering valves. This will allow for efficient passage of solvent and analyte off-line recoveries. 20. Attach the SFE Purge Adaptors (P/N 7710) to the slip-free connectors of the extractor discharge line.
  • Page 32 OPTIONS SECTION 6 Spe-ed ™ SFE Modifier Pump Module The Spe-ed™ SFE Modifier Pump Module (P/N 7170, 120VAC or P/N 7172, 240VAC) is a special pump design that is capable of going to 10,000 psi (690 BAR). ™ ™ Connecting the Spe-ed SFE Modifier Pump to the Spe-ed SFE Basic 1.
  • Page 33 MAINTENANCE SECTION 7 Cleaning It is recommended that the transfer lines from the outlet valve to the micro-metering valve be flushed with an appropriate solvent after each run to remove any extracted material remaining in the tubing. This procedure prevents any sample carry-over and ensures quantitative collection of all extracted material.
  • Page 34 4. CO output flow rate is too high during and micro-metering valve. extraction. 5. Pump check valves may 5. Call Applied Separations be defective. (Ex. erratic Engineering Services pressure readings on Office. Major fittings may pressure gauge.) need to be replaced.
  • Page 35 Symptom Cause Remedy Desired CO pressure 1. Fluid level or head 1. Replace CO cylinder. cannot be attained. pressure in CO cylinder may be too low. 2. CO output flow rate too 2. Reduce flow rate via FC high. valves. 3.
  • Page 36 Symptom Cause Remedy Lack of Adjustment 1. Valve stem may be 1. Remove micro-metering capability or erratic flow on damaged or worn. valve stem; if severely micro metering valves (FC scored, replace module) 2. Extraction vessel is 2. Fill extraction vessel. empty.
  • Page 37 Symptom Cause Remedy Vessel heater does not heat. 1. MAIN power switch 1. Turn MAIN power on. is off. 2. Turn HEATER switch 2. HEATER switch is off. 3. Contact Applied 3. Defective thermocouple. Separations Engineering Services Office. No flow through extractor 1.
  • Page 38 ACCESSORIES SECTION 9 Catalog Number Part Name 7132 Flexible Hose Assembly w/fittings to connect from CO cylinder to pump 7115 Air Line nylon tubing and connector 7740 Slip-free connectors (2) with 10” tubing 7741 Vespel sealing ferrules (2) for slip-free connectors 7750 Wrench set* (includes: 5/16”, 1/2”, 9/16”, 5/8”) 7130...
  • Page 39 7921 In-line 1mL SPE cartridge holder (Teflon) for 1” OD extractor vessel (made to fit) 7923 In-line 3mL SPE cartridge holder (Teflon) for 1” OD extractor vessel (made to fit) 7930 Tamping rod for 1” OD extractor vessel (fits 24, 32, 50mL vessels) 7944 SFE filling funnel, fits 1”...
  • Page 40 20% to increase porosity or to bind water. (See Method 3560, 7.3 Sample Handlings) Analyte: TRPHs ™ Instrument: Applied Separations Spe-ed SFE Basic SFE: Use supercritical CO Pressure: 5000 psig Oven Temperature: 80°...
  • Page 41 Determination of Fat (%) in Potato Chips Sample Matrix: Potato chips Sample Preparation: Grind sample with a mortar and pestle and fill a tared extractor vessel with sample. ™ Instrument: Applied Separations Spe-ed SFE Basic SFE: Use supercritical CO Pressure: 10,000 psi Oven Temperature: 80°...
  • Page 42 Should the system become defective due to faulty parts or workmanship within the guarantee period, it will be repaired at no charge to the customer. Applied Separations will at its option send a representative to repair the system or have the customer remove the defective component and return it to Applied Separations for repair.

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