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Applied Separations Spe-ed SFE-2 Operation Manual

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Summary of Contents for Applied Separations Spe-ed SFE-2

  • 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

    Fluid Delivery Valves Operating the Spe-ed SFE 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 Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 4 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 www.appliedseparations.com...

  • Page 5: Introduction Section

    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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 6: Purpose Of Spe-Ed™ Sfe

    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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 7: Site Preparations

    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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 8 Cylinder Safety Requirement Provisions should be made for clamping the CO cylinder to either a permanent table edge or wall by using the appropriate cylinder bracket. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 9: Pre-Installation

    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 (610) 770-0900. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 11: Required Utilities Section

    Recirculating Coolant Recirculating Coolant is required by the Pump Module for CO pressurization. The recirculating coolant should be maintained at a controlled temperature of 0°C. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 12 ASSEMBLY AND SET-UP SECTION 3 Figures 2 and 3 Front View of Spe-ed SFE Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 13 Rear Panel of Spe-ed SFE Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 14 No t e F o r u s e w i t h o p t i o n a l e l e c t r i c C O p u m p . R e f e r t o A p p e n d i x F...

  • Page 15: Co 2 Safety Head Outlet

    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.) Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 16 No t e F o r u s e w i t h o p t i o n a l e l e c t r i c C O p u m p . R e f e r t o A p p e n d i x F...

  • Page 17: Connecting 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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 18 (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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 19: Extractor Vessel Packing Section

    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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 20 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. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 21: In-Line Analyte Trapping

    Spe-ed Matrix and polypropylene wool or a frit and tamp them into place (Figure 13). 7. Clean the extractor vessel to prevent any leakage and replace the seal. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 22: Vessel Packing Example

    5. Push a third polypropylene wool plug or a frit into the vessel and press it firmly against the Spe-ed Matrix. Lastly, place a seal in the vessel and screw the bottom vessel end cap onto the vessel. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 23 15) during the packing process was at the bottom; for mounting in the oven, the vessel is inverted and the end marked “TOP” is now at the top. (Refer to appendix C for other flow configurations.) Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 24: System Operations

    SP (set point) on each temperature control block and enter the temperature using the displayed keypad and select ENTER. 4. Press the Oven and Valve Heater AC switches ON to begin the heating process. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 25: Inlet, Outlet, Vent, Micro-Metering

    Note The vent valves must be closed to perform an extraction. Note Vent valves need only moderate force to effectively shut off the flow. Excessive force on the handles is neither recommended nor desirable. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 26 The fluid delivery valve is a shut-off valve on the flexible hose that allows the liquid CO to enter the pump module and start pressurizing the system (Figure 18e). Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 27: Operating The Spe-Ed Sfe

    4. Begin heating the C&C module by pushing the VALVE switch to “on.” 5. Mount the off-line collection device. Three types of collection procedures can be utilized: SPE, “neat” and solvent. Each procedure is outlined. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 28 Pierce the septum a second time with the extracted material can be forced into collector vessel vent (P/N 7731) and the flowmeter causing flowmeter connect to the flow meter (Figure 20). damage. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 29 (Figure 21). Ensure that the vessel is positioned with the sample end on top. (Refer to Figures 15 and 16.) Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 30 CO leakage. The locking cap will ensure that the tubing is perfectly seated and will prevent slipping or leaking at supercritical CO pressures. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...

  • Page 31: Pressurization Of The Sfe Plumbing System 5.31

    8. Place the tip of the extractor vessel thermocouple between the top of the extractor vessel and the extractor vessel bracket. It will provide the vessel skin temperature which can vary from oven temperature setting (Figure 21). The extraction vessel temperature is displayed as Vessel Temp on the oven touchscreen.
  • Page 32 9. Ensure that both outlet and vent valves are closed. (Refer to Figure 18a, b and c.) 10. 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 “PUMP”...
  • Page 34 Note The Spe-ed SFE has been equipped with four (4) independent safety systems. Audible Alarm - An audible alarm will sound if the 10,000 psi (690 BAR) limit is exceeded. Warning Light - A warning light will give a visual indication that the pressure in the system has exceeded the safety limits.

  • Page 35: Depressurizing The Sfe Via Vent Valves

    Depressurizing the SFE via Vent Valves 5.32 after an Off-line Collection Only 20. Press the PUMP switch once to disable the Pump. The “ON” LED will go OFF to show the CO pump is disabled. Then set the pump pressure setpoint to 0 on the touchscreen controller. 21.

  • Page 36: Flushing The Transfer Lines

    Flushing the Transfer Lines 5.33 for Residual Analyte Recovery 25. Ensure that both vent valves are closed, and fully open both outlet micro-metering valves. This will allow for efficient passage of solvent and analyte off-line recoveries. 26. Attach the SFE Purge Adaptors (P/N 7710) to the oven’s slip-free connectors of the extractor discharge line.
  • Page 37 4. Adjust the air pressure regulator ( for manual pressure control systems) or pressure controller setpoint (for automatic electronic pressure control systems) to the desired CO pressure. 5. Open the inlet valves by turning them counter-clockwise. 6. To check for leaks, pressurize the pump module halfway to the desired pressure and open the oven.
  • Page 38 SFE Oven Manifold port using the supplied ferrule and nut. For SFE-NP: Connect the free end of the 60 inch long tube assembly to the factory-installed SFE-NP Oven Modifier Inlet Tube Assembly using the supplied ferrules and nut. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 39 Figure 26 Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 40 Replacement of Adsorbents in CO Clean-up Cartridge Replace CO clean-up column adsorbent Spe-ed CO Clean (adsorbent P/N 7121) quarterly or as needed, depending on the purity of the CO used. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 41 3. Air leak in pump module. 3. Open pump module cabinet and slowly raise air pressure. Check for tubing leaks. Tighten loose fittings and/or replace fittings or tubing. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 42 3. Blockage in 1/16” tubing 3. First attempt to clean line between outlet valve and with solvent. If it remains C&C module. clogged, open C&C valves before replacing tube. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 43 1. Tighten stem nuts. leaking. 2. Inlet, outlet, or vent valve 2. Tighten inlet, outlet, fittings are loose. and/or vent fittings. 3. Stem packing may be 3. Replace stem packing. worn. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 44 Slip-free connectors leaking 1. Cracked or worn vespel 1. Replace vespel ferrule. ferrule. 2. Replace entire slip-free 2. Damaged slip-free fitting. connector to 3-way valve. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 45 If unsuccessful, replace. 3. Stainless steel frit clogs frequently. 3. Sample extracted material may require larger frit or vessel sample may need a more efficient packing procedure. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 46 32mL extractor vessel (finger tight) 7976 50mL extraction vessel (finger tight) 7907 300mL extraction vessel (finger tight) 7926 500mL extraction vessel (finger tight) 7908 1000mL extractor vessel (finger tight) Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 47 Collection tube vent assembly 7735 Collection tube (16 x 125) with cap and septum (250/box) Clean-up Accessories 7120 clean-up columns 7121 Spe-ed CO Clean (100g) - Replacement adsorbent for CO cleanup columns Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 48 To check the calibration: 1.With the system depressurized, verify that the display indicates 0 +/-15 psi(0+/-1 BAR) 2. If the display indicates a value outside the above range, contact Applied Separations Engineering Services Office for calibration assistance. Applied Separations · 930 Hamilton Street · Allentown, PA 18101...
  • Page 49 This condition will remain providing there are no work load changes in the SFE oven. To compensate for this droop in temperature, the SFE oven must be reset either manually or automatically (integrally). Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 50 2. Do not change more than one parameter at a time. Allow the system to reach equilibrium before making another change. 3. Remember that the amount of time spent tuning the SFE oven is relative to the precision of control needed. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 51 (droop) from the set point occurs. At this point in tuning the system, the process variable should be in a state of equilibrium, but not right on the desired set point. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 52 Since each SFE oven has its own oven cycle time, the auto reset time constant (repeats/minute) must be tuned to match the overall SFE oven response time. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 53 For additional information on resetting the heating parameters of the Spe-ed SFE, contact the Applied Separations Engineering Offices at (610) 770-0900. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 54 Your Spe-ed SFE was factory assembled for extractors using this arrangement. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 55 Figure B. This arrangement is possible with the versatile Spe-ed SFE. The only change required to the instrument is the replacement of the factory installed slip-free connectors and tubing with longer lengths. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 56 1g C18 SFE cartridge or 3mL Tetrachloroethylene Analytical Method: GC/FID or IR (EPA method 8015 or 8440) Note This method is not suitable for the extraction of low-boiling TPHs such as gasoline. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 57 Cool 20 minutes. The difference in weight is calculated as weight percent fat. Direct Method: Weigh tared collection tube before extraction. Collect fat in tared collection tube and reweigh collection tube after extraction. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 58 APPENDIX E Finger Tight Extractor Vessel Information Applied Separations’ vessels have standard 1/16” female end-fittings for easy use with finger tight vessel connectors. No wrenches are needed. Warning After use, the vessels should remain sealed until they have cooled to room temperature (20 - 30°...
  • Page 59 5. Put the plunger into the end of the insertion tool body and press smoothly until the plunger meets the body. 6. Unscrew the insertion tool body from the vessel tube. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 60 Recirculating Coolant Bath (RCB). Note The Electric CO Pump Pressure display reads in units of PSI, up to 9,999 PSI. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com www.appliedseparations.com...
  • Page 61 Outlet Check Valve on right side of the pump cabinet. Refer to Figure 3 on page 13 of Spe-ed SFE Operations Manual for location of oven tube. Pump CO Outlet Check Valve Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 62 Connect the tubing from the RCB coolant inlet to the electric pump’s coolant outlet on left side of pump cabinet. Pump Coolant Outlet Operation Refer to the included electric CO pump user manual for operation and programming details. Applied Separations · 930 Hamilton Street · Allentown, PA 18101 www.appliedseparations.com...
  • Page 63 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.

This manual is also suitable for:

Spe-ed sfe-4Spe-ed sfe-np

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