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Dionex ASE 100 Operator's Manual

Accelerated solvent extractor
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ASE 100
ACCELERATED SOLVENT EXTRACTOR
OPERATOR'S MANUAL
© 2002 Dionex Corporation
Document No. 031842
Revision 01
May 2002

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Summary of Contents for Dionex ASE 100

  • Page 1 ® ASE 100 ACCELERATED SOLVENT EXTRACTOR OPERATOR'S MANUAL © 2002 Dionex Corporation Document No. 031842 Revision 01 May 2002...
  • Page 2 Dionex Corporation, 1228 Titan Way, Sunnyvale, California 94088-3603 U.S.A.

  • Page 3: Table Of Contents

    Contents 1 • Introduction Overview ..........1-1 About This Manual .
  • Page 4 ASE 100 Accelerated Solvent Extractor 3 • Operation and Maintenance Preparing to Run an Extraction ......3-1 3.1.1...
  • Page 5 Contents 4 • Troubleshooting Error Messages ......... . .4-1 Liquid Leaks .
  • Page 6 ASE 100 Accelerated Solvent Extractor Replacing the Static Valve ....... . . 5-18 Replacing the Source Needle .
  • Page 7 Contents B.2.6 Rinsing the System ....... . B-11 B.2.7 Adjusting the Cell Holder ......B-13 B.2.8 Inspecting the Cell.
  • Page 8 ASE 100 Accelerated Solvent Extractor Doc. 031842-01 5/02...

  • Page 9: Introduction

    100 Accelerated Solvent Extractor is a system for extracting either organic or inorganic compounds from a variety of solid and/or semisolid samples. The ASE 100 accelerates the traditional extraction process by using solvent at elevated temperatures and pressures. Pressure is applied to the sample extraction cell to maintain the heated solvent in a liquid state during the extraction.
  • Page 10 12 collection bottles. Ordering Extraction Cells in Other Sizes The ASE 100 accommodates four extraction cell sizes (10 mL, 34 mL, 66 mL, or 100 mL). To perform an extraction with a cell in any size other than the size included with your system, order the appropriate cells from Dionex.

  • Page 11: About This Manual

    Solvent Extractor. Explains the meaning of safety messages and icons in the manual and safety labels on the instrument. Chapter 2 Describes the physical aspects of the ASE 100: the front Description panel controls, rear panel connections, electronics, and mechanical components. Briefly describes the extraction process.

  • Page 12: Typefaces

    ASE 100 Operator’s Manual 1.2.1 Typefaces Uppercase bold type indicates an ASE 100 front panel button, the name of a screen, or an on-screen entry. For example: Press to start the rinse cycle. RINSE screen has four options. MAIN Move the cursor to the field.
  • Page 13 1 • Introduction Messages d’avertissement en français Signale une situation de danger immédiat qui, si elle n'est pas évitée, entraînera des blessures graves à mortelles. Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures graves à mortelles. Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures mineures à...

  • Page 14: Safety Labels

    ASE 100 Operator’s Manual Safety Labels The TUV GS, C, US Mark safety label and the CE Mark label on the ASE 100 indicate that the ASE 100 is in compliance with the following standards: EN 61010-1:1993 (safety), CAN/CSA-C22.2 No. 1010.1-92 (safety), UL 3101- 1/10.93 (safety), EN 50082-1:1992 (susceptibility), and EN 55011:1991...

  • Page 15: Description

    Section 2.4 describes method control of the ASE 100. Section 2.5 lists the operating parameters for preprogrammed methods. Operating Features Figure 2-1 illustrates the main operating features of the ASE 100. Figure 2-1. ASE 100 Key Operating Features Doc. 031842-01 5/02...
  • Page 16 Solvent Bottle A 1-liter or 2-liter solvent bottle is installed in a recess on top of the ASE 100. The recess contains a plastic liner to contain any solvent leaks or spills that may occur. Waste Bottle The waste bottle is a 250 mL collection bottle that is sealed with a special cap assembly.

  • Page 17: Control Panel Screen

    Control Panel Screen The control panel screen displays status and operating information for the ASE 100. Use the screen, in conjunction with the control panel keypad (see Section 2.1.2), to control ASE 100 operation. You can edit any field on the screen that contains a blinking cursor. A field without a blinking cursor is for display only.

  • Page 18: Control Panel Keypad

    , the up arrow, and the MENU ENTER down arrow) are used in conjunction with the ASE 100 display to access less frequently used functions. The action of the navigation keys depends on whether the cursor is in normal mode or editing mode: In normal mode, the cursor does not blink and looks like this.
  • Page 19 2 • Description Button Function Normal mode: Exits the screen currently displayed and returns to the screen one level up in the hierarchy. For example, if the screen is displayed, METHOD EDITOR pressing returns you to the screen. See MENU MAIN Figure C-1 for an overview of the screens.

  • Page 20: Extraction Cells And Rinse Cells

    Extraction Cells ASE 100 extraction cells are available in four sizes: 10 mL, 34 mL, 66 mL, and 100 mL. Interchangeable end caps screw onto each end of the cell body.

  • Page 21: Collection Bottle

    2 • Description Rinse Cells During a rinse cycle, solvent passes directly through the blue rinse cell and into the collection bottle. For more information about rinse cycles, see Section 3.1.7 and Section B.2.6. The rinse cell size (short, medium, or long) must be matched to the size of the extraction cell, as indicated in the table below.

  • Page 22: Solvent Bottle

    ASE 100 Operator’s Manual 2.1.5 Solvent Bottle The ASE 100 Ship Kit (P/N 059397) includes a 2-liter glass bottle with shatterproof plastic coating (P/N 045901) and a bottle cap assembly (P/N 051977) with tubing and fittings for the inlet and outlet connections.

  • Page 23: Waste Bottle

    For VENT installation instructions, see Section B.2.1. The model data label lists fuse and power information, as well as the ASE 100 serial number. You will be asked to provide the serial number when ordering replacement parts for the system.
  • Page 24 ASE 100 Operator’s Manual Figure 2-4. ASE 100 Rear Panel 2-10 Doc. 031842-01 5/02...

  • Page 25: Extraction Process

    Place the extraction cell in the cell holder and close the cell door. Press START to begin the run. From this point, the ASE 100 automatically performs the extraction process. An extraction consists of six main steps: Filling the cell with solvent Heating the cell (equilibration)
  • Page 26 ASE 100 Operator’s Manual You can monitor the progress of an extraction on the screen (a STATUS MAIN screen option). Operating parameters are updated in real time. Figure 2-5 illustrates a typical screen. Table 2-1 describes the screen parameters. STATUS Figure 2-5.

  • Page 27: Method Control

    A method defines all of the timed events that occur during a sample extraction (see Table 2-2). There are two types of methods: Preprogrammed methods are application-specific methods created by Dionex. These methods cannot be changed or deleted by the user. For a list of the parameters for each preprogrammed method, see Section 2.5.

  • Page 28: Preprogrammed Methods

    ASE 100 Operator’s Manual Preprogrammed Methods To enable you to quickly produce results with the ASE 100, Dionex provides nine preprogrammed methods. These methods are designated by three-letter abbreviations (see the table below). Preprogrammed Method Method Name Semivolatiles Total Fat (crude)
  • Page 29 2 • Description FAT (Total Fat) Method Parameters Solvent Hexane/Acetone (4:1) Temperature 125 °C Static Time 5 min Flush Volume 100% Purge Time 60 sec Static Cycle HRB (Chlorinated Herbicides) Method Parameters Solvent MeCl /Acetone (1:1) with 1% Temperature 100 °C Static Time 5 min Flush Volume...
  • Page 30 ASE 100 Operator’s Manual OPP (Organophosphorous Pesticides) Method Parameters Solvent MeCl /Acetone (1:1, v/v) 100 °C Temperature Static Time 5 min Flush Volume Purge Time 100 sec Static Cycle PCB (Polychlorinated Biphenyls) Method Parameters Solvent Hexane 100 °C Temperature Static Time...
  • Page 31 2 • Description PPE (Polymer Additives) Method Parameters Solvent 2.5% Cyclohexane in Isopropyl Alcohol Temperature 140 °C Static Time 3 min Flush Volume 100% Purge Time 60 sec Static Cycle TPH (Total Petroleum Hydrocarbons) Method Parameters Solvent MeCl /Acetone (1:1, v/v) 175 °C Temperature Static Time...
  • Page 32 ASE 100 Operator’s Manual 2-18 Doc. 031842-01 5/02...

  • Page 33: Operation And Maintenance

    Do not use solvents with an autoignition point of 40 to 200 °C (104 to 392 °F). The table below is a partial list of solvents that should not be used with the ASE 100. If you have a question about solvent suitability, contact Dionex.
  • Page 34 Lösungsmittel, deren Selbstentzündungstemperatur bei 40° bis 200°C liegt. Die untenstehende Tabelle zeigt einige Lösungsmittel, die Sie nicht mit dem ASE 100 verwenden sollten. Bei Fragen zur Eignung von Lösungsmitteln wenden Sie sich bitte an Dionex. Nicht zu verwendende Selbstentzündungstemperatur Lösungsmittel Kohlendisulfid: CS 100 °C...

  • Page 35: Filling The Solvent Bottle

    3 • Operation and Maintenance 3.1.2 Filling the Solvent Bottle Use only Dionex solvent bottles (1-liter, P/N 045900; 2-liter, P/N 045901). These glass bottles with plastic, shatterproof coating. Make sure the pressure applied to the bottles does not exceed 0.07 MPa (10 psi).
  • Page 36 ASE 100 Operator’s Manual Insert the solvent outlet line extending from the underside of the bottle cap assembly into the bottle (see Figure 3-1). Make sure the in- line filter rests on the bottom of the bottle. (This prevents air from being drawn through the line.)

  • Page 37: Preparing The Sample

    If you have successfully followed a particular sample pretreatment procedure for another extraction method (Soxhlet, for example), use the same procedure with the ASE 100. If you have never run an extraction before or if you are preparing a new sample, follow the guidelines here.
  • Page 38 ASE 100 Operator’s Manual Sample Preparation Guidelines The mixtures here are recommendations; adjust the proportions as required for your extraction. If the sample appears dry, use one of these mixtures: 4 grams sample to 1 gram DE 4 grams sample to 4 grams Na...

  • Page 39: Installing The Cell Filter

    There are two types of cell filters: Cellulose filters (P/N 056780, pkg. 100) are appropriate for most extraction methods that use organic solvents. The ASE 100 Ship Kit (P/N 059397) includes a package of cellulose filters. Glass-fiber filters (P/N 056781, pkg. 100) are recommended for aqueous extractions, where cellulose may provide inadequate filtration or may interfere with the analytical technique.
  • Page 40 ASE 100 Operator’s Manual 2. Follow the steps below to install the cell filter. Insert a cellulose or glass-fiber filter into the cell at a slight angle. Position the filter insertion tool (P/N 056929) over the filter. Slowly push the insertion tool straight into the cell.

  • Page 41: Filling The Cell

    1. Carefully load the sample into the top of the extraction cell, using the funnel (P/N 056699) provided in the ASE 100 Ship Kit (P/N 059397). 2. (Optional) To reduce the amount of solvent used during the extraction, fill any void volume in the cell with an inert material such as Ottawa sand (Fisher S23-2).
  • Page 42 ASE 100 Operator’s Manual Figure 3-2. Inspecting Cell O-Rings 3-10 Doc. 031842-01 5/02...

  • Page 43: Installing The Collection Bottle

    3 • Operation and Maintenance 3.1.6 Installing the Collection Bottle 1. Toggle the needle switch on the front panel (see Figure 3-3) to the position. 2. Place a 250 mL collection bottle (P/N 056284, pkg. of 12), with the bottle cap screwed on, in the collection bottle holder (see Figure 3-3). 3.

  • Page 44: Rinsing/Priming The System

    ASE 100 Operator’s Manual 3.1.7 Rinsing/Priming the System During a rinse cycle, approximately 5 mL of solvent is pumped through the system. Run a rinse cycle at the following times: After initial setup After refilling the solvent bottle After changing solvents (rinse twice to remove all of the previous...

  • Page 45: Editing A Custom Method (1-24)

    3 • Operation and Maintenance Editing a Custom Method (1–24) If the ASE 100 preprogrammed methods (see Section 2.5) are not suitable for a particular extraction, edit one of the 24 custom methods provided with the system. All parameters in these methods are initially set to their default values. You can create a new method by editing either a custom method that still contains the default parameters or a custom method that you previously edited.
  • Page 46 ASE 100 Operator’s Manual To edit a custom method (for example, method 1): 1. Press MENU to display the screen. MAIN Figure 3-4. Main Screen 2. Move the cursor to the option and press ENTER METHOD EDITOR screen is displayed (see Figure 3-5).
  • Page 47 3 • Operation and Maintenance 3. The screen displays the parameters for the method last METHOD EDITOR selected on the screen (see Section C.1.3). If method 1 is not currently SETUP displayed, press to move the cursor to the method editing field. Use ENTER an arrow button to step through the method numbers (1 through 24).
  • Page 48 ASE 100 Operator’s Manual To save to a different method number: a. Using an arrow button, move the cursor to SAVE b. Press to move the cursor to the editing field. ENTER SAVE c. Press an arrow button to step through the method numbers (1 through 24).

  • Page 49: Guidelines For Method Development

    3 • Operation and Maintenance Guidelines for Method Development Follow the procedure below to develop a method for a new sample type. 1. Select a solvent(s) (see Section 3.1.1). 2. Prepare the sample (see Section 3.1.3). 3. Press the button to display the screen.
  • Page 50 ASE 100 Operator’s Manual 5. The screen displays the parameters for the method last METHOD EDITOR selected on the screen (see Section C.1.3). If this is not the method you SETUP want to edit, press to move the cursor to the method editing field.
  • Page 51 3 • Operation and Maintenance method to this number and to return the cursor to the left margin of the screen. 9. Run the new method three times (with the same cell and sample) and analyze the extracts. 10. If target analytes are present in extract 2 or 3, make the adjustments listed below (one at a time) to the method.

  • Page 52: Running An Extraction

    ASE 100 Operator’s Manual Running an Extraction 1. Press to display the screen. MENU MAIN Figure 3-9. Main Screen 2. Select and press ENTER SETUP This displays the screen. SETUP Figure 3-10. Setup Screen (Initial view) 3. Check that the selected method is correct. If it is not, use an arrow to move the...
  • Page 53 Replace the septum (P/N 049464, pkg. of 72) in the collection bottle cap after each extraction. Using the septum more than once may cause loss of sample and may damage the ASE 100. 8. Open the cell door and install the cell in the cell holder.
  • Page 54 ASE 100 Operator’s Manual Always install the cell in the cell holder. If you install the cell directly in the oven, the cell door will not close and the run will not start. While holding the extraction cell at a...
  • Page 55 11. If you need to start the next extraction right away, put on the thermal gloves (P/N 060372) supplied in the ASE 100 Ship Kit (P/N 059397), remove the cell from the cell holder, and place it on the cell rack (P/N 059927) to cool.

  • Page 56: Post-Extraction Procedures

    400 °C (752 °F). 3.5.2 Processing Extracts The composition of the extracts generated by the ASE 100 is very close to that generated by Soxhlet and other standard solid-liquid extraction techniques when using the same solvent. Use the same analytical method for ASE 100 extracts that you employed for extracts obtained from other techniques.

  • Page 57: Aborting A Run

    If this occurs, the ASE 100 screen will display an error message; the message will remain on-screen until you press a key to clear it or until it is replaced by another error message.

  • Page 58: Routine Maintenance

    ASE 100 Operator’s Manual Routine Maintenance This section describes routine maintenance procedures that the user can perform. All other ASE 100 maintenance procedures must be performed by qualified Dionex personnel. 3.7.1 Daily Maintenance Fill the solvent bottle, if needed. After filling the solvent bottle, always run two rinse cycles to clear the solvent lines of bubbles (see Section 3.1.7).

  • Page 59: Shutdown

    100% organic solvent or distilled water (see Section 3.1.7) before turning off the power. 2. Turn off the gas supply. Before shipping the ASE 100: 1. After extracting with acidic solvents or basic solvents, rinse the system with either 100% organic solvent (e.g., acetone or methanol) or distilled water (see Section 3.1.7).
  • Page 60 ASE 100 Operator’s Manual 3-28 Doc. 031842-01 5/02...

  • Page 61: Troubleshooting

    If an error message appears on the ASE 100 screen, refer to Section 4.1 for details.
  • Page 62 0.34 ± 0.02 MPa (50 ± 3 psi); if it SYSTEM does not, adjust the pressure regulator for the system gas to 0.34 MPa (50 psi). Action: If the error message appears again, contact Dionex for assistance. Error 003 Oven temperature low. Cause: The heater cable connection to the power supply is loose, or a heater component malfunctioned.
  • Page 63 Action: Install the collection bottle (with the bottle cap screwed on) and toggle the needle switch to the DOWN position (see Section 3.1.6). If the error message reappears, contact Dionex for assistance. Error 008 Cell not detected. Cause: No cell is installed, or the sensor failed to detect the cell.
  • Page 64 If the pump exceeds the volume limit (250 mL), there is probably a leak somewhere in the system. Action: Remove the right side panel of the ASE 100 (see Section 5.3). Inspect the following fittings for leaks (see Figure 4-1): pump fittings, pump check valves, pressure transducer fittings, relief valve fittings, static valve fittings, and solvent line fittings.
  • Page 65 Cause: A leaking fitting(s) somewhere in the system. Action: Remove the right side panel of the ASE 100 (see Section 5.3). Inspect the following fittings for leaks (see Figure 4-1): pump fittings, pump check valves, pressure transducer fittings, relief valve fittings, static valve fittings, and solvent line fittings.
  • Page 66 Oven unable to reach temperature. Cause: The heater cable connection to the power supply is loose, or there is a problem with a heater component. Action: The defective component should be replaced. Contact Dionex for assistance. Error 015 Unable to flush. Cause: The solvent bottle is empty, or is not properly installed.
  • Page 67 Insufficient pressure was applied to the cell during an extraction. Action: Remove the right side panel of the ASE 100 (see Section 5.3). Inspect the following fittings for leaks (see Figure 4-1): pump fittings, pump check valves, pressure transducer fittings, relief valve fittings, static valve fittings, and solvent line fittings.

  • Page 68: Liquid Leaks

    (see Section C.2.5). Leak in solvent flow path Remove the right side panel of the ASE 100 (see Section 5.3). Inspect the following fittings for leaks (see Figure 4-1): pump fittings, pump check valves, pressure transducer fittings, relief valve fittings, static valve fittings, and solvent line fittings.
  • Page 69 4 • Troubleshooting Figure 4-1. ASE 100 Plumbing Diagram Doc. 031842-01 5/02...

  • Page 70: Gas Leaks

    System Stops Electrical cables improperly installed Remove the right side panel of the ASE 100 (see Section 5.3). Check that all electrical cables are seated properly in their connectors on the main PCB (printed circuit board).

  • Page 71: Service

    All repairs involving the electronics must be performed by Dionex personnel. Before replacing any part in the ASE 100, refer to the troubleshooting information in Chapter 4 of this manual to isolate the cause of the problem. When ordering replacement parts, please specify the ASE 100 serial number listed on the model data label on the rear panel.

  • Page 72: Replacing The Seal In The Cell End Cap

    2. Remove the snap ring from the end cap, using the snap ring tool (P/N 056684) provided in the ASE 100 Ship Kit (P/N 059397). a. Insert the pointed ends of the tool into the two holes in the snap ring.
  • Page 73 5 • Service Figure 5-1. Extraction Cell Assembly 9. With the cap assembly upright on the workbench, install the snap ring: a. Insert the snap ring tool into the holes on the ring. b. Squeeze the tool handles to bring the ends of the ring together. c.

  • Page 74: Replacing The Cell O-Ring

    O-ring from sealing properly and may result in leaks during operation. 1. Use the small flathead screwdriver (P/N 046985) provided in the ASE 100 Ship Kit (P/N 059397) to remove worn O-rings. To do so, insert the tip of the screwdriver into the end cap and carefully pick out the O-ring.

  • Page 75: Removing The Right Side Panel

    If a collection bottle is installed, remove the bottle from the bottle holder and set it aside. 4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel. 5. Remove the lower trim panel of the ASE 100: a.
  • Page 76 ASE 100 Operator’s Manual d. Note the small round depressions on the left and right sides of the trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.
  • Page 77 4. Reinstall the waste bottle. 5. Turn on the ASE 100 main power switch. 6. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. Doc. 031842-01 5/02...

  • Page 78: Cleaning And/Or Replacing Pump Check Valves

    If a collection bottle is installed, remove the bottle from the bottle holder and set it aside. 4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel. 5. Remove the lower trim panel of the ASE 100: a.
  • Page 79 10. Disconnect the gray cable from the pump PC board (see Figure 5-6). 11. Using a 3 mm hex-screw driver (P/N 060154), remove the screws in the left and right end plates (see Figure 5-6) that secure the pump to the component panel. Figure 5-6. ASE 100 Pump Doc. 031842-01 5/02...

  • Page 80: Removing The Check Valves

    ASE 100 Operator’s Manual 5.4.2 Removing the Check Valves 1. Use a 1/2-inch open-end wrench to loosen the inlet check valve housing. Remove the housing, and then remove the check valve cartridge from the housing. 2. Turn the pump over, so that the outlet check valve is facing down.

  • Page 81: Reinstalling The Outlet Check Valve

    5 • Service 5.4.5 Reinstalling the Outlet Check Valve 1. The outlet check valve assembly housing has a 10-32 port. (This is the smaller of the two ports.) Place the outlet check valve cartridge (P/N 057346) in the outlet check valve housing so that the arrow points inward.

  • Page 82: Replacing The Piston Seal

    3. Reinstall the waste bottle. 4. Turn on the ASE 100 main power switch. 5. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. 6. Rinse the system (see Section 3.1.7) and check that the pump flow is normal.

  • Page 83: Replacing The Piston Seal

    Pull the trim panel completely off, exposing the inner front panel, and set the trim panel aside. 6. Remove the right side panel of the ASE 100: a. Using a Phillips screwdriver, remove the two screws on the inner front panel, near the needle assembly (see Figure 5-5).

  • Page 84: Reinstalling The Pump

    ASE 100 Operator’s Manual 4. If tapping the head on the bench does not remove the piston guide, use the wooden end of a cotton-tipped swab to pry the guide out of the pump head. Discard the used piston guide.

  • Page 85: Replacing The Relief Valve

    If a collection bottle is installed, remove the bottle from the bottle holder and set it aside. 4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel. 5. Remove the lower trim panel of the ASE 100: a.
  • Page 86 ASE 100 Operator’s Manual 6. Remove the right side panel of the ASE 100: a. Using a Phillips screwdriver, remove the two screws on the inner front panel, near the needle assembly (see Figure 5-5). b. Insert a screwdriver into the hole located beneath the top screw hole (see Figure 5-5).
  • Page 87 17. Reinstall the waste bottle. 18. Turn on the ASE 100 main power switch. 19. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. 5-17 Doc. 031842-01 5/02...

  • Page 88: Replacing The Static Valve

    If a collection bottle is installed, remove the bottle from the bottle holder and set it aside. 4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel. 5. Remove the lower trim panel of the ASE 100: a.
  • Page 89 5 • Service 7. The static valve is installed in the lower left corner of the component panel (see Figure 5-8). Disconnect the orange tubing from the elbow press fitting on the valve. 8. Disconnect the stainless steel line from the right side of the valve. (This line connects to the source needle.) 9.

  • Page 90: Replacing The Source Needle

    16. Reinstall the waste bottle. 17. Turn on the ASE 100 main power switch. 18. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. Replacing the Source Needle 1.
  • Page 91 Pull the trim panel completely off, exposing the inner front panel, and set the trim panel aside. 6. Remove the right side panel of the ASE 100: a. Using a Phillips screwdriver, remove the two screws on the inner front panel, near the needle assembly (see Figure 5-5).
  • Page 92 15. Reinstall the waste bottle. 16. Turn on the ASE 100 main power switch. 17. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. 5-22 Doc. 031842-01 5/02...

  • Page 93: Replacing The Solvent Outlet Line

    If a collection bottle is installed, remove the bottle from the bottle holder and set it aside. 4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel and let the system vent. 5. Turn off the ASE 100 main power switch.
  • Page 94 ASE 100 Operator’s Manual 8. Remove the right side panel of the ASE 100: a. Using a Phillips screwdriver, remove the two screws on the inner front panel, near the needle assembly (see Figure 5-5). b. Insert a screwdriver into the hole located beneath the top screw hole (see Figure 5-5).
  • Page 95 5 • Service 10. Locate the static valve in the lower left corner of the component panel (see Figure 5-11). The stainless steel solvent outlet line is connected to the top of the static valve. (The other end of the solvent outlet line is connected to the lower AutoSeal tip.) Remove the fitting that connects the solvent outlet line to the static valve.
  • Page 96 ASE 100 Operator’s Manual 11. The stainless steel solvent outlet line is connected to the lower AutoSeal tip (see Figure 5-12). From there, the solvent outlet line is routed through a vertical guide. Figure 5-12. Lower AutoSeal Tip–Solvent Outlet Line Connection 5-26 Doc.
  • Page 97 5 • Service 12. Loosen the three Phillips screws that secure the cover to the vertical guide. Slip the solvent outlet line out the left side of the cover (see Figure 5-13). Figure 5-13. Removing the Solvent Outlet Line from the Vertical Guide 5-27 Doc.
  • Page 98 ASE 100 Operator’s Manual 13. Lift the lower AutoSeal tip out of the support tube located on top of the air cylinder shaft (see Figure 5-14). 14. Note the indentation along the top edge of the support tube, where it meets the lower AutoSeal tip (see Figure 5-14).

  • Page 99: Replacing The Lower Autoseal Tip

    23. Reinstall the waste bottle. 24. Turn on the ASE 100 main power switch. 25. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. 5.10 Replacing the Lower AutoSeal Tip 1.
  • Page 100 ASE 100 Operator’s Manual 7. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing palm upwards. b. Hook the first two fingers of each hand under the top edges of the...
  • Page 101 5 • Service 9. The stainless steel solvent outlet line is connected to the lower AutoSeal tip. From there, the outlet line is routed through a vertical guide with a cover (see Figure 5-15). Figure 5-15. Lower AutoSeal Tip–Solvent Outlet Line Connection 5-31 Doc.
  • Page 102 ASE 100 Operator’s Manual 10. Loosen the three Phillips screws that secure the cover to the vertical guide. Slip the solvent outlet line out the left side of the cover (see Figure 5-16). Figure 5-16. Removing the Solvent Outlet Line from the Vertical Guide 5-32 Doc.
  • Page 103 5 • Service 11. Lift the lower AutoSeal tip out of the support tube located on top of the air cylinder shaft (see Figure 5-17). 12. Note the indentation along the top edge of the support tube, where it meets the lower AutoSeal tip (see Figure 5-17).

  • Page 104: Replacing The Main Power Fuses

    19. Reinstall the waste bottle. 20. Turn on the ASE 100 main power switch. 21. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply. 5.11 Replacing the Main Power Fuses 1.
  • Page 105 5. Reconnect the main power cord. Turn on the ASE 100 main power switch. 5-35 Doc. 031842-01 5/02...
  • Page 106 ASE 100 Operator’s Manual 5-36 Doc. 031842-01 5/02...

  • Page 107: A • Specifications

    Humidity Decibel Level 76 db (“A WEIGHING” setting) A.3 Electrical Main Power 100-120/220-240 Vac, 50/60 Hz; 6 amps; the ASE 100 main Requirements power supply adjusts automatically to the power source at the installation site Oven Power Select the oven voltage range (100-120 Vac or 220-240 Vac) via Requirements switches on the rear panel power supply;...

  • Page 108: Pneumatic

    ASE 100 Operator’s Manual A.4 Pneumatic Nitrogen 1.03 to 1.38 MPa (150 to 200 psi) A.5 Front Panel Display and Keypad Display Vacuum fluorescence display (VFD) Keypad Seven buttons for entering commands and selecting screen parameters A.6 Extraction Cells Extraction Cells Stainless steel cell bodies and end caps with seals and stainless steel frits.
  • Page 109 A • Specifications Hydrocarbon Monitors the hydrocarbon vapor level Sensor Cell Sensor When the cell door is closed, the sensor can detect whether a cell is installed in the cell holder. Doc. 031842-01 5/02...
  • Page 110 ASE 100 Operator’s Manual Doc. 031842-01 5/02...

  • Page 111: B • Installation

    The ASE 100 requires a grounded, single-phase power source of from 100 to 240 Vac and 50/60 Hz. The ASE 100 oven voltage setting is controlled by two switches on the rear panel power supply. The switch settings must match the voltage from the power source at the ASE 100 installation site.

  • Page 112: Installation Instructions

    ASE 100 Operator’s Manual B.2 Installation Instructions The ASE 100 Ship Kit (P/N 059397) should be at hand before beginning the installation procedure. The Ship Kit contains several items (tubing, fittings, solvent bottle, etc.) that are required to install the system.
  • Page 113 B • Installation Figure B-1. ASE 100 Rear Panel Doc. 031842-01 5/02...

  • Page 114: Electrical Connections

    Electrical Connections 1. Connect a modular power cord (IEC 320 C13) from the power receptacle on the ASE 100 rear panel (see Figure B-1) to a grounded, single-phase power source of 100 to 240 Vac and 50/60 Hz. SHOCK HAZARD—To avoid electrical shock, use a grounded receptacle.
  • Page 115 B • Installation 2. The settings for the two oven voltage switches on the ASE 100 rear panel (see Figure B-2) must match the voltage from the power source at the installation site. Check that both switches are set to either 110 (for voltages between 100 and 120 Vac) or 220 (for voltages between 220 and 240 Vac).

  • Page 116: Checking Pressure Readings

    ASE 100 Operator’s Manual B.2.3 Checking Pressure Readings 1. Press to display the screen. MENU MAIN 2. Select and press ENTER. DIAGNOSTICS This displays the screen (see Figure B-3). DIAGNOSTICS Figure B-3. Diagnostics Screen (Additional text shown) 3. Select and press ENTER.
  • Page 117 B • Installation 4. Compare the pressure readings on the screen with the REGULATORS values listed in the table below. If a pressure reading does not meet specification, contact Dionex. Field Function Pressure Spec 0.34 ± 0.02 MPa SYSTEM Pressure applied to the system (50 ±...

  • Page 118: Solvent Bottle Connections

    ASE 100 Operator’s Manual B.2.4 Solvent Bottle Connections se only Dionex solvent bottles (1-liter, P/N 045900; 2-liter, P/N 045901). These glass bottles with plastic, shatterproof coating. To prevent personal injury, make sure the pressure applied to the bottles does not exceed 0.07 MPa (10 psi).
  • Page 119 B • Installation Insert the solvent outlet line extending from the underside of the cap assembly (P/N 051977) into the solvent bottle (see Figure B-5). Make sure the in-line filter rests on the bottom of the bottle. (This prevents air from being drawn through the line.) Hand-tighten the red lock ring cap securely over the stopper.

  • Page 120: Waste Bottle Installation

    A built-in waste bottle cap is installed above the bottle holder on the ASE 100 front panel (see Figure B-6). 1. Lift the built-in waste bottle cap with one hand. With your other hand, tilt the waste bottle at a slight angle and position it below the bottle cap.

  • Page 121: Rinsing The System

    Adjusting the Cell Holder When the ASE 100 is shipped from the factory, the cell holder (on the inside of the cell door) is positioned to accommodate either a 100 mL extraction cell or a long rinse cell (see Figure B-9).
  • Page 122 If you need to start the next extraction right away, put on the thermal gloves (P/N 060372) supplied in the ASE 100 Ship Kit (P/N 059397), remove the cell from the cell holder, and place it on the cell rack (P/N 059927) to cool.

  • Page 123: Adjusting The Cell Holder

    B.2.7 Adjusting the Cell Holder When the ASE 100 is shipped from the factory, the cell holder is positioned to hold a 100 mL extraction cell (or a long rinse cell). To accommodate a cell of any other size, move the lower latch of the cell holder to the appropriate mounting site on the cell door (see Figure B-9).
  • Page 124 ASE 100 Operator’s Manual 4. Position the latch in the new location on the cell door and install the hex screws. Figure B-9. Mounting Sites for the Cell Holder Lower Latch B-14 Doc. 031842-01 5/02...

  • Page 125: Inspecting The Cell

    B • Installation B.2.8 Inspecting the Cell O-rings are installed in the exterior ends of each extraction cell end cap, as well as in the ends of the rinse cell. Before each run, inspect the O- rings (see Figure B-10). If an O-ring is dislodged: Press it into place, using the O-ring insertion tool (P/N 049660).

  • Page 126: Completing The Installation

    Figure B-12). Figure B-12. Setup Screen (Initial view) Use the screen to specify the default settings for various ASE 100 SETUP parameters. These include the unit of measure for on-screen pressure displays, for how long the relief valve is open, the duration of the preheat period, and whether a beep is emitted when a front panel keypad button is pushed.
  • Page 127 C • User Interface This appendix describes all of the screens that can be displayed on the ASE 100 front panel (see Figure C-1). There are two functional categories for screens: operational and diagnostic. Operational screens let you select certain default parameters for the ASE 100, run the methods that control an extraction, and create and edit custom methods.

  • Page 128: Operational Screens

    C.1 Operational Screens C.1.1 Main Screen screen is a “menu” that provides top-level access to the most MAIN frequently used ASE 100 screens. To display the screen, press the MAIN button on the front panel. MENU Figure C-2. Main Screen...

  • Page 129: Status Screen

    C • User Interface C.1.2 Status Screen Use the screen to monitor the progress of a method run. The STATUS screen is updated three times per second. You cannot edit any information on this screen. Figure C-3. Status Screen Parameter Description STATUS The method step in progress, if any, or the current...

  • Page 130: Setup Screen

    C.1.3 Setup Screen Use the screen to specify which method to run, the extraction cell SETUP size, and certain ASE 100 default parameters. Figure C-4. Setup Screen (Initial view) Parameter Description METHOD Specifies the name or number of the method to run.
  • Page 131 C • User Interface Figure C-5. Setup Screen (Second view) Parameter Description PREHEAT TIME Specifies for how long the oven heats up without solvent (0 to 99 minutes). PREHEAT Enables and disables purging of the cell (without PURGE solvent) during the preheat period. BYPASS HEAT- Specifies whether to bypass the heat-up period for the extraction cell.
  • Page 132 ASE 100 Operator’s Manual Figure C-6. Setup Screen (Third view) Parameter Description KEY SOUND Determines whether a beep is emitted when a keypad button is pushed. ERROR SOUND Determines whether a beep is emitted when an error occurs (for example, you press the wrong keypad button).

  • Page 133: Method Editor Screen

    PURGE TIME Amount of time the cell is purged with nitrogen (0 to 900 seconds). Dionex recommends the following settings: 40 to 80 seconds for a 10 mL cell, 70 to 110 seconds for a 34 mL cell, 160 to 200 seconds for a 66 mL cell, and 250 to 290 seconds for a 100 mL cell.
  • Page 134 ASE 100 Operator’s Manual Parameter Description SAVE Method number that the selected parameters will be saved to (1 through 24). Doc. 031842-01 5/02...

  • Page 135: Diagnostic Screens

    C.2 Diagnostic Screens C.2.1 Diagnostics Screen screen is a “menu” that provides top-level access to DIAGNOSTICS ASE 100 screens with diagnostic functions (see Figure C-8). Figure C-8. Diagnostics Screen (Additional text shown) To display the DIAGNOSTICS screen: 1. Press the...

  • Page 136: Sensors Screen

    ASE 100 Operator’s Manual C.2.2 Sensors Screen Use the screen to monitor information reported by various SENSORS internal sensors. You cannot edit any information on this screen. Figure C-9. Sensors Screen Parameter Description CELL DETECT When the cell door is closed, the sensor can detect whether a cell is installed in the cell holder.

  • Page 137: Regulators Screen

    Regulators Screen Use the screen to monitor various pressure readings for the REGULATORS ASE 100. You cannot edit any information on this screen. NOTE Select the unit of measure for on-screen pressure readings on the screen (see Section C.1.3). SETUP Figure C-10.

  • Page 138: Hydrocarbon Sensor Screen

    ASE 100 Operator’s Manual C.2.4 Hydrocarbon Sensor Screen Use the screen to monitor the hydrocarbon level HYDROCARBON SENSOR at the ASE 100 installation site and to adjust the solvent vapor threshold, if necessary. Figure C-11. Hydrocarbon Sensor Screen Parameter Description ACTUAL Indicates the hydrocarbon level detected by the hydrocarbon sensor.

  • Page 139: Extraction Counters Screen

    Indicates the number of extractions performed since the ASE 100 was installed or the extraction counter was last reset. PUMP STROKE Indicates the number of pump strokes performed since the ASE 100 was installed or the pump stroke counter was last reset. EXTR. RESET Select RESET to reset the extraction counter to zero.

  • Page 140: Moduleware Screen

    Moduleware Screen screen indicates which version of ASE 100 MODULEWARE Moduleware is currently installed. The screen is also MODULEWARE displayed for a few seconds when the ASE 100 power is turned on. Figure C-13. Moduleware Screen C-14 Doc. 031842-01 5/02...
  • Page 141 D • Reordering Information Part Number Item Quantity 060074 Extraction cell, 10 mL Pkg. 6 060075 Extraction cell, 34 mL Pkg. 6 060076 Extraction cell, 66 mL Pkg. 6 060077 Extraction cell, 100 mL Pkg. 6 060070 Extraction cell, 10 mL 060071 Extraction cell, 34 mL 060072...
  • Page 142 ASE 100 Operator’s Manual Part Number Item Quantity 056929 Filter insertion tool 056699 Aluminum funnel 059927 Cell cooling rack 060372 Thermal gloves 1 pair 060174 Rinse cell, short 060175 Rinse cell, medium 060176 Rinse cell, long 045900 Solvent bottle, plastic-coated glass, 1 liter...
  • Page 143 Acetone, 2-6, 3-2 Acidic solvents, 3-2 Shutdown procedure, 3-12, 3-27 Basic solvents, 3-2 Arrow buttons, 2-5 Shutdown procedure, 3-12, 3-27 ASE 100 BNA method parameters, 2-14 Control panel, 2-2 Bottle, solvent, 2-2, 2-8 Decibel level, A-1 Cap assembly, D-2 Dimensions, A-1 Bubbles in solvent lines, 3-12 Display screen, 2-2 –...
  • Page 144 Selecting options, C-9 Changing the size, 1-2 Diatomaceous earth (DE), 3-5 – 3-6 Does not fit in cell holder, B-13 Dionex Technical Support, 4-1, 5-1 Handling hot cells, 3-23, B-12 – B-13 Dispersing agents, 3-5 Installation, 3-21 – 3-22 Display and keypad specifications, A-2 Matching to rinse cell size, 1-2, 2-7, 3-12, Display screen, 2-2 –...
  • Page 145 Index Replacing the end cap seal, 5-2 Replacing the O-ring, 5-4 Replacing the seal, 5-2 – 5-3 Leaks, 4-10 Sizes available, 1-2 Source requirements, B-1 Specifying the size, C-4 Gloves, thermal, 3-23, B-12 – B-13 Extractions Part number, D-2 Aborting, 3-25 Monitoring, 2-12 Overview of process, 2-11 Preliminary steps, 2-11...
  • Page 146 OVEN READY status, 2-11, 3-21, 4-7 Moduleware, 4-1, C-14 OVEN WAIT status, 3-21 Version number, C-1, C-14 Moduleware screen, C-14 Parameters Displaying values, 2-5 Needle switch, 2-2 Parts, non-Dionex, 5-1 Needles, 2-2, 2-9 PCB method parameters, 2-16 Nitric acid, 3-2 Index-4 Doc. 031842-01 5/02...
  • Page 147 Index PDF method parameters, 2-16 Rear panel, 2-9 PEEK seals Illustration, 2-10, B-3 Part number, D-1 Regulators screen, C-11 When to replace, 3-26 Relief valve, 2-9 Physical specifications, A-1 Replacing, 5-15 Piston seals Selecting the valve position, B-16, C-4 Replacing, 5-12 – 5-14 Replacement parts, D-1 Power cord, B-4 Right side panel...
  • Page 148 ASE 100 Accelerated Solvent Extractor Septum (collection bottle), 2-2, 2-7 Source needle, 2-2 When to replace, 2-7, 3-21 Liquid drips, 4-8 Service procedures Location, 5-21 AutoSeal lower tip replacement, 5-29 Maintenance, 3-26 Cell O-ring replacement, 5-4 Moving, 2-2 Cell seal replacement, 5-2 – 5-3...
  • Page 149 Index Snap ring tool, D-1 TPH method parameters, 2-17 Troubleshooting, 4-1 Electrical cables, 4-10 Excessive cell pressure, 4-3 Liquid leaks, 4-8, 4-10 System stopped, 4-10 Tubing Vent, B-2 Up/Down switch, 2-2 Valves Pressure relief, 2-9 Vapor threshold exceeded, 4-5 Vent lines, 2-9 Vent needles, 2-2 Moving, 2-2 Vent, system, 2-2...
  • Page 150 ASE 100 Accelerated Solvent Extractor Index-8 Doc. 031842-01 5/02...

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