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Micromeritics VacPrep 061 Operator's Manual

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VacPrep 061
Operator's Manual
061-42802-01
Feb 2013

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Summary of Contents for Micromeritics VacPrep 061

  • Page 1 VacPrep 061 Operator’s Manual 061-42802-01 Feb 2013...
  • Page 2 © Micromeritics Instrument Corporation 2002-2013. All rights reserved.
  • Page 3 MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including, but not limited to, the implied warranties of merchantability or fitness for use.

  • Page 5: Table Of Contents

    VacPrep 061 Table of Contents TABLE OF CONTENTS INSTALLATION Description ..............1-1 Conventions .
  • Page 6 Table of Contents VacPrep 061 Replacing Flexible Tubing ........... 3-7 Cleaning and Replacing Vacuum Fittings .

  • Page 7: Installation

    Description 1. INSTALLATION Description The VacPrep 061 Degasser prepares samples for adsorption analysis. Moisture and other con- taminants are removed by heating the sample while using any of the following methods: • applying a vacuum to the sample • passing a flowing gas over the sample •...

  • Page 8: Conventions

    Conventions VacPrep 061 Conventions This manual uses the symbols shown below to identify notes of importance, warnings, and cautions. Notes contain important information pertinent to the subject matter. Warnings contain information that help you prevent actions that may cause personal injury.

  • Page 9: Specifications

    VacPrep 061 Specifications Specifications The following table gives the specifications of the VacPrep 061 Degasser. Table 1-1. Specifications Characteristic Specification Sample Tubes Up to 3.0-cm (1 3/16-in.) OD bulbs with 1/4-, 3/8-, or 1/2-in., 9mm, 12mm OD stems. Heating Block Temperature: 10 ºC above ambient to 400 ºC...

  • Page 10: Unpacking And Inspection

    If equipment is damaged or lost in transit, you are required to make note of the damage or loss on the freight bill. The freight carrier, not Micromeritics, is responsible for all damage or loss occurring during shipment. If you discover damage or loss of equipment during shipment, report the condition to the carrier immediately.

  • Page 11: Selecting The Input Power

    VacPrep 061 Selecting the Input Power Selecting the Input Power All instruments leave the factory set for 120 VAC and with the line fuse removed. The correct setting of the universal power entrance must be checked and the appropriate fuse installed before the degasser can be operated.
  • Page 12 Selecting the Input Power VacPrep 061 4. Orient the voltage selector card so that the desired voltage is indicated at the bottom. Orient the indicator pin so that it points upward as shown in the following illustration. Indicator Pin Voltage 5.
  • Page 13 VacPrep 061 Selecting the Input Power a. Observe the position of the fuse block (shown on previous page) for reference. If the single-fuse arrangement is desired, the fuse block should be positioned such that the side with the single fuse slot and the jumper bar is away from the cover.

  • Page 14: Rear Panel Connections

    Rear Panel Connections VacPrep 061 Rear Panel Connections 1. Insert one end of the power cord into the input power connector at the rear of the degasser and the other end into the appropriate power source. When the VacPrep leaves the factory, stabilizing tubes are placed in heating stations 1 and 6 to prevent the heater block from shifting during shipment.
  • Page 15 VacPrep 061 Rear Panel Connections 6. Attach the other end of the copper tubing to the fitting on the back of the degasser. Copper Tubing Vacuum Port Gas Fitting 7. Open the gas bottle shut-off valve. 8. Use the regulator pressure control knob to adjust the pressure. The following table shows pressures and their resulting flow rates (tested with helium and nitrogen).
  • Page 16 (An appropriate vacuum pump is available from Micromeritics. Refer to Ordering Information in Chapter 4. The vacuum pump system offered by Micromeritics includes hose clamps and tubing. Cut the tubing to the length needed. Follow the installation instructions provided with the pump.)

  • Page 17: Attaching Flexible Tubing

    VacPrep 061 Attaching Flexible Tubing Attaching Flexible Tubing Six pieces of flexible tubing are included in the accessories kit. Attach one piece of tubing to the barbed vacuum/gas fitting at each degas station on the front panel. Attaching Vacuum Fittings for Vacuum Preparation If your sample fluidizes easily and you are using a Flow Control Valve, install it at this time using the instructions provided with the valve.

  • Page 18: Attaching Gas Delivery Tubes For Flowing Gas Preparation

    Attaching Gas Delivery Tubes for Flowing Gas Preparation VacPrep 061 Attaching Gas Delivery Tubes for Flowing Gas Preparation Six stainless steel gas delivery tubes are included in the accessories kit. Attach a gas delivery tube to the flexible tubing at any degas station that will be used for flowing gas preparation.

  • Page 19: Calibrating The Vacuum Gauge

    Calibrating the Vacuum Gauge Calibrating the Vacuum Gauge The vacuum gauge on the VacPrep 061 was calibrated and tested at the factory using a 115 V, 60 Hz electrical supply. When powered by other voltages and frequencies, the gauge must be recalibrated.

  • Page 20: Creating A Sorption Pump

    VacPrep 061 Creating a Sorption Pump You can improve the vacuum in the VacPrep 061 by creating a sorption pump using a sample tube and a microporous material with a high surface area. The following steps describe how to create a sorption pump.

  • Page 21: Operation And Sample Preparation

    VacPrep 061 Operation 2. OPERATION AND SAMPLE PREPARATION Operation Front Panel Features Vacuum Gauge VACUUM/GAS Control Knobs Temperature Controller Temperature Controller The temperature controller displays both the set point and the current temperature of the heating stations and enables you to change the temperature set point.

  • Page 22: Rear Panel Features

    Operation VacPrep 061 Rear Panel Features Vacuum Port Gas Port Power On/Off Switch Power On/Off Switch Place the switch in the up position ( | ) to turn on the degasser, and in the down position (0) to turn off the degasser.

  • Page 23: Controlling The Temperature Of Heating Stations

    VacPrep 061 Operation Controlling the Temperature of Heating Stations The temperature controller, shown below, enables you to specify the temperature of the heat- ing stations and displays the current temperature. Lights when power is being applied to heating stations Displays current temperature...

  • Page 24: Sample Preparation

    Sample Preparation VacPrep 061 Sample Preparation Cleaning Sample Tubes Sample tubes must be clean to obtain accurate analysis results. Clean the tubes in an ultrasonic cleaning unit as follows. The materials required for cleaning and weighing samples are: • Ultrasonic cleaning unit •...
  • Page 25 VacPrep 061 Sample Preparation 5. Using either rubber gloves or a lint-free cloth (but not bare hands), remove the sample tube from the bowl. 6. Clean the interior of the sample tube with a brush. 7. Rinse the sample tube thoroughly with hot water. Then rinse it with isopropyl alcohol, using a waste container to collect used isopropyl alcohol.

  • Page 26: Weighing Samples

    Sample Preparation VacPrep 061 10. After degassing the empty sample tube, install the stopper and weigh it while it still contains inert gas. To get an accurate weight of a degassed sample, the gas in both the empty sample tube and in the tube when it contains the sample must be the same.
  • Page 27 VacPrep 061 Sample Preparation 6. Pour the sample from the sample weighing container into the sample tube using a funnel. 7. Insert the sample tube stopper. 8. Weigh the sample tube, sample, and rubber stopper. Record the weight as sample plus sample tube weight.

  • Page 28: Inserting And Removing Heating Station Adapters

    Sample Preparation VacPrep 061 Inserting and Removing Heating Station Adapters Heating station adapters are included in the VacPrep accessories kit for use with sample tubes. There are three models of heating station adapters. Use the appropriate model as shown in Table 1-3 and follow the instructions in this chapter for removing and inserting adapters.
  • Page 29 VacPrep 061 Sample Preparation Table 2-1. Heating Station Adapters Analyzer Model Sample Tubes Adapter Model TriStar ASAP Series 1/4, 3/8, or 1/2-in. Stem, 1-in Bulb P/N: 065-25815-00 Gemini (Bulb Tube) P/N: 065-25811-00 3/8-in. Stem, 3/4-in Bulb Gemini (Straight-Wall Tube) 3/8-in. Stem...
  • Page 30 Sample Preparation VacPrep 061 TriStar 3Flex P/N: 065-25815-00 1/4, 3/8, 1/2-in. 9mm, 12mm Stem 2-10 Feb 2013...

  • Page 31: Tristar And Asap Series Sample Tubes

    VacPrep 061 Sample Preparation TriStar and ASAP Series Sample Tubes Adapters for these sample tubes are included as a standard accessory with the SmartPrep. Additional adapters may be ordered if needed (refer to Chapter 5 for ordering information). Sample tubes and heating station adapters may be very hot. Wear the proper gloves and hold the sample tube by the upper part of its stem.

  • Page 32: Removing Adapters

    Sample Preparation VacPrep 061 Removing Adapters Use caution when moving sample tubes and heating station adapters to the cooling station. Sample tubes and heating station adapters may be very hot. Wear the proper gloves and hold the sample tube by the upper part of its stem. Hold the isothermal type of adapter by its handle.

  • Page 33: Gemini Sample Tubes

    VacPrep 061 Sample Preparation Gemini Sample Tubes Adapters are included as a standard accessory with the VacPrep. Additional adapters may be ordered if needed (refer to Ordering Information, page 4-1). Sample tubes and heating station adapters may be very hot. Wear the proper gloves and hold the sample tube by the upper part of its stem.

  • Page 34: Degassing Samples

    • Vacuum-backfill preparation - The sample is heated as the operator alternately applies a vacuum and then flows gas into the sample tube to remove moisture and other contaminants. The alternating process may be repeated several times. The VacPrep 061 is designed for low-pressure backfilling only.

  • Page 35: Vacuum Preparation

    Some fine-powdered samples such as controlled pore glass, fluid-cracking catalysts, and carbon may be difficult to prepare by vacuum preparation. Such materials tend to fluidize and float up the sample tube toward the vacuum source. Micromeritics recommends that such samples be first prepared by flowing gas preparation and, if necessary, then be subjected to vacuum preparation.
  • Page 36 Sample Preparation VacPrep 061 The vacuum fitting for the sample tube may be hot enough to cause burns if it was stored in a heating station instead of a cooling station. Wear the cotton gloves supplied in the accessories kit and handle the fitting carefully to avoid burns.
  • Page 37 VacPrep 061 Sample Preparation 10. Using an appropriate heating station adapter, insert the sample tube into the heating station. 11. Allow the sample(s) to degas for the desired length of time. One to two hours is typical for many samples at temperatures above 200 ºC. To determine the optimum time, select the highest safe temperature for your sample, then degas it for various intervals, determining the surface area after each interval.
  • Page 38 Sample Preparation VacPrep 061 13. Place the sample tube, with the vacuum fitting still in place, in a cooling station. Backfilling the sample tube increases its pressure to a level greater than atmospheric pressure. If the gas pressure is greater than the recommended maximum of 5 psig (35 kPag), the sample tube could be ejected from the fitting or broken.

  • Page 39: Alternating Vacuum-Backfill Preparation

    Some fine-powdered samples such as controlled pore glass, fluid-cracking catalysts, and carbon may be difficult to prepare by vacuum preparation. Such materials tend to fluidize and float up the sample tube toward the vacuum source. Micromeritics recommends that such samples be prepared by flowing gas preparation and, if necessary, then subjected to vacuum preparation.
  • Page 40 Sample Preparation VacPrep 061 9. After the sample is sufficiently degassed, remove the sample tube from the heating station. Leave the VAC/GAS control knob in the VAC position. Keep the sample tube attached to the vacuum fitting while cooling to prevent contamination from the ambient atmosphere.

  • Page 41: Flowing Gas Preparation

    VacPrep 061 Sample Preparation Flowing Gas Preparation Samples that contain a high level of moisture could benefit from a higher flow rate than 5 psi regulator pressure when using the flowing gas method. A flow rate up to 50 cm3/min (approximately 16 psi regulator pressure) may be used to aid in purging moisture form the sample when using the flowing gas preparation only.
  • Page 42 Sample Preparation VacPrep 061 The end of the gas delivery tube may be hot enough to cause burns if it was stored in a heating station instead of a cooling station. Wear the cotton gloves supplied in the accessories kit and handle the gas delivery tube carefully to avoid burns.
  • Page 43 VacPrep 061 Sample Preparation 7. Using the appropriate heating station adapter, place the sample tube in a vacant heating station. 8. Allow the sample to degas for the desired length of time. One to two hours is typical for many samples at temperatures above 200 ºC. To determine the optimum time, select the highest safe temperature for your sample, then degas it for various intervals, determining the surface area after each interval.
  • Page 44 Sample Preparation VacPrep 061 10. Place the sample tube, with stopper and gas delivery tube still in place, in a cooling station. 11. The sample tube should be cool enough to handle after several minutes. Remove the tube from the cooling station. Hold the stopper loosely in the tube and slowly pull out the gas delivery tube.
  • Page 45 VacPrep 061 Sample Preparation 13. Place the VAC/GAS control knob in the OFF position. 14. Wipe the gas delivery tube with a clean cloth to remove any particles of sample that may have adhered to it. Then place the gas delivery tube in a cooling station until needed again.
  • Page 46 Sample Preparation VacPrep 061 2-26 Feb 2013...

  • Page 47: Troubleshooting And Maintenance

    Troubleshooting 3. TROUBLESHOOTING AND MAINTENANCE The VacPrep 061 requires very little maintenance to remain in top operating condition. The gas flow tubes should be wiped clean after each use and inspected weekly to ensure that they do not become clogged. This chapter contains instructions for inspecting and replacing gas flow tubes and vacuum fittings, as well as a troubleshooting chart and other maintenance procedures.
  • Page 48 Troubleshooting VacPrep 061 Table 3-1. Common Operational Problems (continued) What Happened What To Do Gas seems to be leaking The flow control valves were Keep the flow control valve from gas bottle. left in the open (GAS) position closed (OFF) at on all stations when stations were not in use.
  • Page 49 VacPrep 061 Troubleshooting Table 3-1. Common Operational Problems (continued) What Happened What To Do Vacuum reading too high. Vacuum pump is turned off. Turn the vacuum pump on. Vacuum tubing leak. Replace tubing if cracked. Vacuum connection leak. Check connections and tighten clamps.

  • Page 50: Temperature Controller Error Messages

    Temperature Controller Error Messages VacPrep 061 Temperature Controller Error Messages The temperature controller performs self-diagnostics when the degasser is turned on and while operating. If an error occurs during self-diagnostics, one of the following error messages will be displayed. uuuu...

  • Page 51: Maintenance

    3-9). Gas delivery tubes and flexible tubing may be ordered in sets of six from Micromeritics. Refer to Chapter 4, Ordering Information. If gas flow is not present in other stations, refer to the following table. Table 3-2. Gas Flow Problems What To Do Gas pressure is set too low.

  • Page 52: Cleaning And Replacing Gas Delivery Tubes

    Maintenance VacPrep 061 Cleaning and Replacing Gas Delivery Tubes Gas delivery tubes should be wiped with a lint-free cloth after each use to remove any particles of sample that may have adhered to the tube. If a gas delivery tube becomes clogged or damaged, it should be replaced as follows: 1.

  • Page 53: Replacing Flexible Tubing

    VacPrep 061 Maintenance Replacing Flexible Tubing If the flexible tubing becomes damaged, replace it as follows. 1. Remove the flexible tubing from the barbed fitting on the front panel. 2. Attach new flexible tubing. Barbed Fitting Flexible Tubing Cleaning and Replacing Vacuum Fittings The interior of vacuum fittings should be wiped with a lint-free cloth after each use to remove any particles of sample that may have adhered to the fitting.
  • Page 54 Maintenance VacPrep 061 2. If you are cleaning the fittings, disassemble them and clean the components with isopropyl alcohol (IPA). If the fitting O-ring is cracked or broken, replace the O-ring. Ensure adequate ventilation when using solvents for cleaning purposes.

  • Page 55: Connecting Or Replacing Valve Inlet Tubing

    VacPrep 061 Maintenance Connecting or Replacing Valve Inlet Tubing Flexible tubing connects the valves to the gas manifold inside the degasser. If there is no gas flow to a particular valve, the tubing could be disconnected. To check the tubing: 1.

  • Page 57: Ordering Information

    VacPrep 061 Ordering Information 4. ORDERING INFORMATION VacPrep 061 components and accessories can be ordered through our Order Entry Department. When ordering, use the information provided below. Table 4-1. VacPrep Components and Accessories Part Number Item and Description 061-00023-00 VacPrep 061 for use with Gemini Series analyzers, degasses up to six samples at up to 400ºC with either flowing gas or by evacuation...
  • Page 58 Ordering Informatioin VacPrep 061 Upper Front Panel View from Rear with Top Panel Removed Item Part Number Item and Description 004-27041-00 Dust Frit, 20 micron 004-25466-00 O-ring, Buna-N, size 010, for sealing dust frit and for 1/4-in. OD sample tube stem...
  • Page 59 VacPrep 061 Ordering Information 004-25079-06 O-ring 9mm tube 350-25843-01 Ferrule, 9mm tube 004-25013-02 O-Ring 12mm Tube 350-25843-00 Ferrule, 12mm Tube Feb 2013...
  • Page 60 Ordering Informatioin VacPrep 061 Feb 2013...
  • Page 61 VacPrep 061 Index INDEX types of, 2-9 Adapter Heating station adapters, 2-8 Maintenance procedures, 3-1 checking gas flow, 3-5 Cleaning/replacing gas delivery tubes, 3-6 Calibrating vacuum gauge, 1-13 cleaning/replacing vacuum fittings, 3-7 Cautions, defined, 1-2 connecting/replacing valve inlet tubing, 3-9...
  • Page 62 Index VacPrep 061 VacPrep description, 1-1 front panel, 2-1 rear panel, 2-2 specifications, 1-3 Vacuum fittings, attaching, 1-11 fittings, replacing, 3-7 gauge, calibrating, 1-13 Vacuum degas, 2-14 preparation, 1-11, 2-15 Vacuum-backfill degas, 2-14 preparation, 1-11, 2-19 Valve inlet tubing, replacing, 3-9...

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