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Micromeritics VacPrep Operator's Manual

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V
P
AC
REP
S
P
S
AMPLE
REPARATION
YSTEM
O
M
PERATOR
ANUAL
061-42802-01
Apr 2021
(Rev B)

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Summary of Contents for Micromeritics VacPrep

  • Page 1 ™ AMPLE REPARATION YSTEM PERATOR ANUAL 061-42802-01 Apr 2021 (Rev B)
  • Page 2 RADEMARKS Micromeritics is a registered trademark of Micromeritics Instrument Corporation. VacPrep is a trademark of Micromeritics Instrument Corporation. Copyright The software described in this manual is furnished under a license agreement and may be used or copied only in accordance with the terms of the agreement.

  • Page 3: Warranty

    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 4: Corporate Profile

    The company has R&D and manufacturing sites in the USA, UK, and Spain, and direct sales and service operations throughout the Americas, Europe, and Asia. Micromeritics systems are the instruments-of-choice in more than 10,000 laboratories of the world’s most innovative companies, prestigious government, and academic institutions. Our world-class scientists and responsive support teams enable customer success by applying Micromeritics technology to the most demanding applications.

  • Page 5: Contact Us

    Norcross, GA / USA / 30093-2901 Phone: 1-770-662-3636 Fax: 1-770-662-3696 www.Micromeritics.com Instrument Service or Repair Phone: 1-770-662-3666 International — contact your local distributor or call 1-770-662-3666 Service.Helpdesk@Micromeritics.com Micromeritics Learning Center Phone: 1-770-662-3607 www.Micro.edu VacPrep Operator Manual 061-42802-01 (Rev B) — Apr 2021...

  • Page 6: About This Manual

    NOTE — Notes contain important information applicable to the topic. CAUTION — Cautions contain information to help prevent actions that may damage the analyzer or components. WARNING — Warnings contain information to help prevent actions that may cause personal injury. VacPrep Operator Manual 061-42802-01 (Rev B) — Apr 2021...

  • Page 7: General Safety

    General Safety ENERAL AFETY Do not modify this instrument without the authorization of a Micromeritics service per- sonnel. Use caution in the areas where this symbol is displayed on the instrument — such as near the heating stations. These surfaces may be hot and could cause serious burns.
  • Page 8 General Safety NTENDED The VacPrep 061 degasser prepares samples for adsorption analysis. Moisture and other contaminants are removed by heating the sample.The degasser has six heating stations for degassing samples and six cooling stations. The required degassing temperature is set and checked at the temperature controller.
  • Page 9 EFUP (for example, battery modules) and so are marked to reflect such. The Environmentally Friendly Use Period is valid only when the product is operated under the conditions defined in the product manual. VacPrep Operator Manual viii 061-42802-01 (Rev B) — Apr 2021...

  • Page 11: Table Of Contents

    Table of Contents Warranty Corporate Profile Contact Us About this Manual General Safety 1 About the VacPrep 1 - 1 Specifications for VacPrep 1 - 3 2 Installation 2 - 1 Unpacking and Inspection 2 - 1 Shipping Damage 2 - 2...
  • Page 12 5 - 15 A Temperature Controller Error Messages A - 1 B Sample Data Worksheet for Gas Adsorption B - 1 VacPrep 061 CE Declaration of Conformity DoC - 1 Index Index - 1 VacPrep Operator Manual 061-42802-01 (Rev B) — Apr 2021...

  • Page 13: About The Vacprep

    1 About the VacPrep BOUT THE Use caution in the areas where this symbol is displayed on the instrument — such as near the heating stations. These surfaces may be hot and could cause serious burns. Use the gloves supplied in the accessories kit.
  • Page 14 1 About the VacPrep ANEL A. Power switch B. Gas port C. Vacuum port VacPrep Back Panel Description Component Use to connect the gas supply to the degasser. Gas Port Use to power ON or power OFF the degasser. Power Switch Use to connect the external vacuum pump to the degasser.

  • Page 15: Specifications For Vacprep

    Specifications for VacPrep PECIFICATIONS FOR Sample Tubes Up to 3.0 cm (1 3/16 in.) OD bulbs with 1/4, 3/8, 1/2 in., 9 mm, or 12 mm OD stems Heating Block Temperature 10 ºC above ambient to 400 ºC Accuracy within ± 10 °C...
  • Page 16 A vacuum source achieving better than 20 μmHg at the instrument inlet and having a device to reduce oil vapor backstreaming is recommended. The vacuum system must also have an anti- suckback valve to prevent oil from flowing into the VacPrep should there be a power failure. Sample Capacity...

  • Page 17: Installation

    Sort through all packing material before declaring missing equipment or parts. Micromeritics recommends saving all shipping containers until installation of the equip- ment is complete. All shipping containers where equipment is to be declared as dam- aged or lost must be examined by the claims investigator prior to completion of the inspection report.

  • Page 18: Shipping Damage

    QUIPMENT ETURNS Micromeritics strives to ensure that all items arrive safely and in working order. If it is necessary to return equipment (damaged either during shipment or while in use) to Micromeritics for repair or replacement, follow these procedures: 1.

  • Page 19: Guidelines For Connecting Gases

    500 psi (3500 kPa) on the high pressure gauge. Contaminants absorbed to the walls of the cylinder will desorb as the pressure decreases. Ensure the gas cylinder is closed before connecting to the analyzer. VacPrep Operator Manual 2 - 3 061-42802-01 (Rev B) — Apr 2021...

  • Page 20: Connect Gas To Analyzer

    The degasser ships with stabilizing tubes in heating stations 1 and 6 to prevent the heater block from shifting during shipment. Ensure these tubes are removed before powering on the degasser. VacPrep Operator Manual 2 - 4 061-42802-01 (Rev B) — Apr 2021...

  • Page 21: Select Input Power

    Use of other fuses could result in electrical shock and/or damage to the instrument. Fuses may be obtained from Micromeritics or a vendor of your choice as long as they meet the requirements specified in this section.
  • Page 22 4. Invert the fuse block and slide the block back onto the Phillips screw and pedestal. 5. Tighten the Phillips screw and and replace the cover. The fuse(s) that go into the housing first are the active set. VacPrep Operator Manual 2 - 6 061-42802-01 (Rev B) — Apr 2021...
  • Page 23 Select the Voltage on the next page then continue with these steps. 4. Slide the block back onto the Phillips screw and pedestal. 5. Tighten the Phillips screw and replace the cover. VacPrep Operator Manual 2 - 7 061-42802-01 (Rev B) — Apr 2021...
  • Page 24 3. Insert voltage selector card into the housing. The printed side of the card must face toward IEC connector and the edge displaying the voltage goes in first. 4. Replace the fuse cover. 5. Verify that the indicator pin shows the required voltage. VacPrep Operator Manual 2 - 8 061-42802-01 (Rev B) — Apr 2021...

  • Page 25: Rear Panel Connections

    5. Attach the copper tubing to the brass reducer fitting. 6. Attach the other end of the copper tubing to the fitting on the back of the degasser. VacPrep Operator Manual 2 - 9 061-42802-01 (Rev B) — Apr 2021...
  • Page 26 Use hose clamps to keep the hose in place. An appropriate vacuum pump system that includes hose clamps and tubing is available from Micromeritics. Cut the tubing to the length needed. Follow the installation instructions provided with the pump.

  • Page 27: Connect The Power Cable

    Use of a power cord or power supply not provided with the instrument could cause personal injury or damage to the equipment. If a replacement is needed, contact your Micromeritics Service Representative. Detachable power supply cords with an inadequate rating could cause significant instrument damage or physical harm.

  • Page 28: Attach 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. Barbed fitting Flexible tubing installed VacPrep Operator Manual 2 - 12 061-42802-01 (Rev B) — Apr 2021...

  • Page 29: Attach Gas Delivery Tubes

    A. Flexible tubing B. Ferrule C. Gas delivery tube VacPrep Operator Manual 2 - 13 061-42802-01 (Rev B) — Apr 2021...

  • Page 30: Attach Vacuum Fittings For Vacuum Preparation

    1/2 in. or 12 mm O-ring and 3/8 in. or 9 mm O-ring and ferrule (for 1/2 in. or 12 mm ferrule (for 3/8 in. or 9 mm sample tubes) sample tubes) VacPrep Operator Manual 2 - 14 061-42802-01 (Rev B) — Apr 2021...

  • Page 31: Vacuum Gauge Calibration

    Create a Sorption Pump on the next page The vacuum gauge on the VacPrep 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 32: Create A Sorption Pump

    REATE A ORPTION The VacPrep vacuum can be improved by creating a sorption pump using a sample tube and a microporous material with a high surface area. 1. Partially fill a sample tube with material of a high surface area, such as aquarium charcoal, other forms of activated carbon, or zeolite.

  • Page 33: Sample Preparation

    The keys may be held down to rapidly increase or decrease the setting. The set point is retained when the degasser is powered off then back on. VacPrep Operator Manual 3 - 1 061-42802-01 (Rev B) — Apr 2021...
  • Page 34 4. Fill the sample tubes with warm water and place them in the ultrasonic cleaning unit, then place the filler rods in the unit. Turn on the ultrasonic cleaning unit for approximately 15 minutes. VacPrep Operator Manual 3 - 2 061-42802-01 (Rev B) — Apr 2021...

  • Page 35: Clean And Label Sample Tubes

    9. Remove the sample tubes and filler rods from the oven and allow to cool. Do not insert the filler rods at this time. Filler rods are inserted before the sample tube is installed on the analysis port. VacPrep Operator Manual 3 - 3 061-42802-01 (Rev B) — Apr 2021...
  • Page 36 11. Rinse the sample tube closure with isopropyl alcohol, then wipe the sample tube closure dry with a clean, lint-free cloth. 12. Label the sample tube and stopper for identification. 13. Replace the rubber stopper. VacPrep Operator Manual 3 - 4 061-42802-01 (Rev B) — Apr 2021...

  • Page 37: Determine The Sample Mass

    7. Remove either the rubber stopper from the sample tube. 8. Use the sample tube funnel (provided in the accessories kit) and pour the sample from the weighing container into the sample tube. VacPrep Operator Manual 3 - 5 061-42802-01 (Rev B) — Apr 2021...
  • Page 38 9. On the Sample Data Worksheet, record the following: Mass of the sample tube set with the sample. Subtract the Mass of empty sample tube set from the Mass of sample tube set plus sample. VacPrep Operator Manual 3 - 6 061-42802-01 (Rev B) — Apr 2021...

  • Page 39: Heating Station Adapters

    Use the appropriate model as shown in the Heating Station Adapters table. Additional adapters can be ordered from Micromeritics. The adapters used with Gemini sample tubes may remain in the stations until a different type of sample tube is needed.
  • Page 40 1.2 in. (30 mm) bulb Gemini (bulb tube) 3/8 in. stem, 3/4 in. (19 mm) bulb Part number: 065-25811-00 Gemini (straight-wall tube) 3/8 in. stem Part number: 065-25812-00 VacPrep Operator Manual 3 - 8 061-42802-01 (Rev B) — Apr 2021...
  • Page 41 Heating Station Adapters Heating Station Adapters (continued) Sample Tubes Adapter Model Analyzer Model TriStar Flex 1/4, 3/8, 1/2 in. Part number: 060-25850-00 9mm, 12mm stem VacPrep Operator Manual 3 - 9 061-42802-01 (Rev B) — Apr 2021...

  • Page 42: Tristar And Asap Series Sample Tubes

    Use caution when moving sample tubes and heating station adapters to the cooling station. 1. Hold the stem of the sample tube and the adapter handle and remove the adapter and sample tube. VacPrep Operator Manual 3 - 10 061-42802-01 (Rev B) — Apr 2021...
  • Page 43 2. Place the adapter and sample tube in a cooling station. After the sample tube has been installed on the analyzer, place the adapter back into the heating station for storage. VacPrep Operator Manual 3 - 11 061-42802-01 (Rev B) — Apr 2021...

  • Page 44: Gemini Sample Tubes

    Slide the adapter into the heating station and remove the adapter. Heating Station Sample Tube Adapter Heating Station Sample Tube Adapter Insertion / Removal Tool A. Adapter insertion tool B. Sample tube adapter VacPrep Operator Manual 3 - 12 061-42802-01 (Rev B) — Apr 2021...
  • Page 45 Gemini Sample Tubes Remove Adapters Adapters for the Gemini may remain in the heating station when not in use. If removing the adapter, use the adapter tool. VacPrep Operator Manual 3 - 13 061-42802-01 (Rev B) — Apr 2021...

  • Page 47: Degas The Sample

    5 psi regulator pressure when using the flowing gas method. A flow rate up to 50 cm /min (approximately 16 psi regulator pressure) may be used to aid in purging moisture from the sample when using flowing gas preparation only. VacPrep Operator Manual 4 - 1 061-42802-01 (Rev B) — Apr 2021...

  • Page 48: 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 49 200 ºC. To determine the optimum time, select the highest safe temperature for the sample, then degas it for various intervals, determining the surface area after each interval. VacPrep Operator Manual 4 - 3 061-42802-01 (Rev B) — Apr 2021...
  • Page 50 18. Reweigh the sample tube with stopper and sample to ensure that the correct sample weight is recorded. The weight recorded at this step may be compared to the weight recorded before preparation to determine if adequate degassing has occurred. VacPrep Operator Manual 4 - 4 061-42802-01 (Rev B) — Apr 2021...

  • Page 51: Alternating Vacuum Backfill Preparation

    REPARATION Alternating vacuum-backfill sample preparation utilizes a combination of vacuum and gas backfilling techniques to remove contaminants and prepare samples for analysis. The VacPrep is designed for low-pressure backfilling only. Do not exceed 5 psi regulator pressure when backfilling sample tubes. If the gas pres- sure is greater than the recommended maximum of 5 psig (35 kPag), the sample tube could be ejected from the fitting or broken.
  • Page 52 18. When the sample has sufficiently cooled, turn the VAC/GAS control knob to the OFF pos- ition and then to the GAS position. 19. Allow the gas to flow for approximately 30 seconds; then turn the VAC/GAS control knob to the OFF position. VacPrep Operator Manual 4 - 6 061-42802-01 (Rev B) — Apr 2021...
  • Page 53 22. Reweigh the sample tube with stopper and sample to ensure that the correct sample mass is recorded. The weight recorded at this step may be compared to the weight recorded before preparation to determine if adequate degassing has occurred. VacPrep Operator Manual 4 - 7 061-42802-01 (Rev B) — Apr 2021...

  • Page 54: Flowing Gas Preparation

    Then tilt the sample tube back to a ver- tical position and tap the tube to settle the sample bed around the gas delivery tube. VacPrep Operator Manual 4 - 8 061-42802-01 (Rev B) — Apr 2021...
  • Page 55 It is unnecessary to use a stopper with sample tubes having an inside diameter of only 5 mm (0.2 in.). 7. Using the appropriate heating station adapter, place the sample tube in a vacant heating station. VacPrep Operator Manual 4 - 9 061-42802-01 (Rev B) — Apr 2021...
  • Page 56 Keep the gas delivery tube and stopper in the sample tube while cooling to prevent contamination from the ambient atmosphere. 10. Place the sample tube, with stopper and gas delivery tube still in place, in a cooling station. VacPrep Operator Manual 4 - 10 061-42802-01 (Rev B) — Apr 2021...
  • Page 57 15. Reweigh the sample tube with stopper and sample to ensure that the correct sample mass is recorded. The weight recorded at this step may be compared to the weight recorded before preparation to determine if adequate degassing has occurred. VacPrep Operator Manual 4 - 11 061-42802-01 (Rev B) — Apr 2021...

  • Page 59: Troubleshooting And Maintenance

    Safe operation and handling of the instrument, supplies, and accessories is the responsibility of the operator. Do not modify this instrument without the authorization of a Micromeritics service per- sonnel. When lifting or relocating the instrument, use proper lifting and transporting devices for heavy instruments.
  • Page 60 Action B: Decrease the flow rate by turning the regulator pressure control knob clockwise. Cause C: A flow control valve is leaking. Action C: Contact the appropriate service personnel. No gas flow when the flow control valve is open. VacPrep Operator Manual 5 - 2 061-42802-01 (Rev B) — Apr 2021...
  • Page 61 Action F: Check O-ring and replace if necessary. Cause G: Sample tube is broken or cracked. Action G: Replace the sample tube. Cause H: One of the other sample tubes has a loose fitting. VacPrep Operator Manual 5 - 3 061-42802-01 (Rev B) — Apr 2021...

  • Page 62: Parts And Accessories

    5 Troubleshooting and Maintenance Action H: Close all valves to verify proper operation of the vacuum pump. ARTS CCESSORIES Parts and accessories can be found online at www.Micromeritics.com. VacPrep Operator Manual 5 - 4 061-42802-01 (Rev B) — Apr 2021...

  • Page 63: Safe Servicing

    Safe Servicing ERVICING Do not modify this instrument without the authorization of a Micromeritics service per- sonnel. To ensure safe servicing and continued safety of the instrument after servicing, service personnel should be aware of the following risks: Product specific risks that may affect service personnel: Electrical.

  • Page 64: Power

    It is not necessary to remove knobs, screws, etc. while cleaning. Do not allow liquid to penetrate the casing of the instrument. Doing so could result in damage to the unit. VacPrep Operator Manual 5 - 6 061-42802-01 (Rev B) — Apr 2021...

  • Page 65: Check The Gas Flow

    Replace the gas cylinder. Gas cylinder is empty Check the valve inlet tube connections. Valve inlet tubing is disconnected Contact the appropriate service personnel. Flow control valve is damaged VacPrep Operator Manual 5 - 7 061-42802-01 (Rev B) — Apr 2021...
  • Page 66 5 Troubleshooting and Maintenance Gas Flow Rate for the VacPrep A flow rate of 10-15 cm /min is the maximum Gauge Pressure Flow flow rate that would generally be used in /min normal operation. Do not exceed 5 psi regulator pressure when backfilling sample tubes. 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 67: Gas Delivery Tubes

    2. Attach a new gas delivery tube by pressing the flexible tubing over the gas delivery tube. Ensure that the flexible tubing completely covers the ferrule at the end of the gas delivery tube. VacPrep Operator Manual 5 - 9 061-42802-01 (Rev B) — Apr 2021...

  • Page 68: Replace Flexible Tubing

    5 Troubleshooting and Maintenance EPLACE LEXIBLE UBING 1. Remove the flexible tubing from the barbed fitting on the front panel. 2. Attach new flexible tubing. Barbed fitting Flexible tubing installed VacPrep Operator Manual 5 - 10 061-42802-01 (Rev B) — Apr 2021...

  • Page 69: Valve Inlet Tube

    (one per valve) B. Gas manifold C. Gas port D. Vacuum port E. Vacuum gauge tube 5. Replace the top rear panel. 6. Power ON the vacuum pump. VacPrep Operator Manual 5 - 11 061-42802-01 (Rev B) — Apr 2021...

  • Page 70: Replace The Vacuum Fittings

    5 Troubleshooting and Maintenance EPLACE THE ACUUM ITTINGS 1. Remove the flexible tubing from the barbed fitting on the front panel. 2. Attach new flexible tubing. Barbed fitting Flexible tubing installed VacPrep Operator Manual 5 - 12 061-42802-01 (Rev B) — Apr 2021...

  • Page 71: Clean And Replace Vacuum Fittings

    O-ring. Clean all components with IPA or use an ultrasonic bath may be used. If the dust filter O-ring is cracked or broken, replace it. Reattach the dust frit, O-ring, and port nipple. VacPrep Operator Manual 5 - 13 061-42802-01 (Rev B) — Apr 2021...
  • Page 72 4. Attach the cleaned or replacement fittings by pressing the flexible tubing completely over the barbed nipple on the end of the fitting. Loosely attach the knurled retaining nut, ferrule, and O-ring. VacPrep Operator Manual 5 - 14 061-42802-01 (Rev B) — Apr 2021...

  • Page 73: Preventive Maintenance

    AINTENANCE Perform the following preventive maintenance procedures to keep the analyzer operating at peak performance. Micromeritics also recommends that preventive maintenance procedures and calibration be performed by a Micromeritics Service Representative every 12 months. Frequency Maintenance Required Clean after each use and replace as needed...

  • Page 75: A Temperature Controller Error Messages A

    Observe the display. The temperature will be displayed if it is decreasing. If the tem- Action: perature does not decrease, the message will remain displayed. Power off the instrument and contact the appropriate service personnel. VacPrep Operator Manual A - 1 061-42802-01 (Rev B) — Apr 2021...

  • Page 77: B Sample Data Worksheet For Gas Adsorption B

    Mass of sample tube set plus sample Mass of sample (step 2 minus step 1) Degas Information Degas apparatus Temperature (°C) Time (hours) Actual time started Actual time finished Degas Notes: VacPrep Operator Manual B - 1 061-42802-01 (Rev B) — Apr 2021...
  • Page 80 2 - 11 preventive maintenance 5 - 15 filler rod, clean 3 - 2 flowing gas preparation, VacPrep 4 - 8 rear panel connections 2 - 9 check flow 5 - 7 delivery tubes, attach 2 - 13...
  • Page 81 2 - 1 VacPrep about 1 - 1 specifications 1 - 3 vacuum backfill preparation, VacPrep 4 - 5 vacuum fittings replace 5 - 12 vacuum fittings, attach 2 - 14 vacuum fittings, clean and replace 5 - 13...

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