Micromeritics VacPrep, Operator'S Manual

Page 1: ...OPERATOR MANUAL 061 42802 01 Apr 2021 Rev B VACPREP SAMPLE PREPARATION SYSTEM...

Page 2: ...ument 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: ...igations of this warranty will be limited under the following conditions 1 Certain products sold by MICROMERITICS are the products of reputable manufacturers sold under their respective brand names or...

Page 4: ...ity testing of catalysts 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 t...

Page 5: ...ax 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 Microme...

Page 6: ...r in 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 Warnin...

Page 7: ...er lifting and transporting devices for heavy instruments Ensure that sufficient personnel are available to assist in moving the instrument The VacPrep weighs approximately 10 kg 22 lb n Always pay at...

Page 8: ...indication of the valve state A built in vacuum gauge provides a constant indication of the system vacuum The instrument is intended to be operated by trained personnel familiar with the proper opera...

Page 9: ...o o o o o o Temperature Controller o o o o o o Electronic Components x o o o o o External Controls x o o o o o Hazardous Substances Table o Hazardous substance is below the specified limits as describ...

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Page 11: ...ases 2 3 Connect Gas to Analyzer 2 4 Remove Stabilizing Tubes 2 4 Select Input Power 2 5 Rear Panel Connections 2 9 Connect the Power Cable 2 11 Attach Flexible Tubing 2 12 Attach Gas Delivery Tubes 2...

Page 12: ...arts And Accessories 5 4 Safe Servicing 5 5 Power 5 6 Clean the Instrument 5 6 Check the Gas Flow 5 7 Gas Delivery Tubes 5 9 Replace Flexible Tubing 5 10 Valve Inlet Tube 5 11 Replace the Vacuum Fitti...

Page 13: ...ponent Description Cooling Stations Six stations to cool the sample Heating Stations Six stations to heat the sample Temperature Controller Displays the set point and the current temperature of the he...

Page 14: ...mponent Description Gas Port Use to connect the gas supply to the degasser Power Switch Use to power ON or power OFF the degasser Vacuum port Use to connect the external vacuum pump to the degasser Va...

Page 15: ...60 Hz Electrical Temperature 10 to 35 C operating 0 to 50 C non operating Humidity 45 to 90 relative non condensing Indoor or Outdoor Use Indoor only Altitude 2000 m max Pollution degree of the intend...

Page 16: ...anti suckback valve to prevent oil from flowing into the VacPrep should there be a power failure Vacuum System 6 heating stations and 6 cooling stations Sample Capacity Height 43 cm 17 in Width 36 cm...

Page 17: ...ly inert gasses helium nitrogen or argon should be used for sample preparation Inert gasses in the quantities used by the degasser do not pose a health hazard to users UNPACKING AND INSPECTION When th...

Page 18: ...not discard shipping boxes and containers until installation is complete If space is avail able it is recommended that shipping containers be saved for future use in the event of return to factory fo...

Page 19: ...o remove ambient gases When possible avoid placing gas cylinders in remote locations It is always best to have gas cylinders located near the analyzer n Use a retaining strap or other appropriate teth...

Page 20: ...gas line to the instrument 1 Loosen then remove the plug from the gas port on the back of the degasser 2 Insert the gas line into the port and hand tighten the connector nut Use a 7 16 in 11 mm wrench...

Page 21: ...o disconnect the power cord could result in electrical shock n The input power connector can be used with either a single fuse arrangement 100 120VAC or a double fuse arrangement 230 240VAC Use the ap...

Page 22: ...open b Loosen the Phillips screw two turns c Remove the fuse block by sliding it up then away from the Phillips screw and lifting the block from the pedestal A Fuse cover B Fuse block C Fuses D Jumper...

Page 23: ...c Remove the fuse block by sliding it up then away from the Phillips screw and lifting the block from the pedestal A Fuse cover B Fuse block C Jumper D Fuse 2 Insert the fuse 3 Set the voltage See Se...

Page 24: ...ing indicator 2 Set the voltage a Position the selector card so that the required voltage is readable at the bottom and the selector pin is pointing up 100V 120V 230V 240V 3 Insert voltage selector ca...

Page 25: ...the gas cylinder Leave the gas cylinder shut off valve closed until instructed otherwise 3 If the regulator has a 1 8 in outlet proceed to Step 4 If the regulator has a 1 4 in outlet attach the reduc...

Page 26: ...mple tube could be ejected from the fitting or broken 9 Close the gas cylinder shut off valve Check the pressure If it decreases gas is probably leaking at the fitting Tighten the fitting Then check t...

Page 27: ...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 Detachab...

Page 28: ...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 2 12...

Page 29: ...the flexible tubing at any degas station that will be used for flowing gas preparation Attach the tube by pressing the flexible tubing completely over the ferrule at the end of the gas delivery tube...

Page 30: ...the accessories kit Attach a fitting to the flexible tubing at any degas station that will be used for vacuum or vacuum backfill sample preparation Press the flexible tubing completely over the barbe...

Page 31: ...ncluded in the accessories kit through the opening on the back of the degasser and into the slot on the adjustment screw To confirm the accuracy of the vacuum pump gauge attach an independent gauge to...

Page 32: ...osition and move the sample tube to a cool ing station 6 After the sample tube has cooled sufficiently immerse the lower two thirds of the tube into a liquid nitrogen bath 7 The resulting sorption pum...

Page 33: ...o cause burns after the sample has been heated Wear the cotton gloves supplied in the accessories kit and handle the fitting carefully to avoid burns CONTROL THE TEMPERATURE OF THE HEATING STATIONS Us...

Page 34: ...Rubber gloves or clean lint free cloth n Safety glasses n Sample tubes n Sample tube brush n Sample tube rack n Sample tube stopper n Funnel n Ultrasonic cleaning unit n Waste container n Safety glass...

Page 35: ...water may be used 8 Stand the sample tubes on the sample tube rack and place the filler rods in a basket or in the rack Bake in a vacuum oven for two hours at 110 C Samples tubes can also be cleaned w...

Page 36: ...ed air 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...

Page 37: ...ed with forceps Analysis results are expressed in units of surface area per gram of sample therefore it is important to know the true sample mass Follow the instructions on the Sample Data Worksheet a...

Page 38: ...t fits inside the sample tube to keep the inside wall of the sample tube clean Balance 9 On the Sample Data Worksheet record the following n Mass of the sample tube set with the sample n Subtract the...

Page 39: ...from Micromeritics The adapters used with Gemini sample tubes may remain in the stations until a different type of sample tube is needed The adapters used with the TriStar and ASAP Series sample tubes...

Page 40: ...3 8 or 1 2 in stem 1 2 in 30 mm bulb Part number 060 25850 00 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 He...

Page 41: ...el Sample Tubes Adapter Model TriStar Flex 1 4 3 8 1 2 in 9mm 12mm stem Part number 060 25850 00 Heating Station Adapters continued Heating Station Adapters VacPrep Operator Manual 061 42802 01 Rev B...

Page 42: ...lied in the accessories kit Insert Adapters 1 Place the adapter over the sample tube 2 Hold both the adapter handle and sample tube stem when placing the sample tube and adapter in the heating station...

Page 43: ...e in a cooling station After the sample tube has been installed on the analyzer place the adapter back into the heating station for storage TriStar and ASAP Series Sample Tubes VacPrep Operator Manual...

Page 44: ...fore inserting the sample tube An adapter may be inserted into the heating station with either end in the upward position To insert the adapter insert the tool into the adapter so that the pronged tip...

Page 45: ...Adapters Adapters for the Gemini may remain in the heating station when not in use If removing the adapter use the adapter tool Gemini Sample Tubes VacPrep Operator Manual 061 42802 01 Rev B Apr 2021...

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Page 47: ...isture and other contaminants This method should be used only with materials which are not likely to fluidize n Vacuum backfill preparation The sample is heated as a vacuum is alternately applied and...

Page 48: ...sure that the vacuum pump is powered ON and that gas is being supplied to the degasser 2 Attach a vacuum fitting to each piece of flexible tubing at a degas station to be used for sample preparation 1...

Page 49: ...sample If the analyzer begins to pull sample material out of the tube imme diately turn the VAC GAS control knob to the OFF position 9 When the vacuum gauge reads 100 millitorr 100 mHg or less turn th...

Page 50: ...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 14 When the sample has sufficiently cooled turn the VAC GAS cont...

Page 51: ...on and if necessary then be subjected to vacuum preparation If sample has been accidentally sucked into the instrument see Clean and Replace Vacuum Fittings on page 5 13 1 Turn all VAC GAS control kno...

Page 52: ...and turn the VAC GAS control knob to the GAS position 11 Allow gas to flow into the sample tube for 5 to 10 seconds 12 If preparing other samples on the degasser which are not to be evacuated turn the...

Page 53: ...ation until the next sample is attached 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 we...

Page 54: ...ion A Cooling stations B Degasser stations C VAC GAS control knobs D Vacuum gauge E Temperature controller 4 Wipe the gas delivery tube with a clean lint free cloth to remove any residue left from the...

Page 55: ...avoid burns 6 Insert the stopper loosely into the sample tube The stopper helps prevent cool moist air and dust from entering the tube but it must be inserted loosely to allow a path for the escaping...

Page 56: ...ace area Repeat this process until the surface area no longer increases The length of time required to reach this point is the minimum amount of time required to degas the sample 9 After the sample is...

Page 57: ...ol knob in the OFF position 14 Wipe the gas delivery tube with a clean lint free cloth to remove any particles of sample that may have adhered to it Then place the gas delivery tube in a cooling stati...

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Page 59: ...t sufficient personnel are available to assist in moving the instrument The VacPrep weighs approximately 10 kg 22 lb Use of a power cord or power supply not provided with the instrument could cause pe...

Page 60: ...maged or disconnected Action B Contact the appropriate service personnel A newly installed fuse is blown Cause A Line voltage is too high Action A Check the line voltage See Select Input Power on page...

Page 61: ...ol valve is damaged Action F Contact the appropriate service personnel Vacuum reading too high Cause A Vacuum pump is powered off Action A Power on the vacuum pump Cause B Vacuum tubing leak Action B...

Page 62: ...ntenance Action H Close all valves to verify proper operation of the vacuum pump PARTS AND ACCESSORIES Parts and accessories can be found online at www Micromeritics com 5 4 VacPrep Operator Manual 06...

Page 63: ...he heating stations to cool prior to servicing Protective measures for these risks n Electrical The majority of electrical components operate at low voltage 24V or less and pose low risk when energize...

Page 64: ...ted power line Other devices such as motors generators or ovens should not be placed on the same power line Replacement power supply cords must be rated for the specifications stated above CLEAN THE I...

Page 65: ...in the beaker of water If bubbles appear the problem is a clogged gas delivery tube If the tube cannot be unclogged replace it with a new one If bubbles do not appear check the valve inlet tubing Gas...

Page 66: ...min is the maximum flow rate that would generally be used in normal operation Do not exceed 5 psi regulator pressure when backfilling sample tubes If the gas pressure is greater than the recommended m...

Page 67: ...d or damaged it should be replaced A Flexible tubing B Ferrule C Gas delivery tube 1 Remove the gas delivery tube from the flexible tubing 2 Attach a new gas delivery tube by pressing the flexible tub...

Page 68: ...nance REPLACE FLEXIBLE TUBING 1 Remove the flexible tubing from the barbed fitting on the front panel 2 Attach new flexible tubing Barbed fitting Flexible tubing installed 5 10 VacPrep Operator Manual...

Page 69: ...e of the spokes on the manifold If it is disconnected at either end connect it by pressing firmly into place If a spoke on the man ifold is loose tighten it finger tight plus 1 2 turn with a wrench Do...

Page 70: ...nce REPLACE THE VACUUM FITTINGS 1 Remove the flexible tubing from the barbed fitting on the front panel 2 Attach new flexible tubing Barbed fitting Flexible tubing installed 5 12 VacPrep Operator Manu...

Page 71: ...d ferrule for 3 8 in or 9 mm sample tubes 2 To clean 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 Ens...

Page 72: ...Port nipple 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 a...

Page 73: ...ervice Representative every 12 months Maintenance Required Frequency Vacuum fittings Clean after each use and replace as needed Vacuum gauge Calibrate when the electrical supply voltage or frequency i...

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Page 75: ...isplayed if it is increasing If the tem perature does not increase the message will remain displayed Power off the instrument and contact the appropriate service personnel uuuu Cause Temperature has r...

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Page 77: ...ss of empty sample tube set g 2 Mass of sample tube set plus sample g g g 3 Mass of sample step 2 minus step 1 g g g Degas Information Degas apparatus Temperature C Time hours Actual time started Actu...

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Page 80: ...2 9 S safe servicing 5 5 sample mass determine 3 5 preparation 3 1 INDEX A about this manual v ASAP Series sample tubes 3 10 C clean filler rod 3 2 sample tubes 3 2 contact us iv corporate profile ii...

Page 81: ...maintenance preventive maintenance 5 15 tubing flexible attach 2 12 tubing replace flexible 5 10 U unpack and inspect 2 1 V VacPrep about 1 1 specifications 1 3 vacuum backfill preparation VacPrep 4...