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PET Plus Viscometer User Manual

1. Fit the top cap to the top of the barrel and tighten securely using the tightening tool to seal the barrel Press the key under FULL to apply the nitrogen gas to the barrel Wait until the gas can be heard flowing freely through the die noting that the sound will change when the die is clean Press the key under GAS OFF to release the gas pressure check that the display shows nominally zero then remove the top cap using the tightening tool 7 6 PURGE THE BARREL WITH NITROGEN GAS Press the key under PURGE to allow a low volume of nitrogen gas to flow through the barrel to displace any air that may be present Allow the gas to flow for a few seconds to ensure that the barrel is full of nitrogen PET Plus User Manual 45 7 7 INSERT THE POLYMER INTO THE BARREL Note that this part of the procedure must be carried out as quickly as possible to prevent the polymer from being affected by moisture and so achieve the correct IV value Please refer to the relevant sections that show how to prepare the sample then transfer it into the barrel m Place the relevant filling funnel onto the top of the barrel m Press the key under GAS OFF to stop the flow of nitrogen gas E Insert the polymer into the top of the filling funnel m Remove the filling funnel from the top of the barrel m Insert a clean follower into the top of the barrel m Push the charging tool into the top of the barrel E Immediately press the green GO key to start the tes
2. Ring must now be fitted into the die recess by inserting the die with the O ring into the wide end of the contraction taper tool and gently pushing it with the cleaning tool until it emerges from the narrower opening PET Plus User Manual 77 14 2 CLEANING THE DIE RETAINING NUT Normally the die retaining nut does not require cleaning unless there has been a leakage of molten polymer past the die O ring or the extrudate has lipped back and coated the underside of the nut Molten polymer can be removed by wiping with a piece of cleaning cloth when the nut is hot If the die retaining nut becomes completely encrusted with polymer then the nut should be burned off in a similar fashion to that described for the followers The sealing ring in the top of the die retaining nut should protrude above the level of the metal holder When worn down remove the old washer by levering it out via the slot cut into the top of the nut Place the new washer into the circular recess around top of nut and press down firmly until washer is evenly embedded 14 3 SERVICING THE POLYMER CHIP GRINDER Clean the grinder bowl and funnel using a vacuum cleaner or by hand using a soft brush and cleaning cloth Check that the lubricator on the air regulator set contains a suitable quantity of the correct grade of oil e g Shell Morlina 10 or Tellus R10 Rotate the silencer cover on the rear of the grinder slightly anti clockwise then remove the cover
3. If the pressure is too low increase it using the pressure regulator on the right hand side of the equipment If the pressure is too high rotate the pressure regulator on the right hand side of the equipment anti clockwise press the key under GAS OFF to release the pressure then press the same key now labelled GAS ON to re apply the pressure Finally increase the pressure using the pressure regulator to give the required value Note that if the GO key is not pressed within one minute after the Fit probe then press GO message is displayed then the test will end and the warning screen below will be displayed ERROR Condition Test Ended Probe Not fitted Press ENTER to Continue PET Plus User Manual 47 7 10 WAIT UNTIL THE TEST HAS FINISHED The test is now running The Pre Conditioning part of the test allows the sample to heat up and become fluid and so start to flow through the die The pre conditioning ends 3 minutes after the sample was first inserted into the barrel then the Speed Check screen is displayed Set Temp 295 0C Barrel Temp 295 0C Pressure 24 35Bar Probe Speed 0 522 Gas Off The Probe Speed should initially be between 0 5 and 1 0 mm min and this is determined by the IV of the polymer and the applied gas pressure A high IV polymer will require a high gas pressure and a low IV polymer will require a low gas pressure Set Temp 295 0C Barrel Temp 295 0C Pressure 18 75Bar Probe Speed 0
4. PET Plus User Manual 11 2 0 EQUIPMENT AND ACCESSORIES 2 1 PET PLUS AND ACCESSORIES The PET Plus is supplied with the following tools and accessories 1 Top Blanking Nut and PTFE Sealing Washer p n 778 98 amp 778 99 HO Used during die cleaning and pressure testing 2 Follower p n 750 45 Follows the movement of the polymer down the barrel during extrusion O a 3 Contraction Taper Tool part of p n 750 41 r Used to fit a new O ring to the die 4 Expansion Taper Tool part of p n 750 41 _ Used to fit a new O ring to the die ake 5 Tightening Tool p n 778 35 i Used to fit and remove the die retaining nut top blanking nut and bottom blanking plug 6 Barrel Cleaning Tool p n 778 55 Used to charge the sample push a clean ing cloth down the barrel and for die O ring fitting 7 Die Retaining Nut and Fibre Sealing Washer p n 778 53 amp 778 54 Secures the die in the barrel 8 Die and PTFE O Ring E p n 778 82 amp 750 1019 Certified die used for extrusion testing 12 PET Plus User Manual Shown PET PLUS with Probe attached 9 Bottom Blanking Plug and PTFE Sealing Washer p n 778 51 amp 778 52 Used during pressure testing 10 Standard Filling Funnel p n 778 50 Used for loading dry gra
5. Part No 01 3514 AMETEK November 2014 TEST amp CALIBRATION INSTRUMENTS PET Plus Viscometer including Polymer Dryer and Polymer Grinder User Manual Davenport ne polymer test equipment WARRANTY This instrument is warranted against defects in workmanship material and design for one 1 year from date of delivery to the extent that AMETEK will at its sole option repair or replace the instrument or any part thereof which is defective provided however that this warranty shall not apply to instru ments subjected to tampering or abuse or exposed to highly corrosive conditions THIS WARRANTY IS IN LIEU OF ALL OTHER WARRANTIES WHETHER EXPRESS OR IMPLIED AND AMETEK HEREBY DISCLAIMS ALL OTHER WARRANTIES INCLUDING WITHOUT LIMITA TION ANY WARRANTY OF FITNESS FOR A PARTICULAR PURPOSE OR MERCHANTABILITY AMETEK SHALL NOT BE LIABLE FOR ANY INCIDENTAL OR CONSEQUENTIAL DAMAGES INCLUDING BUT NOT LIMITED TO ANY ANTICIPATED OR LOST PROFITS This warranty is voidable if the purchaser fails to follow any and all instructions warnings or cautions in the instrument s Instruction Manual If a manufacturing defect is found AMETEK will replace or repair the instrument or replace any defec tive part thereof without charge however AMETEK s obligation hereunder does not include the cost of transportation which must be borne by the customer AMETEK assumes no responsibility for dam age in transit and any claims for such damage shou
6. QTY Description Part No 1 Probe Rod 750 1042 1 Probe Calibration Tool 750 35 1 Probe Repair Kit 778 103 1 Chip Transfer Vessel Repair Kit MT CON CTV 2 11 OPTIONAL EQUIPMENT Not Supplied by AMETEK COMPUTER A computer with the minimum specification as stated below will be required if the optional NEXYGEN Plus software is to be used e 2GHz Pentium III or better e RAM 256MB or more e Monitor resolution 1024 x 768 or higher e CD ROM drive e Unused COM Port with a 16550 UART e Microsoft Office 2000 or later for reports 3 0 INSTALLATION CAUTION The Viscometer and Polymer Grinder are heavy instruments Great care must be taken when lifting the equipment EMPLOY SAFE LIFTING PRACTICES Use lifting equipment and or two persons to lift the equipment into position Do not position hands or fingers so that they may become trapped 3 1 CONSIDERATIONS Consideration should be given to the following before starting to set up the supplied equipment 1 The location and strength of the bench where the equipment is to be used The bench must be strong enough to support the equipment without deforming and be solid enough not to vibrate Consider that The Viscometer weighs 34Kg The Polymer Grinder weighs 41Kg The Polymer Dryer weighs 15Kg e The weight of the optional computer system Plus when cleaning the barrel of the Viscometer a large proportion of the operator s weight may be applied to the top of the
7. 1 5 2008 To change the Day press the key under SET DAY To change the Month press the key under SET MONTH To change the Year press the key under SET YEAR Press the ENTER key to return to the UTC TIME screen 32 PET Plus User Manual Press the ENTER key to return to the second Global Options screen Press a key to change a parameter UTC Local Data Time Time Format To set the difference between Local Time and UTC press the key under LOCAL TIME Set the Local Time Local Time 14 52 01 05 2008 1HR 1 2HR 1 2HR 1HR Press the relevant keys to set the time offset then press the ENTER key Press the key under DATA FORMAT Press a key to change a parameter Std Decimal ASCII Export Dev n Separator Delimiter Test Name n Dot Tab No Each of the options toggle when the relevant key is pressed The STD DEV N has options of n and n 1 The Decimal Separator has options of Dot and Comma The ASCII Delimiter has options of Tab and Comma The Export Test Name has options of Yes and No Select the required options then press the ENTER key to return to the second Global Options screen Press the key under lt to display the first Global Options screen Press a key to change a parameter Change Current Password Language Calibrate lt None gt English Mode PET Plus User Manual 33 4 2 OVER TEMPERATURE DEVICE Asecondary temperature measuring device is fitted to protect the
8. 74 1 9 7 6 1 1 7 8 7 9 7 10 7 11 7 12 7 13 7 14 i190 8 0 9 0 9 1 9 2 9 3 9 4 9 5 9 6 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 11 0 11 1 11 2 11 3 11 4 11 5 11 6 12 0 12 1 12 2 12 3 12 4 Page TRAINING MODE ccccceccseeseeeeeeees 41 Selecting Training Mode scsecceeeeees 41 PERFORMING ATEST cccceceeeeees 42 Selecting the Required Test Setup 42 Test PFOCEQUIG i c ostucciitanonuactdnannaurrodinnrenancsson 44 Check that the Barrel is Clean 00 00 44 Prepare Follower and Funnel 008 45 Clean the Die Bore ccccseeeeseereeees 45 Purge the Batrel ccscssssssssseesessseerees 45 Inserting Polymer into Barrel ccee 46 Apply Pressure to Barrel ccccecseeeees 47 Fit Probe to Batre icsstacuatssisttiiuatpindebeinadiradasni 47 Wait Until Test has Finished ccccee 48 Cleaning the Barrel cccsssesessseereeres 50 Cleaning the Die Bore ccsssseeeeees 51 Storing the DIS siessen 51 Cleaning the Followers cssssesseeeees 51 Viewing Previous Test Data cece 53 SAMPLE PREPARATION 0000 56 SUPPLIED PET GRANULES 57 Testing Principles vcicosinsrscauciasnsvansscnsircasdsisesuans 57 Polymer MING sccctstrccietniiteriasictasnaninaadentede dean 57 CRIP S ZE visserie nieren ei 58 Drying Principle cs
9. 86 20 8363 4768 lloyd ametek com cn Information in this document is subject to change without notice 2014 by AMETEK Inc www ametek com All rights reserved
10. Place each phial into the storage area at the sides of the polymer drier then push each of the metal tubes into a quick release connector along the top of the drier Note that the tube clicks into place in the connector and cannot be pulled out again until the release lever is pressed Check that each of the vacuum valves is open lever is in line with the vacuum pipe Wait for 5 minutes to ensure that a good vacuum is applied to the samples then place each of the phials into the heated block This is to ensure that the polymer is not initially heated when air and or moisture is present in the tube The samples MUST be dried for a time period between 16 and 24 hours A typical procedure is to place the samples in the drier at say 4PM so that they are ready for testing the next morning from 8AM onwards At the end of the drying time remove the phials from the heated block and place in the storage areas at the sides of the polymer drier WARNING Hot tubes Wear Heat Protective Gloves Note that the plastic tubes MUST still be attached to the quick release connectors and the vacuum pump MUST be left running Dried samples of polymer can remain in the parking area for up to 24 hours before testing with the vacuum pump running Therefore a number of samples from 1 to 6 can be dried at the same time 9 6 TESTING THE POLYMER NOTE It is very important that the Die the Barrel and the Follower are scrupulously clean wy and have been as
11. True Pressure 30 0Bar Measured Pressure 29 7Bar Change Clear True Accept Points Cancel Press the key under CHANGE TRUE then enter the pressure measured by the reference pressure gauge e g 29 9Bar The display will now show the entered value for the true pressure Press the key under ACCEPT to correct the pressure reading Nitrogen Gas is ON Measured Pressure 29 7Bar Gas Cal View View off Point Points Readings If a calibration point had already been entered at 30Bar or approx this value a warning message will be displayed Press the key under OVERWRITE POINT to accept this new calibration point Press the ENTER key to return to the Pressure Calibration screen Press the key under GAS OFF to release the pressure inside the barrel Rotate the pressure regulator on the right hand side of the equipment fully anti clockwise Press the key under GAS ON to re apply the pressure Adjust the pressure inside the barrel using the pressure regulator on the right hand side of the equip ment and check the readings at approx 5Bar 10Bar 15Bar 20Bar and 25Bar PET Plus User Manual 87 If any of the readings differ from the true pressure measured on the reference pressure gauge by more than 0 1Bar add a calibration point as shown earlier Finally press the key under GAS OFF to release the pressure inside the barrel 15 4 PROBE CALIBRATION Note that a special probe calibration tool part number 750 35 is required for th
12. 0 78 and 0 82 Note that BOTH limits MUST be defined Column Properties BIE Column Properties apes Title Appearance Format Limits Statistics New Test Title Appearance Format Limits Statistics New Test Column Title g pem C No Limits C Relative to Nominal Set to default fo 789328622 7 fio Z Within Range 78 Cancel Apply Cancel Apply Click on the OK button to close the dialog and display the data table in colour Any rows shown in green pass the PASS FAIL parameters and any rows shown in red fail the parameters Pet Plus Tests batch PET Plus User Manual 101 The statistics can be viewed by clicking on the STATISTICS Tab at the bottom of the screen y Pet Plus Tests batch p loj x Maximum Minimum Mean Median Coefficient Standard Standard of Variance Deviation N Deviation N 1 M at zero 0 805 0 787 0 794 0 793 0 861 0 006 0 007 Degradation factor 0 003 0 004 0 004 0 004 12 26 0 000 0 000 MM 600 00 534 00 561 00 557 00 408 22 876 25 060 Number of Rows that Passed 6 Number of Rows that Failed O Results Graph statistics r BarRange Histogram i 6 Rows 4 The XBAR RANGE and or HISTOGRAM charts can also be viewed Note however that 10 or more rows are normally required to view the XBAR RANGE chart because this normally groups the test results into groups of 5 rows Note that the XBAR RANGE and HISTOGRAM charts can ONLY b
13. 25 04 2008 11 51 No 2 No 11 To view the data for any other test select the test using the keys Note that the inner 2 keys move through the data one test at a time and the outer 2 keys move through the data 10 tests at a time The screens below show tests number 11 and 2 Test No 11 of 12 Select using keys IV Degrad n Date Time 0 801 0 011 25 04 2008 10 13 No 1 No 10 No 12 Test No 2 of 12 Select using keys IV Degrad n Date Time 0 799 0 011 20 04 2008 13 52 No 1 No 3 No 12 Press the key under STATS to view the test statistics Note that a warning message will be displayed if there is no data present for this test set up There is no data for this test setup Press ENTER to continue 54 PET Plus User Manual The Statistics screen shows the Mean and Standard Deviation values for the IV and the Degradation Factor together with the number of samples used to calculate the statistics Note that the Standard Deviation uses either the n or the n 1 formula as selected in the GLOBAL options The data can be exported using the supplied RS232 cable to HyperTerminal etc The RS232 protocol is 9600 Baud Rate 8 Data Bits 1 Stop Bit and No Parity To export the data press the key under EXPORT IV Degrad n Samples Mean 0 0798 0 011 12 Dev n 0 015 0 003 Export Reset The test results and statistics can be erased form the internal memory by pressing the key under RESET A confirmatory screen will be disp
14. 81 14 9 CHANGING A DAMAGED PROBE ROD If the probe rod becomes damaged and will no longer slide freely inside the probe bush then it must be replaced as shown below Loosen the grub screw securing the probe bush to the main body of the probe then unscrew and remove the probe bush Remove the probe rod and replace with a new one Re assemble the probe then calibrate as shown in the calibration section The part number of the probe rod is 750 1042 A probe repair kit is also available part number 778 103 82 PET Plus User Manual Shown Probe 15 0 CALIBRATION 15 1 SELECTING THE CALIBRATION MODE Display the Select Test screen to display one of the pre defined test set ups Select the required test 20THOU_ 284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit Press the key under EDIT to display the edit test screen Press a key to select an option 20THOU_284C Rename Global Delete Setup Press the key under GLOBAL to display the first Global Options screen Press a key to change a parameter Change Current Password Language Calibrate lt None gt English Mode Press the key under CALIBRATE MODE to display the Calibration screen Calibration Mode Cal Cal Cal Temp Pressure Probe PET Plus User Manual 83 15 2 TEMPERATURE CALIBRATION Note that an accurate reference thermometer is required for this procedure The barrel temperature is calibrated by measurin
15. EN 61326 1 2013 Electrical Equipment for Measurement Control and Laboratory use General Requirements This declaration of conformity is the result of testing and evaluation performed by Ametek Inc and Product Safety Engineering LLOYD is a brand name owned by Ametek Inc USA SIGNATORY David orter Division Vice President Engineering amp Operations Ametek Inc 8600 Somerset Drive Largo Florida 33773 USA 805 595 5477 or Email david porter ametek com or FAX 805 595 5466 Document ER 444 EUROPEAN SIGNATORY Lik del Frie Division Vice President amp Business Unit Manager Ametek Inc Gydevang 32 3450 Lillerod Denmark 45 48168031 or Email joel frie ametek com or FAX 45 48168080 mrt KULA ax EA S ST reo Certificate Number 1918 04 PET Plus User Manual 5 1 0 INTRODUCTION 000 8 1 1 General Eee enn eon re ent meme 1 2 ECUIDIIG IN i sscsasscaierassinnencocesicntenacearont 1 3 Equipment Operation ccccce 1 4 Uses of the Equipment 06 1 5 Measurement Range cccee 1 6 Advantages of the PET Plus 2 0 EQUIPMENT amp ACCESSORIES 2 1 PET Plus and Accessories 2 2 Consumable Items cccseeeees 2 3 Polymer Drier and Accessories 2 44 Vacuum PUMP 2 5 Polymer Chip Transfer Vessel 2 6 Sample Melt Pop uu 2 7 Polymer Chip Grinder 0 cc00 2 8 Industrial Grinder si ccintitGninaetnicsnincn
16. Note that the third line alternates between the Date and Time display and the Barrel Temperature Select the required test 20THOU 284C 0 Samples Barrel Temperature 295 0C Select gt Edit Also note that the barrel heaters are not switched on until either the key under SELECT is pressed or the PC software is started The heaters are then active and the barrel will heat and maintain the required test temperature until the equipment is switched off The required test temperature is specified either in the test set up as shown earlier or in the PC Test set up Press the key under gt or lt to select the test set up that is to be used for the sample testing When the required test set up is displayed press the key under SELECT to display the Analysis screen Set Temp 295 0C Barrel Temp 295 0C Pressure 0 OBar Probe 15 85mm 20THOU_295C Test Results Stats Suspend 42 PET Plus User Manual Press the key under TEST to display the Pre Test screen Set Temp 295 0C Barrel Temp 295 0C Pressure 0 OBar Probe 15 85mm Insert sample follower then press GO Gas Off Purge Full Exit Note that the Pre Test screen will NOT be displayed if the probe is not electrically connected to the probe socket on the rear of the vertical column If the probe is not connected the warning screen below will be shown ERROR CONDITION Probe NOT Connected Press ENTER to Cancel Also note that the intermediate screen sho
17. Polymer Grinder Setting up maintenance and service should only be carried out by trained technicians or service personnel WARNING The blades of the Polymer Grinder rotate at very high speeds Therefore they continue to rotate for a few seconds after the timer has operated or the Timer Valve knob is pulled WAIT FOR 5 SECONDS BEFORE OPENING THE GRINDER AFTER IT HAS BEEN SWITCHED OFF NOTE THAT PULLING THE TIMER VALVE KNOB FORWARDS STOPS THE GRINDER AT ANY TIME 62 PET Plus User Manual Release the clip at the front of the grinder and lift the lid Note that for safety the blades CANNOT rotate when the lid is lifted Ensure that the grinder blade grinding bowl with slits collecting funnel and collecting bowl are thoroughly clean The recommended way to clean these items is by using a vacuum cleaner and or by hand using a soft brush Weigh out 20 to 30g of polymer which can be in the form of cube cut masson cut or lace cut material and place into the grinding bowl with 0 5mm wide slits Place a clean receiving bowl under the funnel at the front of the grinder to collect the ground sample Place the filled grinding bowl centrally in the top of the cleaned collecting funnel of the grinder Using a suitable container pour liquid nitrogen into the grinding bowl until the level of the liquid is about 1cm or 1 2 above the polymer chip level Shown 0 5mm Grinding Bowl WARNING ALWAYS WEAR SAFETY GLASS
18. SUPPLIED PET GRANULES 9 1 TESTING PRINCIPLES The polymer must be dried using the polymer drier and vacuum pump both of which are optional extras When the polymer is dry it MUST be transferred to the PET Plus barrel using a procedure that ensures that the polymer does not come into contact with any external air gt NOTE Drying time is a function of both temperature and vacuum A lt 0 1mm Hg vacuum is essential 9 2 POLYMER DRYER Shown Poymer drier The Polymer Dryer has been designed for drying PET and other hygroscopic materials and incorporates the following features 1 Atemperature controlled heated block that has been machined to hold and heat six sample phials The temperature controller can control the temperature from ambient to 200 C 2 C 2 Six quick release valves at the top of the unit to connect each sample phial to the vacuum supply 3 Two Storage or Parking areas to hold six sample phials These areas are at the side of the heated block but are not heated They are provided to allow the dried samples to be stored under vacuum until required 4 An On Off Switch for the Vacuum Pump 5 Atimer settable from seconds to hours with an audible alarm This is mainly for use when drying polymer powder PET Plus User Manual 57 9 3 CHIP SIZE For optimum drying the chip size should be approximately 1mm diameter i e an average chip weight of 20mg Larger granules i e 40 mg and a
19. VesiMo Text Numerical Define as many questions as required noting x that each question can be configured to accept Basic Settings Festils ProTest Boolean True False Yes No etc text numbers or quantities numbers with units e g 10g as required C Miscellaneous Post Test PET Questions E Test Options _ Click on the RESULTS tab then click on the PET o el Icon to display the available test results sore I DAG Device Machine Settings OK Details Cancel x Basic Settings Results Pre Test mi Questions C Miscellaneous 2m Post Test c Questions IV Results Probe Speed Results Temperature Results Test Options _ Test Automation ei Video Capture ie DAG Device m Machine Settings _ OK Details Cancel Click on the required result title e g IV Results xl to display the available results Calculable Results Details OW at zero O Degradation factor O mv Select the required results using the checkboxes Note that the selected results can be modified at any time after the test has been performed Click on the OK button 2 times to close the TEST CONFIGURATION screen PET Plus User Manual 97 16 6 PERFORMING A TEST Click on the OPEN AN EXISTING BATCH button on the Welcome screen Note that if the Welcome screen is not displayed it can be displayed by clicking on the 9th Icon from the left on the toolbar An OP
20. a non return valve The second chamber has a 5 PSI 0 35Bar pressure release valve The dispensing mechanism has an adjustable bore to preset the volume of polymer that will be dispensed with each operation of the dispensing lever The transfer vessel will keep enough granules dry for up to ten tests and dispense the correct amount required for each test 3 8g Add polymer to the top chamber 5 pis pressure relief valve Surplus gas will discharge from this Dispensing lever valve Schader quick release valve Nitrogen gas inlet PET Plus User Manual 69 11 3 CHECKING THE DISPENSED VOLUME The transfer vessel should be adjusted so that 3 8g of polymer is dispensed when the dispensing lever is turned Remove the top cap cap on larger chamber from the transfer vessel then half fill the chamber with polymer Refit the top cap then remove the bottom cap Place a container on the bench then hold the transfer vessel upright over the container Turn the dispensing lever until the lever is pointing upwards This allows the polymer to enter the dispensing mechanism Turn the dispensing lever until the lever is pointing downwards This will dispense a quantity of polymer into the container Weigh the dispensed polymer and check that it weighs 3 8g 0 1g If the weight is not correct the dispensing mechanism must be adjusted 11 4 ADJUSTING THE DISPENSED VOLUME The dispensing mechanism contains a central
21. batch statistics can be viewed either as a data table an X Bar Range chart or a Histogram The NEXYGEN Plus PET program can print test graphs SPC charts and simple test reports with statistics from its built in statistical and print features and can also produce custom reports when used together with Microsoft Word 2000 or later Therefore Microsoft Word SHOULD be installed on the computer and it is HIGHLY RECOMMENDED that Office 2000 or Office XP or later is installed if data is to be exported to Microsoft Excel and or Microsoft Access 16 2 ADVANCED SECURITY The NEXYGEN Plus PET software has an optional Security and Audit Trail Feature which can be configured to prevent unauthorised personnel from using the software The benefits of the security features are that the Quality Manager can define the controlled tests required for the QC or test department and only authorised operators can perform these tests Whenever a test or sequence of tests is to be performed the operator has to log on to the software using a previously specified log on name and user password This logging on and off is stored in a separate audit database which can be viewed by the Quality Control manager to monitor who has been performing the tests This ensures that only trained operators can perform tests so minimises the chances of the test being incorrectly performed and incorrect data being reported The NEXYGEN Plus PET also enters the log on na
22. from the studs SILENCER COVER pa Carefully remove the foam element from the end of the silencer then wash thoroughly in paraffin Dry the foam element then refit onto the end of the silencer Refit the silencer cover Shown Silencer cover Shown Foam element in Silencer 78 PET Plus User Manual 14 4 TENSIONING THE DRIVE BELT The polymer grinder blade is driven by an air motor via a smooth drive belt A smooth belt is used to allow the belt to slip if the blade contacts a solid material The drive belt may become loose after an extended period of time and may slip under normal operation To check the belt tension the top cover has to be removed from the top of the polymer grinder To remove the top cover first remove the silencer cover from the rear of the grinder by twisting anticlockwise by a few degrees then lifting away Remove the foam element and the rubber seal from the end of the silencer Unscrew the brass silencer then pull out from the top cover Unscrew and remove the two 2 domed nuts and washers securing the top cover to the main lid assembly Lift the top cover away from the lid assembly Check that the belt can be twisted by 90 degrees between the two 2 pulleys If the belt can be twisted by more than 90 degrees it must be tightened The motor is held in an eccentric boss so that the motor position can be moved closer or further away from the blade spindle Screw t
23. is the result of testing and evaluation performed by Ametek Inc and approved CE testing laboratories LLOYD is a brand name owned by Ametek Inc Division Vice President Engineering Ametek Inc 8600 Somerset Drive Largo Florida 33773 USA 727 538 6026 or Email douglas tilghman ametek com or FAX 727 535 4391 Document ER 440 EUROPEAN SIGNATORY 6 30 74 oel Frie Division Vice President amp Business Unit Manager Ametek Inc Gydevang 32 3450 Lillerod Denmark 45 48168031 or Email joel frie ametek com or FAX 45 48168080 id i Goruhgate Huimin Ot 4 PET Plus User Manual AMETEK MEASUREMENT amp CALIBRATION TECHNOLOGIES DIVISION EUROPEAN DECLARATION OF CONFORMITY NAME ADDRESS OF MANUFACTURER AND LOCATION OF TECHNICAL CONSTRUCTION FILE Ametek Inc 8600 Somerset Drive Largo FL 33773 USA PHONE 727 538 6084 FAX 727 535 4391 DESCRIPTION OF EQUIPMENT Product Ametek Polymer Dryer Device Models LLOYD 01 2776 amp 01 2777 Polymer Dryer LLOYD Effective Date November 14 2014 materials testing HARMONIZED STANDARDS USED A sample of this product has been assessed against the essential health and safety requirements of the Low Voltage and the EMC Directives listed below Based on conformity with the listed directives Ametek Inc declares the products mentioned above are in compliance with the following BS EN 61010 1 2010 Safety Requirement for Electrical Equipment BS
24. shows that the Security Feature is not enabled Click on the NEXT button to proceed The dialog shows the default program folder and this can be changed if required Select the Everyone option to create a Start Menu item for all users then click on the NEXT button to proceed Click on the NEXT button to install the main part of the program The dialog loading status bar will be displayed during the installation process fie NEXYGEN Plus PET 215 x Security and Audit Trail a Install the security database If ticked all users will be required to log in to use the software and functionality may be restricted by a supervisor I Security Enabled Cancel lt Back i fi NEXYGEN Plus PET Select Installation Folder The installer will install NEXYGEN Plus PET to the following folder To install in this folder click Next To install to a different folder enter it below or click Browse Folder C Program Files Lloyd Instruments Ltd NEXYGEN Plus PET Browse Disk Cost Install NEXYGEN Plus PET for yourself or for anyone who uses this computer Everyone C Justme Cancel Back i NEXYGEN Plus PET Confirm Installation The installer is ready to install NEXYGEN Plus PET on your computer Click Next to start the installation Cancel lt Back ip NEXYGEN Plus PET Installing NEXYGEN Plus PET NEXYGEN
25. 102 The Select Test screen will be automatically displayed after 3 seconds This screen is used to select one of the pre defined test set ups as shown later Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit Press the key under EDIT to set the date time and test result format Press a key to select an option 20THOU_284C Rename Global Delete Setup Press the key under GLOBAL to display the first Global Options screen Press a key to change a parameter Change Current Password Language Calibrate lt None gt English Mode The required language can be changed by repeatedly pressing the key under CURRENT LANGUAGE Press the key under gt to display the second Global Options screen PET Plus User Manual 31 Press a key to change a parameter UTC Local Data Time Time Format Press the key under UTC TIME Set the UTC Time 13 52 01 05 2008 Date Format Set Set DD MM YYYY Time Date To change the Time press the key under SET TIME Press a key to change a parameter set Set Hour Minute 13 52 To change the Hour press the key under SET HOUR To change the Minute press the key under SET MINUTE Ensure that the time is set to UTC GMT and NOT to the LOCAL TIME Press the ENTER key to return to the UTC TIME screen To change the Date press the key under SET DATE Press a key to change a parameter Set Set Set Day Month Year
26. 445 Probe Speed Slow Increase Pressure Gas Off If the Probe Speed is below 0 5 the equipment will beep and display the screen below to request that the gas pressure is increased Increase the pressure using the pressure regulator on the right hand side of the equipment until the probe speed is above 0 5 Set Temp 295 0C Barrel Temp 295 0C Pressure 18 75Bar Probe Speed 0 445 Probe Speed Slow Increase Pressure Gas Off If the Probe Speed is above 1 0 the equipment will beep and display the screen below to request that the gas pressure is decreased If the pressure is too high rotate the pressure regulator on the right hand side of the equipment anti clockwise press the key under GAS OFF to release the pressure then press the same key now labelled GAS ON to re apply the pressure Finally increase the pressure using the pressure regulator to give a probe speed below 0 7 Set Temp 295 0C Barrel Temp 295 0C Pressure 28 58Bar Probe Speed 1 005 Probe Speed High Decrease Pressure Gas Off 48 PET Plus User Manual Note that the probe speed MUST be set within the first 5 minutes after the sample was first poured into the barrel i e the soeed SHOULD only be altered when the bottom line of the display shows Gas Off Note that the gas pressure must NOT be altered for the rest of the test duration After 5 minutes of total test time the IV screen is displayed This shows the current IV value and this changes
27. 6 0 TRAINING MODE 6 1 SELECTING THE TRAINING MODE The predefined test set up called TRAINING is provided for operator training purposes This is to familiarise the operator with the test procedure and the equipment controls without actually testing a sample Display the Select Test screen Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit Press the key under gt or lt to select TRAINING Select the required test TRAINING 0 Samples Date and Time 29 05 2008 19 50 Select lt gt Edit Press the key under SELECT to display the Analysis screen Set Temp 295 0C Barrel Temp 295 0C Pressure 25 0Bar Probe 1 23mm TRAINING Test Results Stats Suspend This screen displays the requested barrel temperature the actual barrel temperature the nitrogen pressure within the barrel and the position of the probe rod Note that the training mode will automatically set the barrel temperature to 295 C the nitrogen pressure to 25Bar and repeatedly increase the position of the probe rod to simulate a real test Note that the barrel heaters are not powered when the training mode is selected PET Plus User Manual 41 7 0 PERFORMING A TEST 7 1 SELECTING THE REQUIRED TEST SETUP Display the Select Test screen to select one of the pre defined test set ups Select the required test 20THOU_295C 0 Samples Date and Time 30 05 2008 07 48 Select lt gt Edit
28. ACUUM POWER 0 wi 1 Place each phial into the storage area at the sides of the polymer drier then push each of the metal tubes into a quick release connector along the top of the drier Note that the tube clicks into place in the connector and cannot be pulled out again until the release lever is pressed Open each of the vacuum valves SLOWLY by turning the lever until it is in line with the vacuum pipe so that powder is NOT drawn up the plastic tube by the initial vacuum Wait for 5 minutes to ensure that a good vacuum is applied to the samples then place each of the phials into the heated block This is to ensure that the polymer is not initially heated when air and or moisture is present in the tube The samples MUST be dried for a time period of 50 minutes IV lt 0 7 or 55 minutes IV gt 0 7 If the timer is to be used press the START button on the front of the polymer drier The light in the top left hand corner of the timer will light A buzzer will sound at the end of the timer period if the timer was used Press the RESET button to stop the buzzer At the end of the drying time remove the phials from the heated block and place in the storage areas at the sides of the polymer drier WARNING Hot tubes Wear heat protective gloves when handling phials 66 PET Plus User Manual Note that the plastic tubes MUST still be at tached to the quick release connectors and the vacuum pump MUST be left running Dri
29. DUCTION TO THE PET PLUS VISCOMETER 1 1 GENERAL The PET Plus is a microprocessor controlled capil lary Melt Viscometer that is specifically designed to test the flow properties of PET The system can be used to test other polymers and because it does not require solvents it can also be used to test insoluble polymers It consists of a heated vertical barrel a calibrated die a small piston called a follower a displace ment transducer called a probe and control systems for the nitrogen gas flow and extruder temperature The equipment is based on a system developed by ICI It is designed for both research and quality control of polyethylene terephthalate PET which is hygroscopic and liable to degrade due to oxidation in the melt phase The apparatus Is recommended for use in the quality control of poly ester polymers to measure the Intrinsic Viscosity and degradation rates The Viscometer extrudes molten PET similar to an MFI but is specially developed to prevent the polymer from degrading due to contact with the atmosphere The polymer is isolated from moisture and oxygen because the barrel is sealed and the polymer is extruded through the die using pure nitrogen at high pressure Therefore an external supply of Nitrogen gas of 30 Bar pressure is required This nitrogen gas not only provides an oxygen and moisture free environment for the sample but also applies the extrusion force The quantity of polymer
30. EN dialog will be displayed as shown Select the required test file then click on the OPEN button Note that the above steps do not have to be performed if the test is run immediately after the test file has been defined as shown in the previous section The graph screen will be displayed as shown Click on the green START TEST button at the left hand side of the graph to start the test If any pre test questions have been defined a dialog will be displayed requesting the answers 98 PET Plus User Manual Welcome to NEXYGEN Plus NEXYGEN PLUS il B Create a New Batch of Tests Open an Existing Batch Create a New Query Open an Existing Query a Create New Batch from B Standards Library amp Print a Batch Report Vv Show this screen each time I Open 21x Look in Data O ft fi fe zs chris batch J i Test batch My Recent Documents Desktop My Documents wr My Computer T foe z amp E Files of type Batch Files batch 7 Cancel PETE I Open as read only u ss00rF w NAIR Se A Pind oH F e fo Bl Tort Typos D rem Test batch Goch ten For Helo brews Fi x Therm marked with an asterisk MUST contain answers abot Sample Type The display on the PET Plus will automatically change to the PC Pre Test screen Set Temp 295 0C Barrel Temp 295 0C Pressure 0 0Bar Probe 15 85mm Insert sample follower t
31. ES AND HEAT RESISTANT GLOVES WHEN HANDLING LIQUID NITROGEN WHICH IS AT 196 C PET Plus User Manual 63 Allow the liquid nitrogen to just evaporate to dryness then lower the grinder lid and lock with the clip Start the grinder by pushing the pre set timer valve fully inwards to give approximately 30 45 seconds grinding The grinder stops automatically to prevent over grinding and heat build up which could degrade the sample Wait until the grinding period has finished and the grinding blade has ceased to rotate Release the clip at the front of the grinder and lift the lid Shown Preset timer valve Lift the grinding bowl and shake it gently by hand until all the powder has been sieved out into the collecting bowl Pour more liquid nitrogen into the grinding bowl until the level of the liquid is about 1cm or 1 2 above the remaining polymer chip level Allow the liquid nitrogen to just evaporate to dryness then lower the grinder lid and lock with the clip Start the grinder by pushing the pre set timer valve fully inwards to give approximately 30 45 seconds grinding Wait until the grinding period has finished and the grinding blade has ceased to rotate Release the clip at the front of the grinder and lift the lid Lift the grinding bowl and shake it gently by hand until all the powder has been sieved out into the collecting bowl Continue the above procedure until most of the sample has been reduced t
32. POT This is a cylindrical metal block containing a PTFE insert and two tight fitting PTFE end caps The top of the pot has a longer stem and has a conical opening The bottom of the pot is shaped to fit onto the top of the PET Plus barrel WARNING Hot surface Wear heat protective gloves 12 3 USING THE SAMPLE MELT POT Before using the sample melt pot ensure that the top and bottom PTFE caps are a tight fit on the unit and that the sample melt pot is clean and dry Remove the top cap and using heat resistant gloves hold the pot under either a sample bleed point or as close as possible to the spinneret face or the die of the extruder to collect a sample of extrudate When filling from a bleed point allow the polymer to run into the pot until it is almost full then replace the top cap When filling from a spinneret the sample should be allowed to spill over the whole top portion of the pot Quickly trim off the excess polymer with a pair of scissors so that the sample is wholly contained in the hollowed top of the pot Withdraw the pot containing the sample and allow the sample to solidify a little forming a skin Push the polymer into the base of the pot using a suitably sized stainless steel rod the barrel cleaning tool Repeat the sampling procedure until the pot is almost full and then replace the top plug PET Plus User Manual 73 12 4 TESTING THE POLYMER NOTE It is very important that the Die the Barrel and the Fo
33. Plus PET is being installed Please wait PET Plus User Manual 93 When the NEXYGEN Plus PET has been installed a confirmation screen will be displayed as shown Click on the CLOSE button then the installer will automatically install the VBA components that are required for NEXYGEN Plus PET When the screen closes the NEXYGEN Plus PET program is installed To complete the configuration leave the CD in the drive then start the NEXYGEN Plus PET using the Windows Start button Ascreen similar to that shown will be displayed while the VBA is automatically configured 16 4 CONFIGURING THE SOFTWARE CON SOLE Connect the supplied RS232 cable part number 09 0639 between the rear of the PET Plus machine and an unused COM port on the computer Start the Software Console by clicking on the Windows START button then selecting NEXYGEN PLUS PET then selecting PET PLUS SERIES CONSOLE Right mouse click on the software console then select PORT SETTINGS Select the appropriate COM port then check that the console shows the Temperature Pressure and Probe Readings The NEXYGEN Plus program is now ready for use 94 PET Plus User Manual ix Installation Complete wy my NEXYGEN Plus PET has been successfully installed Click Close to exit Please use Windows Update to check for any critical updates to the NET Framework isual Basic for Applications R Core La Please wait while Windows co
34. T cccecccecteeeee 75 Testing Principles isicicecinwssits ean searpoiutatineadsisnunadanes T5 Industrial Grinder tiatssixasecnsseustrvssteemnatedamsmonars 75 Using the Industrial Grinder c cccceee 76 MAINTENANCE cccccecccceseeseteeeeeees lai Fitting a New O ring ccscsessssssssseeseeesees tf Cleaning the Die Retaining Nut 0 78 Servicing the Polymer Chip Grinder 78 Tensioning the Drive Belt ccceceeeee 79 Replacing the Drive Belt cesses 80 Result Discrepancies ccsessseescsseerees 81 Faults in Pressure System 81 Basic Electrical Checks cccsescecceeeerees 81 Changing a Damaged Probe Rod 82 CALIBRATION cccccseceesseessseeeeeees 83 Selecting the Calibration Mode 0 83 Temperature Calibration csecssssreeres 84 Pressure Calibration sccecssesssereerees 86 Probe Calibration srisicassatesierwstivacuauinasndasintatadien 88 NEXYGEN PLUS SOFTWARE 91 NEXYGEN PLUS PET wyccecsccscectesatteeccatterccdacs 91 Advanced Security scansidnscisnssdsivsesiasadunianssatiars 91 Installing the Software ecceeeseeeeeees 92 Configuring the Console 94 Creating a Test File cceessseseesseeeeees 95 Performing a TOS ssscccssescesssnceccctaaehetvantewennes 98 TECHNICAL SPECIFICATIONS 104 PET Plus User Manual 7 1 0 INTRO
35. V Mains In 115V AC 2 x T10AH250V Mains In 230V AC 2 x T10AH250V Mains In 115V AC 2 x T10AH250V 5 C to 35 C 20 C to 55 C must be substantially dry O to 80 non condensing 34kg 15kg 41kg 64cm high 94cm with probe fitted 47cm wide 42cm deep 45cm high with tubes fitted 36cm wide 45cm deep 40cm high 52cm high when open 40cm wide 54cm deep PET Plus User Manual 103 AMETEK TEST amp CALIBRATION INSTRUMENTS UK Tel 44 0 1243 833 370 uk far general ametek co uk France Tel 33 0 1 30 68 89 40 general lloyd instruments ametek fr Germany Tel 49 0 2159 9136 510 info mct de ametek de Denmark Tel 45 4816 8000 ametekdk ametek com International Symbols WEEE Directive This equipment contains electrical and electronic circuits and should not be directly disposed of in a landfill site oy RoHS 139 This product is RoHS and China RoHS compliant This symbol indicates the equipment contains some restricted hazardous substances above the recommended level and may offer potential harm to the environment after 15 years from date of manufacture USA Florida Tel 1 727 538 6000 chatillon fl lar ametek com California Tel 1 800 444 1850 sales crystalengineering net India Tel 91 22 2836 4750 ametekdk ametek com www lloyd instruments com Singapore Tel 65 6484 2388 ametekdk ametek com China Shanghai Tel 86 21 5868 5111 Beijing Tel 86 10 8526 2111 Guangzhou Tel
36. an irreversible break in the chain at the ester linkage which gives a drop in the IV Therefore the PET Plus can ONLY give the same IV as the solution method if ALL the moisture is removed from the polymer before it is tested less than 20ppm moisture The PET Plus is a semi automatic system so can be left unattended after the sample has been loaded and pre conditioned The test takes a total of 17 minutes after loading the sample 1 2 EQUIPMENT The equipment is fitted with a control console containing a blue 4 line by 40 character backlit LCD display and a membrane keypad The LCD can display the test set up test procedure and test results in various languages as selected by the user The equipment can be used stand alone or can be connected to a PC running the optional NEXYGEN Plus software When a test is performed in the stand alone mode the test results are stored using a Date Time ID that is created from the internal clock inside the equipment This internal clock has been set during the production process at Davenport Lloyd Instruments Ltd but should be checked during the initial installation Note that if the equipment is used with the NEXYGEN Plus PET software then the internal clock will be automatically synchronised to the PC clock when the software is connected to the equipment The internal clock always operates on UTC GMT time so the time displayed on the control console should be altered if the local time is no
37. assword protected to prevent unauthorised changes by non technical personnel This feature also prevents any stored test data from being erased Display the Select Test screen Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit Press the key under EDIT to display the edit test screen Press a key to select an option 20THOU_284C Rename Global Delete Setup Press the key under GLOBAL to display the first Global Options screen Press a key to change a parameter Change Current Password Language Calibrate lt None gt English Mode Press the key under CHANGE PASSWORD to display the password entry screen Change or create the password BkSp Clear All Enter the required password then press the ENTER key Please make a note of the password because the test set ups cannot be changed without entering the password PET Plus User Manual 39 If a password has been defined then the following screen will be displayed if the key under EDIT is pressed when the Select Test screen is displayed Enter the password to edit this test BkSp Clear All If the correct password is entered then the first Global Options screen is displayed otherwise the Select Test screen is re displayed Please contact your local agent distributor or Lloyd Instruments Ltd if the password is forgotten and a test set up is to be changed 40 PET Plus User Manual
38. barrel via the cleaning tools 2 The equipment should only be used in a well ventilated environment however the area needs to have a stable temperature and be draught free 3 The Viscometer requires an Oxygen free Nitrogen supply with lt 5ppm of water White Spot The Polymer Grinder requires a compressed air supply capable of delivering 16cfm 0 45m min at 80psi 5 5 Bar The Polymer Dryer requires a vacuum line capable of maintaining a 0 1mm Hg vacuum PET Plus User Manual 17 3 2 SAFETY CONSIDERATIONS 1 Before connecting the equipment to the mains supply make sure that it is marked with the voltage of the power supply to be used The Viscometer and its accessories are not adjustable for different supply voltages and must only be used on the supply that they were originally ordered for 2 There are 2 standard versions one for 230V ac 10 and the other for 115V ac 10 3 This equipment complies with electrical safety grade Class 1 which means that it is earthed apparatus and requires the mains plug to contain a protective earth terminal The mains plug shall only be inserted in a socket outlet provided with a protective earth contact The protective action must not be negated e g by the use of an extension cord without a protective conductor 3 3 SITTING THE EQUIPMENT The Viscometer should be situated within two metres of both electrical and nitrogen gas supplies The polymer grinder must be situated as close as possible to t
39. block This switch is marked O and I The switch is ON when the end is pressed and OFF when the O end is pressed The switch also has an indicator lamp to show when the pump is operating Shown Rear of pump Shown Rear of drier VACUUM POWER Shown Front panel on drier block PET Plus User Manual 25 3 14 DE GASSING THE OIL The pump must be run for at least 1 hour prefer ably overnight to remove any traces of gas and to thoroughly purge the oil of contaminants This procedure MUST be carried out to achieve a gu Wy maximum vacuum 3 n Rotate the mode selector item 11 fully anti clockwise to select the High Throughput mode Large Pear Drop Note that this control may be difficult to rotate Set the gas ballast control item 5 to low flow position T Operate the pump for at least 1 hour or over Shown Turn the mode selector fully counter clockwise night to thoroughly purge the oil of contaminants Shown Set the gas ballast control to I 26 PET Plus User Manual 3 15 SETTING THE PUMP TO MAXIMUM VACUUM This setting MUST be used to achieve maximum vacuum Rotate the mode selector fully clockwise to select the High Vacuum mode Small Pear Drop D 5 Shown Rotate mode selector fully clockwise for High Vacuum mode Shown Set the gas ballast control to OFF position O PET Plus User Manual 27 3 16 POLYMER CHIP GRINDER Place the grinder with
40. bore with a bottom screw The volume of the bore is adjusted by moving the bottom screw up or down If the dispensed weight is too low rotate the bot tom screw clockwise i e screw downwards ADJUST FOR If the dispensed weight is too high rotate the bottom screw anticlockwise i e screw upwards This adjustment should only be necessary when the vessel is used for the first time or when the chip size alters e g when changing suppliers If different sizes of polymer chip are used regu larly it may be a good idea to have one transfer vessel for each chip size ate 70 PET Plus User Manual 11 5 USING THE POLYMER CHIP TRANSFER VESSEL Note that the production drying hopper MUST be fitted with a chip outlet This outlet may be part of the flexible hose assembly connected to the inlet of the extruder Turn the dispensing lever until the lever is pointing upwards Ensure that the top and bottom caps are fitted Connect a low pressure nitrogen supply to the Schrader quick release inlet valve Set the external nitrogen pressure to approx 5psi 0 35 Bar and allow the nitrogen to flow through the transfer vessel for about 10 minutes to make sure the cylinder is completely dry Ensure that nitrogen gas flows out of the 5psi pressure relief valve When ready to take a sample disconnect the nitrogen line from the Schrader quick release inlet valve Do NOT remove the top or bottom caps Take the transfer
41. bove should be ground to powder in the polymer chip grinder then the SUPPLIED PET POWDER procedure followed 9 4 DRYING PRINCIPLE Weigh out 3 8g of polymer chip and transfer to a sample drying tube glass phial Dry the chip samples under vacuum at 150 C overnight optimum drying time is 16 24 hours The above values are guidelines based on the experience of many users Adjustment of temperature and drying time may be required to get the best and most repeatable results 9 5 DRYING PROCEDURE Using a suitable container and laboratory balance weigh out 3 8g of polymer chip Pour the sample into a sample drying tube glass phial then screw the cap onto the top of the tube Tighten the cap sufficiently to give a good seal between the silicone rubber gland and the glass tubing but do not over tighten Repeat for the other phials as required noting SET TEMP that a maximum of 6 samples can be dried at a time Set the temperature controller on the Polymer Drier to 150 C switch the drier on and wait for 15 minutes for the drier to reach this temperature and stabilise WARNING CAUTION HOT SUR 4 FACE Metallic Top Plate Surface can reach Temperatures up to 200 C from Dryer Block heat transfer Wear Heat Protective Gloves Start the vacuum pump by pressing the Vacuum Power switch on the front of the polymer drier Shown Temperature control VACUUM POWER Oo Shown Vacuum power switchl 58 PET Plus User Manual
42. but do not over tighten 3 9 FITTING THE OIL MIST FILTER TO THE PUMP Unscrew the red thumb nut from the bolt in the securing clamp then remove the through bolt Place the rubber seal washer over the top of the outlet port item 7 Remove the caps from both ends of the oil mist filter then place the oil mist filter on top of the washer Fit the clamp around the boss on the outlet port and the boss on the bottom of the oil mist filter Refit the through bolt and red thumb nut to the securing clamp Hand tighten the red thumb nut to secure the filter PET Plus User Manual 21 3 10 CONNECTING THE VACUUM HOSE TO THE PUMP Unscrew the red thumb nut from the bolt in the securing clamp then remove the through bolt Place the special rubber seal filter washer over the top of the inlet port item 4 noting that the conical filter must be positioned downwards into the port Place the hose connector on top of the filter washer Fit the clamp around the boss on the outlet port and the boss on the hose connector Refit the through bolt and red thumb nut to the securing clamp Hand tighten the red thumb nut to secure the connector 22 PET Plus User Manual 3 11 CONNECTING THE PUMP TO THE DRIER BLOCK Push the large diameter rubber hose over the hose connector on the inlet port of the pump Note that an additional clamp is not required because the vacuum will secure the hose to the hose connector Push the other end of the rubber hose over the ho
43. cleaned will give variable results and erratic graph Hot funnel used for sample e Purge and full gas supplies not reaching the barrel GO key not pressed immediately after sample has been loaded into the barrel will give variable results The PET Plus is basically simple in operation and construction No form of regular maintenance is required except that the unit is kept in a clean condition 14 7 POSSIBLE FAULTS IN PRESSURE CONTROL SYSTEM LOSS OF PRESSURE 1 Gas cylinder empty 2 Malfunction of gas supply regulator 3 Check all external screwed and compression joints using a soapy water solution if necessary especially where the supply pipe enters the equipment Unscrew leaky joints and wrap PTFE tape around male end re connect and tighten 4 Check the condition of the seals at the top and bottom of the barrel i e PTFE washer in die retaining nut and PTFE washer where probe seals top of barrel 14 8 BASIC ELECTRICAL CHECKS Your equipment has been completely tested and checked for electrical safety before leaving the factory Regular checks should be carried out on the instrument to establish that the instrument is safe to operate Check all connections for mechanical tightness an earth loop impedance check must be carried out to all components which should be at earth potential This should conform to local safety standards and AMETEK recommends that this be carried out at least annually PET Plus User Manual
44. during the test as the sample degrades Set Temp 295 0C Barrel Temp 295 0C Pressure 24 35Bar Probe Speed 0 581 IV Now 0 790 Time to end of test 12 0 minutes After 6 minutes of total test time the Calculated IV screen is displayed This shows the estimate of the actual IV and this also changes during the test as the sample degrades Set Temp 295 0C Barrel Temp 295 0C Pressure 24 35Bar Probe Speed 0 592 IV Now 0 788 IV at Zero 0 807 Time to end of test 11 0 minutes The screen is updated every second during the test until the test finishes Set Temp 295 0C Barrel Temp 295 0C Pressure 24 35Bar Probe Speed 0 680 IV Now 0 772 IV at Zero 0 799 Time to end of test 3 0 minutes The test finishes 17 minutes after the sample was first inserted into the barrel At the end of the test the equipment will beep then automatically turn off the gas pressure to the barrel to stop the extrusion process The Calculated IV result and the degradation factor will be displayed together with the pass fail indication if this was specified in the relevant test set up Sample 1 Passed IV Degrad n Date Time 0 798 0 010 01 05 2008 15 39 Save Delete PET Plus User Manual 49 The Degradation Factor is the reduction of IV per minute so a value of 0 010 means that the polymer has degraded by 0 010 IV per minute during the test This value indicates how the polymer may degrade inside the production extruder Therefore if the polym
45. e displayed if PASS FAIL parameters have been defined for one or more test results A histogram chart is shown ne xYGEN Plus Pet Plus Tests batch De ER Yew Bot Firm tidy GLCTE PE Jeren lE Ee E Pet Phe Teats baich lal alax EJ test Types EF Configuaion amp Mores iB Onto Population 5 Roms For Help press F1 This chart shows the LSL and USL values along the top of the chart and the grey blocks indicate the data distribution The Bell Curve is also displayed for information The Cp and Cpk values are calculated and are displayed at the left hand side of the chart The Default Sub Group size is 5 but this can be changed by selecting the Main Menu item of EDIT SPC SETTINGS as shown To save the test file select FILE SAVE from the Main Menu For further information regarding the many features of the program please refer to the comprehen sive on line HELP within the software SPC Settings x Default Subgroup Size J nas 102 PET Plus User Manual 17 0 TECHNICAL SPECIFICATIONS IV Measurement Range Barrel Dies Heaters Temperature Range Temperature Control Over temperature Device Nitrogen Gas Pressure Input Working Pressure Range Pressure Measurement Mounting Optional Computer Probe Unit Ancillary Equipment optional Electrical Supply Power Consumption PET Plus Polymer Dryer Fuses PET Plus Polymer Dryer Operating Temp
46. ecome hot during the cleaning process Wear heat protecting gloves when handling these items Polymer fumes may be emitted from the top of the barrel during the visual examination process Wear protective glasses or goggles when viewing the interior of the barrel 44 PET Plus User Manual 7 4 PREPARE A CLEAN FOLLOWER AND FUNNEL Ensure that a clean follower and the relevant filling funnel are ready for use Note that the large circular funnel is used for granules and the long funnel is used for powder The long funnel prevents the powder sticking to the sides of the barrel Do NOT place the funnel onto the top of the barrel until the sample is being loaded otherwise it will become hot and the polymer may stick to it 7 5 CLEAN THE DIE BORE The die bore can only be cleaned by blowing through with high pressure nitrogen Do NOT try to clean the die bore by pushing wire etc through it If the wire breaks inside the die then a new die may be required Always clean the die immediately after use even if another test is not going to be performed afterwards Place the die into the recess of the die retaining nut with the end containing the O Ring facing upwards Screw the die retaining nut with the die to the bottom of the barrel and hand tighten using the tightening tool Loosen off by about 1 10th of a turn about 30 degrees otherwise it will be very difficult to remove once it has heated up and expanded Shown Retaining nut with die
47. ecsen 58 Drying Procedure ccccsesessssseeecssserees 58 Testing the Polymer ccssscseesseereeees 59 SUPPLIED PET POWDER 61 Testing Principles ccccccsccssseeeeseereeres 61 Polymer DN GF ccs ctstisiestcnicteittntenteiGurtadaaentyanedied 61 GRIP S ZE clo sect etnies ee ecmietiecsetenenet 62 Drying PRINCIPE ves ceuisansoviredsxnstasssenierastndsecerane 62 Drying PROCCQUIG iaisssscnladnssscaicniseniananenascaceani 62 Setting the TIMEN ica sswsincscnntetandcsosdiacaasiibucaadsn 65 Testing the Polymer ccccscsscseeseseeeeeres 67 PRODUCTION DRIER c cceeceeees 69 Testing Principles aciiscrcaataeaktsennntibnuntatinestiins 69 Polymer Chip Transfer Vessel 0 0008 69 Checking the Dispensed Volume 70 Adjusting the Dispensed Volume 00 70 Using the Transfer Vessel ccescecerees 71 Testing the Polymer ccccssscseeesseeeeeees 72 MOLTEN EXTRUDIATE cccceee 73 Testing Principles i cicaniintas casicanecpitentincaiitancnia eaten 73 Sample Melt Pot sicsiecasssacsacesedasereesrssnsetsrscasens 73 Using the Sample Melt Pot cece 73 Testing the Polymer ccccssseeesseeeeres 74 13 0 13 1 13 2 13 3 14 0 14 1 14 2 14 3 14 4 14 5 14 6 14 7 14 8 14 9 15 0 15 1 15 2 15 3 15 4 16 0 16 1 16 2 16 3 16 4 16 5 16 6 17 0 TABLE OF CONTENTS Page FINISHED PRODUC
48. ection Soap solution around the joints If hissing is heard or a leak is shown up by soap solution then gas will escape allowing a drop in pressure Aleak can usually be cured by using PTFE tape on the leaking connection and then re connecting and tightening using a spanner WARNING Never subject the viscometer the connecting hose or any of the accessories to pressures greater than 35 Bar Have your gas regulator checked at regular intervals n NOTE The Viscometer has an overpressure detector that disconnects the Nitrogen Supply if a pressure exceeding 35 Bar is inadvertently applied Should this detector be activated it can only be re set by reducing the pressure then switching the viscometer off then on again PET Plus User Manual 19 3 6 CONNECTING THE PROBE The probe is connected to the socket on the top rear of the vertical column Store the probe in the probe holder at the right hand side of the vertical column Ensure that the body of the probe rests onto the probe holder so that the large knurled nut is below the holder Shown Probe connection 3 7 VACUUM PUMP The recommended pump is a BOC Edwards RV rotary vane pump which is a two stage oil sealed sliding vane vacuum pump The pump has a NW25 inlet port item 4 and a NW25 outlet port item 7 a gas ballast control item 5 and a mode selector item 11 When the pump is switched off an inlet valve seals the inlet and prevents the suck back of air and oil
49. ed samples of polymer can remain in the parking area for up to 24 hours before testing with the vacuum pump running Therefore a number of samples from 1 to 6 can be dried at the same time 10 7TESTING THE POLYMER NOTE It is very important that the Die the Barrel and the Follower are scrupulously clean Z and have been assembled correctly after cleaning It is also important that the PET Plus is set to the Pre Test screen ready for testing THIS PROCEDURE IS PART OF THE MAIN PROCEDURE SHOWN IN SECTION 7 7 Select a sample phial and turn the vacuum valve in the plastic vacuum tube to closed lever is at 90 degrees to the vacuum pipe Press the release lever on the front of the quick connector so that the metal tube springs up out of the connector Note that the quick release connector has a sealing valve so that the vacuum is not released from the other sample phials Press the key under PURGE to allow a low volume of nitrogen gas to flow through the barrel to displace any air that may be present Allow the gas to flow for a few seconds to ensure that the barrel is full of nitrogen Place the long filling funnel into the top of the barrel Note that the long funnel prevents the powder sticking to the sides of the barrel Also note that the funnel must be cold or the powder may stick to the funnel Place the open metal end from the sample phial into the top of the filling funnel Open the vacuum valve in the plas
50. ed samples to be stored under vacuum until required 4 An On Off Switch for the Vacuum Pump 5 Atimer settable from seconds to hours with an audible alarm This is mainly for use when drying polymer powder PET Plus User Manual 61 10 3 CHIP SIZE The polymer chips must be ground to fine powder lt 0 5mm using the polymer chip grinder 10 4 DRYING PRINCIPLE Weigh out 3 6g of polymer powder and transfer to a sample drying tube glass phial High IV polymers gt 0 7 are dried under vacuum at 170 C for 55 minutes Low IV amorphous polymers lt 0 7 are dried under vacuum at 170 C for 50 minutes Too short a drying time will result in the sample still being wet and so degrade in the test giving low results Too long a drying time will result in the sample starting to polymerise NOTE The above values are guidelines based on the experience of many users yy Adjustment to temperature and drying time may be required to get the best and most repeatable results 10 5 USING THE POLYMER CHIP GRINDER The Polymer Chip Grinder is designed to grind polymer chips down to particles of either 1mm or 0 5mm using the supplied grinder bowls Davenport recommends only using the 0 5mm bowl for the purposes of grinding polymer chips to powder The polymer grinder should only be used for the purpose for which it was designed as an accessory to the Davenport PET Plus as described in this operating manual Compressed air is used to drive the
51. ed test results will also be calculated and stored in the data table To perform the next test click on the NEW button at the left hand side of the graph The button will change to a green START TEST button and clicking on this button will perform the next test When 2 or more tests have been performed in a batch the graphs can be quickly displayed sequentially by clicking on the LEFT or RIGHT buttons at the left hand side of the graph To view the data table click on the RESULTS button at the left hand side of the graph or click on the RESULTS tab at the bottom of the screen to data table will display the results as shown ojx Date Time Sample Type IV atzero Degradation factor MV 1 0107 2 09 33 37 Eastman 0 8 0 789 0 004 543 00 2 0107 2 10 00 11 Eastmano 8 0 790 0 003 544 00 3 0107 2 13 39 59 Eastman 0 8 0 805 0 004 600 00 4 01 07 2 14 00 45 Eastman 0 8 0 797 0 004 570 00 5 01 07 2 14 34 58 Eastman 0 8 0 767 0 003 534 00 6 mar 150644 Eastman 08 4003 57500 Results Graph Statistics xXBar Range Histogra 4 gt 100 PET Plus User Manual A PASS FAIL indication can be provided by specifying the PASS FAIL limits for one or more columns Right mouse click on the required column e g IV at Zero then select PROPERTIES to display the dialog shown Click on the LIMITS Tab at the top of the screen then set suitable PASS FAIL limits e g between
52. ed with the following accessories 1 Sample Phials p n 757 14 Quantity 6 Used to hold PET granules or powder when drying in the polymer drier 2 Vacuum Taps and Hose Quantity 6 This assembly is used to connect the phials to the polymer drier It is also used to isolate the phials from the vacuum line at the end of the drying time 3 Hose for Vacuum Pump p n 468 27 Quantity 1 Used to connect the polymer Drier to the Vacuum Pump 2 4 VACUUM PUMP The Vacuum Pump is an optional item and is used together with the Polymer Drier to dry PET samples before testing to measure the POTENTIAL IV A high quality vacuum pump that can achieve a very good vacuum of better than 0 1mm Hg MUST be used AMETEK recommends the BOC Edwards RV rotary vane pump which is shown above 14 PET Plus User Manual Shown Polymer Dryer Shown Vacuum pump wiith oil mist filter attached 2 5 POLYMER CHIP TRANSFER VESSEL The Polymer Chip Transfer Vessel is an optional item and is used to collect dried polymer from the production hopper to check the IV of the polymer before it is extruded 2 6 SAMPLE MELT POT The Sample Melt Pot is an optional item and is used to collect molten polymer from the produc tion extruder to check the IV of the polymer during the extrusion process It is mainly used to collect a sample from a textile spinneret and is not usually used when making preforms etc 2 7 POLYMER CHIP GRINDER The Poly
53. emove any polymer chip remaining on the rotor blades or coarse sieve Follow the procedure shown in SECTION 10 SUPPLIED PET POWDER to grind the chips to a powder then test using the PET Plus 76 PET Plus User Manual 14 0 MAINTENANCE 14 1 FITTING A NEW O RING TO THE DIE The die O ring is used to prevent polymer from leaking past the die during a test Therefore the O ring diameter should be slightly larger than the die so that it protrudes out slightly from the recess in the die When the O ring becomes worn or damaged it should be replaced otherwise low IV measurements will be produced There is no hard and fast rule as to the frequency that the O ring should be replaced but this may need to be replaced daily if samples are tested on an hourly basis LJ Stretched O ring O ring O ring reformed to Die correct size Shown Expansion Tool Shown Contraction Tool To remove the O ring make a vertical cut in the ring using a sharp pointed scalpel or Craft Knife WARNING Always wear cut resistant gloves such as ones made of Dyneema Lever out the old O ring with the knife Place the die on the bench with the O ring slot uppermost Position the Expansion Tool over the top of the die Place a new PTFE O ring over the tapered end of the expansion tool Slide the O Ring over the tool onto the die by hand Position the O ring into the recess on the die The O
54. enter the required temperature in degrees C The die length cm and die diameter cm are shown on the die certificate and this should be referred to for this information To change a die dimension press the key under DIE LENGTH or DIE DIAMETER then enter the required values in cm Enter the required Pass Fail limits Upper Lower IV IV 0 00 0 00 This screen is used to define the pass fail feature At the end of every test the result screen will display the calculated IV and can also display the pass fail status If a pass fail indication is not required then the Upper IV and Lower IV should be set to Zero Ifa pass fail indication is required then one or both of the IV values should be defined Note that if only the Lower IV is specified then the sample is considered to have passed if the calculated IV is above the Lower IV and no Upper IV is required Also note that if only the Upper IV is specified then the sample is considered to have passed if the calculated IV is below the Upper IV and no Lower IV is required 38 PET Plus User Manual Most polymers are specified with a tolerance of 0 02 so a polymer with a nominal 0 8 IV could have an Upper IV specified as 0 82 and a Lower IV specified as 0 78 Enter the required Pass Fail limits Upper Lower IV IV 0 82 0 78 When the test parameters are correct press the ENTER key to return to the edit test screen 5 5 PASSWORD PROTECTION The test parameters can be p
55. equipment should the main temperature measuring device fail for any reason The temperature at which it is activated is pre set at 400 C 4 3 SETTING THE TEST TEMPERATURE The test temperature is selected using the relevant test set up screen 4 4 WHICH TEST TEMPERATURE TO USE Generally samples of IV up to 0 70 should be tested at 284 C and IVs over 0 70 at 295 C Selecting Melt Temperature Up to 0 7 IV 284 C Above 0 7 IV 295 C 4 5 WHICH DIE SIZE TO USE Note that one die is supplied with the equipment size specified at time or order but additional dies may be purchased as required Die Size cm IV at 284 C IV at 295 C 15 thous 0 0381 0 43 to 0 62 NA 20 thous 0 0508 0 53 to 0 70 0 70 to 0 83 30 thous 0 0762 NA 0 74 to 1 14 40 thous 0 1016 NA 0 93 to 1 43 34 PET Plus User Manual 5 0 CREATING A TEST SETUP 5 1 DEFAULT TEST SETUPS The equipment is supplied with 4 pre defined test set ups called 284 20THOU 295 20THOU 295 30THOU TRAINING The first test set up is preset to give a barrel temperature of 284 C but the other 3 are preset to give a barrel temperature of 295 C The 295 30THOU test set up is preset for a 30 thou die 0 0762cm but the other 3 are preset for a 20 thou die 0 0508cm The test set up called TRAINING sets the equipment into a special training mode and does NOT perform a melt test Note that the special training mode is only available if the test set up is called TRAINING Each test set
56. er stays within the heated zone of the production extruder for 3 minutes the IV will drop by an estimated 0 03 The test result should normally be saved into the internal memory so that the statistics can be calculated If for any reason the result is not to be stored it can be deleted When either action is selected by pressing the relevant key the Pre Test screen is re displayed as below Set Temp 295 0C Barrel Temp 295 0C Pressure 0 0Bar Probe 15 85mm Insert sample follower then press GO Gas Off Purge Full Exit The equipment is now ready for cleaning 7 11 CLEANING THE BARREL Ensure that the pressure displayed on the screen is nominally zero Using heat protecting gloves remove the probe from the barrel and if necessary wipe any polymer from the tip Store the probe in the probe holder at the right hand side of the vertical column Ensure that the body of the probe rests onto the probe holder so that the large knurled nut is below the holder Unscrew the die retaining nut from the bottom of the barrel with the tool provided Note that the die will NOT be attached to the die retaining nut Insert the charging tool into the top of the barrel until it touches the top of the follower Gently push downwards on the barrel cleaning tool until the die is pushed out of the bottom of the barrel Shown Top of PET Plus with probe holder Remove the charging tool from the top of the barrel Hold the die wi
57. erature Storage Temperature Relative Humidity Net Instrument Weights PET Plus Polymer Dryer Polymer Grinder Dimensions HxWxD PET Plus Polymer Dryer Polymer Grinder Minimum 0 45 using 0 015 Bore Die Maximum 1 40 using 0 040 Bore Die Insulated stainless steel barrel with replaceable stainless steel liner One die is supplied with the equipment size specified at time or order but additional dies may be purchased as required Dies are available with bores of 0 015 0 020 0 030 and 0 04 3 x 250 W cartridge type symmetrically positioned for optimum temperature control 50 C 400 C Solid state electronic 3 term controller with set point adjustment Secondary overheating safety limit factory set to 400 C Oxygen free and less than 5ppm of water specification White Spot Recommended 200 Bar capacity bottle 30 Bar 440 psi Maximum 35 Bar 510 psi 7 30 Bar Electronic pressure transducer Bench mounting Enough bench space will also be needed for the optional computer key board and possibly printer PC compatible Optional software supplied on CD Linear Voltage Displacement Transducer encased in non magnetic canister Polymer Drier Vacuum Pump Polymer Grinder Polymer Chip Transfer Vessel Industrial Grinder and Melt Pot 230V AC 10 50 60Hz or 115V AC 10 50 60Hz Not adjustable Mains Power Must be specified at time of order 800 VA max 1000 VA max Mains In 230V AC 2 x T5AH250
58. erred to the PET Plus barrel using a procedure that en sures that the polymer does not come into contact with any external air 13 2 INDUSTRIAL GRINDER High speed grinding and chipping machinery is used to pulverise samples The equipment must be used in accordance with the manufacturers instruction manual and ear protection must be used at all times in the vicinity of the grinding equipment Note that liquid nitrogen is used to pre cool samples WARNING ALWAYS WEAR SAFETY GLASSES AND HEAT RESISTANT GLOVES WHEN HANDLING LIQUID NITROGEN WHICH IS AT 196 C AMETEK recommends the Fritsch Pulverisette 15 which is capable of reducing a pre form to chip in seconds It may be floor or bench mounted and comes complete with an 8mm sieve NOTE A coarse sieve 8mm is used a to produce chip and very little powder thus making cleaning easy A sieve to produce powder could be used but this would necessitate stripping the system for cleaning after pulverising each sample Therefore it is better to chip the sample in the pulveriser and then to grind to powder using the Polymer Grinder PET Plus User Manual 75 13 3 USING THE INDUSTRIAL GRINDER This is used to grind pre forms bottle necks polymer plaques pieces of polymer extrudates and thick sheet samples to approx 8mm chips One complete pre form is usually sufficient for chipping and drying If only the bottle necks are to be used then several bottle necks usually about three a
59. essure Push the knob upwards again after adjustment to lock the regulator setting The grinder blade is driven by an air motor and this is lubricated by an oil mist carried by the compressed air A special oil lubricator is fitted to the air manifold assembly and this supplies oil drops into the air flow When the grinder is running view the glass tube above the air manifold assembly and check the speed of the oil drops The required speed is approximately 1 drop per minute If the oil drop rate is not correct adjust the oil drop regulator screw which is on top of the glass tube Note that the grinder stops automatically after 30 seconds so the grinder will need restarting several times during this procedure Ser PRESsuRE Shown Pressure control gauge pi Max 17 bar t 10 C 75 C P3E LAOOTFN e 2 f Shown Check oil drop rate Shown Adjustment for oil drop rate PET Plus User Manual 29 3 17 INDUSTRIAL GRINDER AMETEK recommends the Fritsch Pulverisette 15 This equipment connects to the mains using a standard mains lead Shown Fritsch Pulverisette 15 30 PET Plus User Manual 4 0 SETTING UP THE VISCOMETER 4 1 INITIAL CONFIGURATION Switch the equipment on to display the sign on screen This screen indicates the embedded version number the equipment serial number and the probe serial number Davenport PET Plus S No 105102 Version 1 0 Issue 7 Probe S No 105
60. extruded is calculated similar to the MFI method B using an LVDT probe to measure the movement of the follower The rate of extrusion is accurately measured by the probe which is designed to operate under the high pressure conditions within the barrel during extrusion The system calculates the total thermal and hydro lytic degradation Therefore a Melt test can show the degradation 8 PET Plus User Manual due to the presence of moisture in the polymer so can be used to check the performance of the production drying system A Melt test can also be used to measure the thermal degradation factor caused by the production extruder PET has historically been measured using the solution method and this indicates the POTENTIAL Intrinsic Viscosity IV of the polymer but does not show how the polymer will behave or degrade during extrusion The solution technique is being phased out due to the insoluble nature of highly crystalline polymer plus high environmental and disposal costs of solutions It is also not so suitable for testing reground or recycled material because the quantity tested is very small and may not show the Average IV of the mixed granules The PET Plus is designed to replace the solution method so directly reports the Intrinsic Viscosity IV of the polymer and not the Melt Flow Rate PET is hygroscopic and any water molecules present at melt temperatures gt 250C will give
61. fect the IV values during the test 7 15 VIEWING PREVIOUS TEST DATA When a test is performed in the stand alone mode the test results are saved into the internal memory This test result is stored together with the test name ID and a Date Time ID that is created from the internal clock inside the equipment Therefore statistics can be calculated and displayed for each of the defined test set ups and the test data can be easily viewed and exported Display the Select Test screen to select one of the pre defined test set ups Select the required test 20THOU_295C 0 Samples Date and Time 30 05 2008 07 48 Select lt gt Edit Press the key under gt or lt to select the test set up for the data that is to be viewed When the required test set up is displayed press the key under SELECT to display the Analysis screen Set Temp 295 0C Barrel Temp 295 0C Pressure 0 0Bar Probe 15 85mm 20THOU_ 295C Test Results Stats Suspend Press the key under RESULTS to view the individual test results Note that a warning message will be displayed if there is no data present for this test set up There is no data for this test setup Press ENTER to continue PET Plus User Manual 53 The Results screen shows the test number IV Degradation Factor Date and Time at the end of test The screen below shows the results for test number 12 Test No 12 of 12 Select using keys IV Degrad n Date Time 0 798 0 010
62. g the actual temperature and entering this value into the system Press the key under CAL TEMP to display the Temperature Calibration screen Set Temp 295 0C Measured Temp 294 8C Set Cal View View Temp Point Points Readings Press the key under SET TEMP then enter 300 C This is the recommended calibration temperature Set Temp 300 0C Measured Temp 300 0C Set Cal View View Temp Point Points Readings Fit the die to the bottom of the barrel then insert approx 2 grams of PET NOTE Use Polythene instead of PET if using a mercury in glass thermometer PET will break a glass thermometer when it cools and contracts Insert the reference thermometer into the melt H Allow the barrel temperature to stabilise approx 5 minutes as shown by the measured temperature display Measure the actual barrel temperature using the reference thermometer and compare with the requested temperature of 300 C If the actual temperature is not 300 C 0 1 C press the key under CAL POINT to display the cal point screen True Temp 300 0C Measured Temp 300 0C Change Clear True Accept Points Cancel 84 PET Plus User Manual Press the key under CHANGE TRUE to display the change true temperature value screen Change true temperature value 301 2 BkSp Clear All Enter the true temperature value as indicated on the reference thermometer The display will now show the true temperature as measured by the
63. he silencer to the end of the air motor Loosen the motor securing clamp using an Allen key Place a smaller Allen key into one of the holes in the motor eccentric boss then rotate the motor eccentric boss clockwise to tighten the belt Shown Polymer grinder top cover and belt gt OD sts Pap 25 mS F A eat ec fen LOOSEN MOTOR CLAMP i JF a Shown Loosen motor clamp Mig GE AA m N bee agne a me ft lt a E 2 a mae PLACE ALLEN KEY INTO HOLEIN ECCENTRIC BOSS __ i n P a Shown Location for loosening clamp PET Plus User Manual N 79 Ensure that the silencer remains in the same position Retighten the motor securing clamp then i 7 recheck the belt tension JA j mme L ey pea Unscrew the silencer from the end of the air motor i 4 3 ee T gr ho Refit the top cover and secure using the two 2 domed nuts and washers Screw the silencer to the end of the air motor This is a little difficult because it is not possible to view the threaded hole in the motor body Refit the rubber seal and foam to the end of the silencer Refit the silencer cover 14 5 REPLACING THE DRIVE BELT LOOSEN 3 GRUB SCREWS A broken drive belt can be replaced as shown ea Remove the top cover as shown in the previous section Loosen the three 3 grub screws in the motor pulley Shown Location of grub screws Lo
64. he vacuum pump if this drying option is used The polymer grinder is operated by compressed air so should be situated close to a suitable air line if this grinding option is used The industrial grinder cutting mill can be noisy in operation so this may need to be sited outside of the testing laboratory The polymer grinder and industrial grinder require liquid nitrogen and this should be handled with care and the user should wear protective gloves because of the danger of cold burns this has a temperature of 196 C 3 4 CONNECTING THE PET PLUS TO THE MAINS Connect the mains supply lead to the switched and fused input connector on the rear of the vertical column The mains switch is marked O and The switch is ON when the end is pressed and OFF when the O end is pressed Only connect to the supply specified on the Serial Number nameplate situated under the mains input connector 2 E Shown PET Plus On Off Switch 18 PET Plus User Manual 3 5 CONNECTING THE NITROGEN GAS SUPPLY Connect the viscometer to a 30 Bar nitrogen supply via a gas regulator and or gas tap Turn off the gas supply then connect the flexible inter connection tube between the regulator tap and the inlet connector on the left hand side of the Viscometer base The connections must be firmly tightened to ensure that they are gas tight Check for gas leaks around the inlet connection by Obvious hissing Shown Nitrogen supply conn
65. hen press GO Gas Off Purge Full Note that the PC Pre Test screen will NOT be displayed if the probe is not electrically connected to the probe socket on the rear of the vertical column If the probe is not connected the warning screen below will be shown ERROR CONDITION Probe NOT Connected Press ENTER to Cancel Also note that the intermediate screen shown below will be displayed if the barrel is not at the required temperature Set Temp 295 0C Barrel Temp 292 8C Under Computer Control Waiting for barrel temp to stabilise Suspend This screen will automatically change to the PC Pre Test screen when the barrel has stabilised at the required temperature Note that the equipment MUST be set to the PC Pre Test screen BEFORE trying to test a sample PET Plus User Manual 99 slelx al l xl The test is performed in exactly the same way SAARES eer antenat ee a as for a stand alone system i e the sample is sam co inserted into the barrel then the GO button is pressed Note that the computer now requires no user intervention until the end of the test NEXYGEN Plus PET will initially plot the barrel temperature and nitrogen pressure and will then plot the probe position probe speed and instan taneous IV at the relevant times during the test At the end of the test the Line of Best Fit will be drawn through the IV values andthe Vat Zero will be calculated The select
66. in easy reach of a compressed air supply capable of providing 16cfm 0 45cmm at 80psi 5 5 Bar Connect the air supply to the inlet connection at the rear of the grinder using the supplied plastic hose Unscrew the oil filler cap then fill the lubricator with the correct grade of oil e g Shell Morlina 10 or Tellus R10 The top of the oil must be visible anywhere inside the sight glass at the front of the lubrica tor Refit the oil filler cap after adding the oil 28 PET Plus User Manual Shown Inlet connectin at rear of grinder OIL FILLER et Men 17 Sor o 7e Shown Oil filler location Although the unit does not use mains power it must be connected to a good earth point to prevent any build up of dangerous static charg es Therefore an additional earth wire must be connected to the unit Note that an earth wire is not supplied with the equipment and this has to be provided by the user To operate the grinder close the lid and fasten with the clip then push the start knob at the front of the unit When the grinder is running check that the pressure gauge on the left hand side of the unit shows 80psi 5 5 Bar Note that the grinder stops automatically after 30 seconds so the grinder may need restarting during this procedure If the pressure gauge does not show the correct pressure when the unit is running pull the orange knob downwards then rotate the knob to achieve the correct pr
67. ing a DAVENPORT product the more stringent rules should take precedence Safety Considerations The PET Plus is completely enclosed and pro vides no potentially hazardous outputs Safety considerations are related to the power connec tions and physical mountings Electronic and mechanical components housed within the PET Plus covers are to be serviced by authorized DAVENPORT representatives only PET Plus User Manual 3 AMETEK MEASUREMENT amp CALIBRATION TECHNOLOGIES DIVISION EUROPEAN DECLARATION OF CONFORMITY NAME ADDRESS OF MANUFACTURER AND LOCATION OF TECHNICAL CONSTRUCTION FILE Ametek Inc 8600 Somerset Drive Largo FL 33773 USA PHONE 727 538 6084 FAX 727 535 4391 DESCRIPTION OF EQUIPMENT Product Ametek PET Polymer Measurement Instrument Models LLOYD PET Plus 01 3440 and PET Plus 01 3480 LLOY PK Effective Date June 2014 HARMONIZED STANDARDS USED A sample of this product has been assessed against the essential health and safety requirements of the Low Voltage and the EMC Directives listed below Based on conformity with the listed directives Ametek Inc declares the products mentioned above are in compliance with the following EMC Directive 2004 108 EC and Machinery Directive 2006 42 EC BS EN 61010 1 2010 Safety Requirement for Electrical Equipment BS EN 61326 1 2006 Electrical Equipment for Measurement Control and Laboratory use General Requirements This declaration of conformity
68. into the top of the barrel Insert the charging tool into the top of the barrel Immediately press the green GO key to start the test The Charging screen will be displayed 60 PET Plus User Manual 10 0 SUPPLIED PET POWDER 10 1 TESTING PRINCIPLE The polymer must be ground to a powder using the polymer grinder then dried using the drier and vacuum pump all of which are optional extras Note that a quantity of liquid nitrogen is required to assist with the grinding process so suitable storage and handling procedures are required When the polymer is dry it MUST be transferred to the PET Plus barrel using a procedure that ensures that the polymer does not come into contact with any external air gt NOTE Drying time is a function of both temperature and vacuum A lt 0 1mm Hg vacuum is essential 10 2 POLYMER DRYER Shown Poymer drier The Polymer Diyer has been designed for drying PET and other hygroscopic materials and incorporates the following features 1 Atemperature controlled heated block that has been machined to hold and heat six sample phials The temperature controller can control the temperature from ambient to 200 C 2 C 2 Six quick release valves at the top of the unit to connect each sample phial to the vacuum supply 3 Two Storage or Parking areas to hold six sample phials These areas are at the side of the heated block but are not heated They are provided to allow the dri
69. into the vacuum system An internal oil pump delivers pressurised oil to the vacuum pumping mechanism in the RV pump The level and condition of the oil can be viewed through a sight glass item 8 Two oil filler plugs item 6 and an oil drain plug item 9 are provided on the oil box The motor is fitted with an on off switch item 12 and an internal thermal overload device When the motor is too hot the thermal overload device switches off the pump The thermal overload device has an automatic reset and when the motor cools down the device resets 1 Electrical inlet 4 NW25 inlet port 10 Rubber feet connector 5 Gas ballast control 11 Mode selector 2 Voltage indicator 6 Oil filler plug 12 On off switch 3 Lifting handle 7 NW25 outlet port 8 Ojl level sight glass 13 Motor fan cover 9 Oil drain plug 14 Correct direction of rotation 20 PET Plus User Manual 3 8 FILLING THE PUMP WITH OIL The recommended oil is Edwards Ultragrade 19 hydrocarbon oil The maximum volume is 0 7 litres and the minimum level is 0 42 litres Remove one of the oil filler plugs item 6 then pour the oil into the pump until the oil level just reaches the MAX mark on the bezel at the top of the sight glass item 8 If the oil level goes above the MAX mark remove the drain plug item 9 and drain the excess oil from the pump After a few minutes recheck the oil level and top up if necessary Refit the oil filler plug and tighten firmly by hand
70. is procedure MICROMETER SET TO Omm END OF MICROMETER N LINE WITH GROOVES Also note that the probe must be connected to the PET Plus and the equipment MUST be left switched on for at least 15 minutes BEFORE performing this calibration The probe is calibrated by moving the probe rod a known distance then indicating this distance into the system Press the key under CAL PROBE to display the Probe Calibration screen Probe Serial Number 105102 Measured Probe 12 671mm Serial Cal View View Number Point Points Readings Set the calibration micrometer to 0 000mm then lock the micrometer into its holder so that the micrometer tip is in line with the two reference grooves Place the probe into the holder at the right hand side of the vertical column Smear petroleum jelly onto the end of the probe rod then attach the calibration tool to the Probe Check that the measured probe is Omm 0 01mm 88 PET Plus User Manual True Probe 1 000mm Measured Probe 1 673mm Change Clear True Accept Points Cancel The true probe should automatically display 0 000mm If it does not show 0 000mm press the key under CHANGE TRUE then enter Omm The display will now show 0 000mm for the true probe Press the key under ACCEPT to correct the zero probe reading True Probe 0 000mm Measured Probe 0 000mm Change Clear True Accept Points Cancel If a calibration point had already been entered at Omm or approx this val
71. it Press the key under gt one or more times to select NEW_TEST Select the required test NEW_TEST 0 Samples Date and Time 29 05 2008 13 09 lt Create When NEW_TEST is displayed press the key under CREATE to display the edit test screen Press a key to select an option NEW_TEST Rename Global Delete Setup Press the key under RENAME to display the rename test screen Rename Test NEW_TEST NEW_TEST Clear A11 Press the key under CLEAR ALL to delete NEW_TEST then enter the required name using the keypad This name could be a supplier name or a production ID such as drier identification Press the ENTER key to return to the edit test screen PET Plus User Manual 37 5 4 DEFINING A TEST SETUP Display the Select Test screen Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit Press the key under gt or lt to select the test set up that is to be defined then press the key under EDIT to display the edit test screen Press a key to select an option 20THOU_284C Rename Global Delete Setup Press the key under SETUP to display the first Set up screen Press a key to change a parameter Set Die Die Temp Length Diameter 284 1 276 0 0508 The test temperature is generally 284 C for polymers having an IV below 0 7 and 295 C for polymers having an IV above 0 7 IV To change the test temperature press the key under SET TEMP then
72. layed to ensure that data is not erased by accident Note that if the system is password protected then this erasing action can only be performed after the password has been entered PET Plus User Manual 55 8 0 SAMPLE PREPARATION The PET Plus system can be used to test both the PET resin and the finished product at various stages throughout the production process 1 Check the IV of the supplied PET granules 2 Check the IV of the PET granules after being dried in the production drier 3 Check the IV of the molten PET after being heated in the production extruder 4 Check the IV of the finished product Test number 1 is to measure the POTENTIAL IV of the PET and is equivalent to the solution method This test will ONLY give the same IV as the solution method if ALL moisture is removed from the polymer before testing less than 20ppm moisture The supplied granules must be dried for 16 to 24 hours before testing but the granules can be ground to a powder in which case the drying time is reduced to 50 55 minutes Test number 2 is to measure the check the efficiency of the heaters and or drying desiccant used in the drying hopper Test number 3 is mainly for use by fibre producers to measure the IV of the extrudate from a spin neret Test number 4 is to measure the IV of a finished pre form or other moulded item The equipment required and the sample preparation is shown in the following sections 56 PET Plus User Manual 9 0
73. ld be presented to the carrier by the purchaser TRADEMARKS AMETEK is a registered trademarks of AMETEK Inc LLOYD INSTRUMENTS is a trademark of AMETEK Inc DAVENPORT is a trademark of AMETEK Inc Other trademarks are the property of their respective owners SUPPORT AMETEK Lloyd Instruments Ltd Steyning Way Bognor Regis West Sussex UK PO22 9ST Tel 44 0 1243 833 370 Fax 44 0 1243 833 401 Email techsupport ametek co uk Internet www lloyd instruments co uk AMETEK Measurement and Calibration Technologies 8600 Somerset Drive Largo FL 33773 USA Tel 1 727 536 7831 Tel 1 800 527 9999 within USA only Email chatillon fl lar ametek com 2 PET Plus User Manual ICONS WARNING The raised hand icon warns of a situation or condition that may lead to personal injury or death Do not proceed until the warning is read and thoroughly understood Warning messages are shown in bold type DANGEROUS VOLTAGE gt The lightning icon warns of the presence of an uninsulated dangerous voltage within the product enclosure that might be of sufficient magnitude to cause serious shocks or death Never open the enclosures unless you are an authorized and qualified LLOYD INSTRUMENTS service personnel Never open any enclosure when power is connected to the system or its components CAUTION gt The exclamation point icon indicates a situation or condition that may lead to equip ment malfunction
74. llower are scrupulously clean yy and have been assembled correctly after cleaning It is also important that the PET Plus is set to the Pre Test screen ready for testing THIS PROCEDURE IS PART OF THE MAIN PROCEDURE SHOWN IN SECTION 7 7 Press the key under PURGE to allow a low volume of nitrogen gas to flow through the barrel to displace any air that may be present Allow the gas to flow for a few seconds to ensure that the barrel is full of nitrogen Press the key under GAS OFF to stop the flow of nitrogen gas Remove the bottom plug from the sample melt pot and position the melt pot onto the top of the barrel Remove the top plug from the sample melt pot and push the plug of polymer into the PET Plus barrel using the charging tool Remove the sample melt pot from the top of the barrel Insert a clean follower into the top of the barrel Insert the charging tool into the top of the barrel Immediately press the green GO key to start the test The Charging screen will be displayed 74 PET Plus User Manual 13 0 FINISHED PRODUCT 13 1 TESTING PRINCIPLE The finished product must first be broken into chips which are ground to a powder using the polymer grinder then dried using the drier and vacuum pump all of which are optional extras Note that a quantity of liquid nitrogen is required to assist with the grinding process so suitable storage and handling procedures are required When the polymer is dry it MUST be transf
75. me into the test file against each test The Quality Control manager can configure the tests to ensure that the operators can only work within specified test conditions These restrictions can be used to prevent the operator from creating new uncontrolled tests changing the test temperature or permanently deleting test data etc If the Quality Manager subsequently changes any controlled test the changes are stored into the audit database to provide an audit trail This database can also store the reason for the changes so that full traceability of test changes is recorded PET Plus User Manual 91 16 3 INSTALLING THE SOFTWARE Insert the CD and the set up wizard will be automatically shown Click on the NEXT button to proceed Select the I Agree option then click on the NEXT button Click on the NEXT button to proceed The dialog shows the default shared folder and this can be changed if required Click on the NEXT button to proceed 92 PET Plus User Manual ii NEXYGEN Plus PET 5 xj Welcome to the NEXYGEN Plus PET Setup Wizard ALD a The installer will guide you through the steps required to install NEXYGEN Plus PET on your computer WARNING This computer program is protected by copyright law and international treaties Unauthorized duplication or distribution of this program or any portion of it may result in severe civil or criminal penalties and will be prosecuted to the maximum extent pos
76. mer Chip Grinder is an optional item and is used to grind polymer chips to a powder to allow a much faster drying time Shown Polymer chip transfer vessel Shown Sample melt pot illustration Shown Polymer chip grinder PET Plus User Manual 15 2 8 INDUSTRIAL GRINDER The Industrial Grinder is an optional item and is used to grind pre forms or other finished products to produce polymer chips AMETEK recommends the Fritsch Pulverisette 15 2 9 EQUIPMENT AND MATERIAL REQUIRED Not Supplied by AMETEK 2 9 1 Nitrogen Supply 1 Nitrogen gas supply with a water content of less than 5ppm parts per million oxygen free white spot specification 2 The supply is to be fitted with an on off gas tap and a regulator that can be set to 30 bar 440 psi 2 9 2 Safety Equipment 1 Cut resistant gloves made of DYNEEMA material Useful when removing O Ring from die or scraping polymer off die or follower 2 Heat resistant gloves 3 Safety glasses 2 9 3 Hot Plate To aid cleaning of follower put the dirty followers on the hot plate PET will carbonate and be easier to remove 2 9 4 PTFE Tape To seal gas connection joints 2 9 5 Razor Blade Scalpel To scrape molten polymer off dies and followers 2 9 6 Scotchbrite Pad To polish followers and dies until shiny 16 PET Plus User Manual Shown Industrial grinder 2 10 OPTIONAL SPARE ITEMS The following optional spares items are avail able
77. nfigures Visual Basic for Applications R Core Gathering required information Cancel PET Plus x Temperature Pressure Probe Position Probe Speed lV Port Name Cancel xj Temperature 295 0 C Pressure 25 00 bar Probe Position 1 09 mm Probe Speed 0 000 mm min IV 0 000 16 5 CREATING A TEST FILE Note that the test parameters test temperature die dimensions and pass fail limits MUST be set in the NEXYGEN Plus PET test set up The parameters stored in the PET Plus are NOT used when performing a test using the NEXYGEN Plus PET software Click on the CREATE A NEW BATCH OF TESTS button on the Welcome screen shown Note that if the Welcome screen is not displayed it can be displayed by clicking on the 9th Icon from the left on the toolbar A SAVE AS dialog will be displayed as shown Enter the required name for this test file noting that the file can be saved in any location e g a networked folder Click on the SAVE button to display the TEST TYPE screen shown Welcome to NEXYGEN Plus Create New Batch from Standards Library amp Print a Batch Report Vv Show this screen each time I log on E3 Save in E Data ec Ee My Recent Documents E Desktop My Documents Pr My Computer T File name Batch Files batch aa amp My Network Save as type Places You must choose which type of test is going to be performed in thi
78. nter a new calibration point overwriting the previous point Reset the calibration micrometer to 0 000mm Check that the measured probe is Omm 0 01mm If the measured probe is not Omm 0 01mm enter a new calibration point overwriting the previous point Set the calibration micrometer to 2 500mm Check that the measured probe is 2 5mm 0 01mm If the measured probe is not 2 5mm 0 01mm enter a calibration point overwriting the previous point if requested Perform the complete calibration by entering points at 2 5mm intervals i e at 5mm 7 5mm 10mm 12 5mm 15mm 17 5mm 20mm 22 5mm and a new calibration pointy at 25mm 90 PET Plus User Manual 16 0 NEXYGEN PLUS SOFTWARE 16 1 NEXYGEN PLUS PET The optional NEXYGEN Plus PET software part number 40 0780 is an accessory for use with the PET Plus equipment It is a multi tasking 32 bit Windows 2000 Windows XP Windows Vista program which has been designed to be easy to use by all operators including those who have little computer knowledge When a TEST SET UP has been selected the NEXYGEN Plus PET program will control the barrel temperature display the test graphs and automatically calculate the required test results e g IV Degradation factor and MV User specified Pass Fail specification Limits can be set for the IV Degradation factor and or MV and the software will indicate which samples have passed or failed When several tests have been performed the
79. nules into the barrel 11 Long Filling Funnel p n FND 0114 00 Used for loading dry powder into the barrel 12 Probe Probe Sealing Washer and Connecting Cable p n 750 048 amp 750 76 amp 09 0980 Displacement transducer used to measure the movement of the follower to calculate the flow rate 13 Barrel Cleaning Brush p n 750 1020 Used for cleaning a badly crusted barrel 14 Coiled Nitrogen Connecting Hose p n 778 31 Used to connect the PET Plus to the nitrogen supply 15 Thermometer 283 C 287 C p n 338 104 16 Used when calibrating to 284 C 16 Thermometer 293 C 297 C p n 338 104 1032 Used when calibrating to 295 C 17 Tweezers p n 92 0404 Used to hold hot die and followers 18 RS232 Cable p n 09 0639 2 2 CONSUMABLE ITEMS The PET Plus is supplied with the following consumable items QTY Description Part No 4 Box of Cleaning Patches 338 132 50 Die O Ring 750 1019 5 Probe Sealing Washer 778 67 5 Plug Sealing Washer 778 52 5 Die Nut Washer 778 54 12 Follower 750 45 5 Top Cap Sealing Washer 778 99 PET Plus User Manual 2 3 POLYMER DRYER AND ACCESSORIES The Polymer Drier is an optional item and is used to dry PET samples before testing to measure the POTENTIAL IV It MUST be used with a high quality vacuum pump that can achieve a very good vacuum of better than 0 1mm Hg and Davenport recommend the BOC Edwards RV rotary vane pump The Polymer Drier is suppli
80. o powder Remove the receiving bowl and transfer the powder to the sample phials as shown later Clean the grinder blade grinding bowl collecting funnel and collecting bowl 64 PET Plus User Manual 10 6 SETTING THE TIMER The timer can be set to a wide range of time periods but its main use is provide a 50 minutes or 55 minutes timing for drying polymer powder Check that the 3 controls are set as below E Function Bottom Left Screw A1 E Time Units Bottom Right Screw 10m E Time Base Top Right Screw 0 2 to 12 Asmall terminal screwdriver is required to adjust Rotate the relevant screw to set the unit as shown below Set the dial to 0 82 to select 50 minutes Set the dial to 0 92 to select 55 minutes Using a suitable container and laboratory balance weigh out 3 6g of polymer powder Pour the sample into a sample drying tube glass phial then screw the cap onto the top of the tube Tighten the cap sufficiently to give a good seal between the silicone rubber gland and the glass tubing but do not over tighten Turn the vacuum valve in the plastic vacuum tube to closed lever is at 90 degrees to the vacuum pipe PET Plus User Manual 65 Repeat for the other phials as required noting that a maximum of 6 samples can be dried at a time Set the temperature controller on the Polymer Drier to 170 C switch the drier on and wait for 15 minutes for the drier to reach this temperature and stabilise V
81. or damage Do not proceed until the caution message is read and thoroughly understood Caution messages are shown in bold type NOTE Z CAUTION THIS EQUIPMENT IS ONLY FOR USE BY TRAINED PERSONNEL IF NOT USED IN MANNER STATED MAY CAUSE HAZARD ALL SPECIFIED SAFETY PROCEDURES SHOULD BE STRICTLY ADHERED TO HIGH TEMPERATURES AND MOLTEN POLYMER ARE INVOLVED IN THE VISCOMETER TESTING PROCESS ES ALWAYS WEAR HEAT PROTECTING GLOVES WHEN HANDLING THE DIE FOLLOWERS PROBE CLEANING TOOL AND AREAS AROUND THE HEATED BARREL THE VISCOMETER AND SOME OF ITS ACCESSORIES ARE POWERED BY MAINS SUPPLY VOLTAGE TO MAINTAIN ALL ASPECTS OF THE SPECIFICATION ONLY DAVENPORT LLOYD INSTRUMENTS APPROVED ACCESSORIES CONNECTIONS AND COMPONENTS SHOULD BE USED NITROGEN GAS UNDER PRESSURE IS USED WORK ING PRESSURE 30 BAR MAX PRESSURE 35 BAR READ THIS MANUAL BEFORE USING THE VISCOM ETER OR ANY OF ITS ACCESSORIES The note icon indicates additional or supplementary information about the action activity or concept Notes are shown in bold type General Safety General safety precautions must be followed when using this LLOYD INSTRUMENTS prod uct Failure to observe precautions and warn ings may result in damage to the equipment or injury to personnel It is understood that safety rules within compa nies vary If a conflict exists between the mate rial contained in all LLOYD INSTRUMENTS User s Guides and the rules of a company us
82. osen the motor securing clamp Pull the motor upwards and pull the pulley downwards until the pulley can be removed from the end of the motor shaft Remove the motor from the casting Remove the old belt if still fitted by holding the front end pulling it forwards and over the blade spindle then pulling it rearwards and away from the casting Position the rear of the new belt under the motor casting Hold the front end of the new belt pull it for wards and over the blade spindle then lower it onto the blade spindle pulley Refit the motor and motor pulley noting that the 3 grub screws should be located into the 3 slots machined into the motor shaft Check the belt tension as shown earlier Shown Loosened drive belt 80 PET Plus User Manual 14 6 RESULT DISCREPANCIES Insufficient drying is by far the most common problem which leads to low results and high variance between results The following is a list referring to some items that can also contribute to unexpected IV results from the equipment Sample condition or size resulting in variable results e Dirty or hot follower will give false high results e New die O ring required low IV e Inadequate gas pressure e g empty bottle e Poor vacuum to Dryer tubes will give low and variable results e Poor drying procedure will give low and variable results e Dryer temperature incorrect e Holes in probe rod blocked e Barrel inadequately
83. re required Cut the bottle necks from the bottles as close to the threaded portion as possible using tin snips or a small clean hacksaw Polymer plaques thick sheet samples or chunks of polymer extrudate should be cut using tin snips or a small clean hacksaw until they are small enough to fit into the pulverisette sample inlet port Using tongs place the selected sample or samples in a Dewar Flask containing sufficient liquid nitrogen to immerse the sample completely WARNING ALWAYS WEAR SAFETY GLASSES AND HEAT RESISTANT GLOVES WHEN HANDLING LIQUID NITROGEN WHICH IS AT 196 C Leave the samples immersed in the liquid nitrogen until the liquid nitrogen has ceased to boil showing that the sample has been cooled to the correct temperature Ensure that a clean collecting bowl is fitted to the bottom of the grinder Start the motor on the industrial grinder Carefully remove the cooled sample from the liquid nitrogen using tongs and place it in the safety interlock sample part of the pulveriser Open the interlock to drop the cooled sample into the sidearm and immediately lift and lower the plunger arm to push the sample onto the pulveriser blades Switch off the motor as soon as pulverisation has ceased usually a few seconds after lowering the plunger arm Wait until the rotor has stopped then unclip the receiving bowl containing the coarsely chipped sample Clean the pulveriser using a jet of clean compressed air or nitrogen to r
84. reference thermometer True Temp 301 2C Measured Temp 300 0C Change Clear True Accept Points Cancel Press the key under ACCEPT to correct the measured temperature value If a calibration point had already been entered at 300C or approx this value a warning message will be displayed Press the key under OVERWRITE POINT to accept this new calibration point The measured temperature value will now change to the entered value True Temp 301 2C Measured Temp 301 2C Change Clear True Accept Points Cancel The system will now cause the barrel temperature to change and stabilise at the corrected temperature value True Temp 300 0C Measured Temp 300 0C Change Clear True Accept Points Cancel Press the ENTER key two times to exit the temperature calibration screen PET Plus User Manual 85 15 3 PRESSURE CALIBRATION Note that an accurate pressure gauge is required for this procedure The barrel pressure is calibrated by measuring the actual pressure and entering this value into the system Press the key under CAL PRESSURE to display the Pressure Calibration screen Nitrogen Gas is OFF Measured Pressure 0 4Bar Gas Cal View View On Point Points Readings This screen indicates the gas status Nitrogen Gas is Off and also displays the measured pressure Check that the measured pressure is OBar 0 1Bar Note that the Zero reading can vary slightly with changes in atmospheric pressure If the measured p
85. ressure is not OBar 0 1Bar press the key under CAL POINT to display the cal point screen True Pressure 0 OBar Measured Pressure O 4Bar Change Clear True Accept Points Cancel The true pressure should automatically display 0 0Bar If it does not show 0 0Bar press the key under CHANGE TRUE then enter 0 0Bar The display will now show 0 0Bar for the true pressure Press the key under ACCEPT to correct the zero pressure reading Nitrogen Gas is OFF Measured Pressure 0O OBar Gas Cal View View On Point Points Readings 86 PET Plus User Manual If a calibration point had already been entered at OBar or approx this value a warning message will be displayed Press the key under OVERWRITE POINT to accept this new calibration point Press the ENTER key to return to the Pressure Calibration screen Fit the barrel blanking nut and washer to the bottom of the barrel Connect a reference pressure gauge to the top of the barrel Press the key under GAS ON to apply pressure to the barrel Adjust the gas regulator on the right hand side of the equipment to apply approx 30Bar as measured by the reference pressure gauge Allow the pressure to stabilise approx 1 minute then measure the actual pressure using the reference pressure gauge and compare with the measured pressure If the measured pressure is not the same as the reference pressure 0 1Bar press the key under CAL POINT to display the cal point screen
86. s batch Each category contains several related tests Select a category and press Next for a more detailed list of the tests within that category PET Plus User Manual 95 Click on the PET icon then click on the NEXT button Click on the IV TEST Icon then click on the FINISH button This action will automatically create the Test File then display the TEST CONFIGURATION screen Enter the required test temperature and the die dimensions as shown on the die certificate lf sample identification is required for traceability of results a pre test dialog can be displayed to enter this information To define any pre test questions click on the PRE TEST QUESTIONS button on the right hand of the screen to display the EXTRA RESULTS screen shown Click on the NEW button to display the EXTRA RESULTS TYPE screen then select which type of question is required 96 PET Plus User Manual You must choose which type of test is going to be performed in this batch Press Back to return to the other categories L IV Test lt Back i Fnish Cancel Help x Basic Settings Results Pre Test Base Sig Petes Test Temperature Post Test am C Questions Die Internal Diameter 0 0508 cm J Die Length haz em Test Options El Test Automation m Video Capture Ej DAQ Device E Machine Settings m Cancel x EESE Extra Results Type i what type of Extra Result should be asked
87. scosity IV and the degradation rate according to the ICI algorithm for PET Although primarily designed to test hygroscopic polymers in an oxygen and water free environment the flow properties viscosity and degradation of most polymers may be tested The range of IVs that can be measured using the available dies is shown below Die IV Range IV Range Internal at at Diameter cm 284 C 295 C 15 thou 0 0381 0 43 to 0 62 NA 20 thou 0 0508 0 53 to 0 70 0 70 to 0 83 30 thou 0 0762 NA 0 74 to 1 14 40 thou 1 1016 NA 0 93 to 1 43 10 PET Plus User Manual 1 6 PET PLUS ADVANTAGES k 2 Avoids handling toxic chemicals which are not only expensive but are costly to dispose of Crystalline samples can easily be measured as crystallinity INCREASES solubility DECREASES Samples can be taken directly from the plant to measure IV of incoming raw material e IV of regrind virgin polymer mixture Drier Efficiency e Drop of IV in extruder e Target value for moisture determination e Melt stability degradation rate e IV in finished product re grind Relatively easy test to operate does not need skilled laboratory staff so shop floor staff can easily be trained to obtain reliable and consistent results Saves time quicker than the solvent method results can be obtained in twenty minutes Saves money after initial cost of equipment and accessories electricity and nitrogen gas are the only on going costs
88. se connector on the rear of the drier block Shown Connection at the drier block PET Plus User Manual 23 3 12 CONNECTING THE DRIER BLOCK TO THE MAINS Connect the mains supply lead to the switched and fused input connector on the side of the drier block The mains switch has an internal lamp and the equipment is powered when the lamp is lit Only connect to the supply specified on the Serial Number nameplate situated alongside the mains input connector The front panel of the drier block also has an indicator lamp to show when the equipment is powered The installer shall not position the equipment so that it is difficult to access the disconnect device The power cord shall be replaced only by an adequately rated power supply cord 24 PET Plus User Manual SEGENSWORTH EAST FAREHAM HAMPSHIRE ENGLAND P015 STT TEL 44 0 1489 574221 VOLTAGE 230V 10 FUSE TYPE FREQ RANGE 50 60 Hz POWER RATING 2000 vA i TYPE No POLYMER DRYER 012778 _ SERIAL No i Shown Mains input connector VACUUM POWER Oo ied 1 Shown Front panel on drier block 3 13 CONNECTING THE PUMP TO THE MAINS The pump is powered from the drier block for ease of use Connect the special lead between the mains input connector on the rear of the pump item 1 to the mains outlet on the rear of the drier block The pump is switched on and off by the Vacuum Power switch on the front panel of the drier
89. sembled correctly after cleaning It is also important that the PET Plus is set to the Pre Test screen ready for testing THIS PROCEDURE IS PART OF THE MAIN PROCEDURE SHOWN IN SECTION 7 7 Select a sample phial and turn the vacuum valve in the plastic vacuum tube to closed lever is at 90 degrees to the vacuum pipe Press the release lever on the front of the quick connector so that the metal tube springs up out of the connector Note that the quick release connector has a sealing valve so that the vacuum is not released from the other sample phials PET Plus User Manual 59 Press the key under PURGE to allow a low volume of nitrogen gas to flow through the barrel to displace any air that may be present Allow the gas to flow for a few seconds to ensure that the barrel is full of nitrogen Place the standard filling funnel onto the top of the barrel Place the open metal end from the sample phial into the top of the filling funnel Turn the vacuum valve in the plastic vacuum tube so that the lever is in line with the vacuum pipe to release the vacuum A slight hissing sound will be heard as the vacuum draws hot dry nitrogen into the sample phial Press the key under GAS OFF to stop the flow of nitrogen gas Unscrew the top cap from the sample phial then carefully pour the polymer from the phial into the top of the filling funnel Remove the filling funnel from the top of the barrel Insert a clean follower
90. sible under the law Cancel ig NEXYGEN Plus PET loj xj License Agreement Please take a moment to read the license agreement now If you accept the terms below click l Agree then Next Otherwise click Cancel Software Licence Agreement You will note that your disk and Licence Registration Form is issued with a Licence Number This is used by Lloyd Instruments Limited as a cross reference to you the customer and to the particular version of software that you have purchased This number must be quoted in any correspondence relating to this software therefore you must carmnlata tha Licanca Daaictratian Carm and ratiurn it ta tha xl Do Not Agree C Aoree Cancel lt Back nerven pus per T NEXYGEN Plus PET Information NEXYGENPIus PET IN THIS RELEASE NEXYGENPlus PET allows you to perform tests on a PET Plus series machine GENERAL INSTALLATION 1 Prerequisites The NEXYGEN Plus installation will not affect an earlier x Cancel lt Back i i NEXYGEN Plus PET ioixi Shared Folder 1 ALM Please check the location of the shared folder If running NEXYGEN Plus as 4 multi user system with more than one workstation this shared folder should be amended to point to a common location such as a file server Location C Program Files Lloyd Instruments Ltd NEXYGEN Plus PET Shared Cancel lt Back i The dialog
91. siten 2 9 Required Equipment amp Materials 2 10 Optional Spare Items 0 2 11 Optional Equipment e 3 0 INSTALLATION ccccee 3 1 Considerations sicscicvnisiscaswszeasaniiendsleeis 3 2 Safety Considerations 00 3 3 Siting the Equipment 0 3 4 Connecting to the Mains 3 5 Connecting the Nitrogen Supply 3 6 Connecting the Probe 0 3 7 WAC UU Pump 3 8 Filling the Pump with Oil 3 9 Fitting the Oil Mist Filter 3 10 Connecting the Vacuum Pump 3 11 Connecting the Pump to Drier 3 12 Connecting Mains to Drier 3 13 Connection Mains to Pump 3 14 De gassing the Oil eee 3 15 Setting for Maximum Vacuum 3 16 Polymer Chip Grinder 0 3 17 Industrial Grinder essiisivtssinnsteisincdsiauts 4 0 SETTING UP THE VISCOMETER 4 1 Initial Configuration ccceeee 4 2 Over Temperature Device 4 3 Setting the Test Temperature 4 4 Which Test Temperature to Use 4 5 Which Die Size to Use 0 5 0 CREATING A TEST SETUP 51 Default Test Setups 5 2 Renaming an Existing Test Setup 5 3 Creating a New Test Setup 5 4 Defining a Test Setup cccee 5 5 Password Protection ccccce 6 PET Plus User Manual TABLE OF CONTENTS 6 0 6 1 7 0 7 1 1 2 7 3
92. t The Charging screen will be displayed PPP PrP rrr Pro PP gt o gt o gt gt gt gt PPP rrr rrr gt gt gt gt gt gt gt gt gt gt gt gt Push gently on the charging tool Note that the gas will be automatically switched on again to provide a low volume of nitrogen gas through the barrel to prevent any air from entering it during this charging period 46 PET Plus User Manual 7 8 APPLY PRESSURE TO THE FOLLOWER Apply slight downwards pressure onto the top of the follower using the charging tool This part of the test takes one minute and the screen indicates this time period by a series of gt gt gt moving across the screen At the end of the time period the equipment will beep and the Fit Probe screen is displayed Fit probe then press GO 7 9 FIT THE PROBE TO THE BARREL Using heat protecting gloves screw the probe onto the top of the barrel and secure the large nut hand tight Press the green GO key to indicate that the probe has been fitted The Pre Conditioning screen will then be displayed Set Temp 295 0C Barrel Temp 295 0C Pressure 24 35Bar Probe 6 15mm Pre Conditioning Gas Off Note that the gas will be automatically switched to full pressure to perform the test The gas pressure inside the barrel is displayed on this screen If the required gas pressure is known testing a sample with a known IV then the pressure can be checked and altered at this stage
93. t UTC e g British Summer Time or if the equipment is used in a country other than the UK The equipment can store up to 600 test results internally and the statistics and results can be easily viewed on the control console display If 600 tests are already stored then when the next test is performed the first test will be deleted to allow the new test to be stored This feature allows the last 600 test results to be stored There are connection points on the cabinet for the nitrogen gas supply and the optional computer A fused switched socket is fitted for connection to the mains electricity supply Ancillary equipment developed for use with the PET Plus to handle the grinding drying and transfer of samples is available as either a package or as individual items 1 3 EQUIPMENT OPERATION When the equipment is first switched on the Select Test screen is displayed as shown below Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit When this Select Test screen is initially displayed the heaters and nitrogen gas valves are automatically switched off The heaters will operate when any of the test set ups are selected by pressing the key under SELECT However note that there is a special test set up called TRAINING and the heaters do NOT operate when this set up is selected The nitrogen gas valves are can only be operated when the relevant screens are displayed and the gas
94. th tweezers then remove any polymer from the sides and faces using a sharp blade WARNING Wear cut resistant gloves when cleaning 50 PET Plus User Manual Insert the charging tool into the top of the barrel until it touches the top of the follower Push the charging tool completely down through the barrel to remove the remaining polymer and the follower Hold the follower with tweezers then remove any polymer from the sides and faces using a sharp blade Fold a cleaning patch in two then place over the tip of the barrel cleaning tool Push the cloth into the top of the barrel using the tool and push the tool down completely through the barrel Carefully remove the cloth from the barrel cleaning tool and withdraw the tool upwards Visually inspect the barrel and if necessary use another cleaning cloth until the barrel is completely free from polymer and the inner bore is shiny A final cloth coated with a small amount of silicone oil may be used to coat the barrel and make future cleaning easier WARNING The cloth and barrel cleaning tool may become hot during the cleaning 4 process Wear heat protecting gloves when handling these items Polymer fumes may be emitted from the top of the barrel during the visual examination process Wear protective glasses or goggles when viewing the interior of the barrel If traces of polymer are still present in the barrel bore these can be removed using the wire brush Note that this procedure sho
95. that the sound will change when the die is clean Press the key under GAS OFF to release the gas pressure check that the display shows nominally zero then remove the top cap using the tightening tool 7 13 STORING THE DIE If another test is not going to be performed remove the die from the barrel using the barrel cleaning tool and store safely Note that the die will be hot after cleaning Do NOT leave the die in the barrel for long periods when not in use 7 14 CLEANING THE FOLLOWERS The followers are cleaned by heating to burn off the excess polymer Note that polymer fumes may be emitted from the followers during the heating burning process so this should be carried out in a fume cupboard or an enclosed laboratory oven There are 3 ways that they can be heated 1 Heated on a hot plate 2 Placed on a wire gauze on a tripod stand then heated using a bunsen burner under the gauze 3 Placed in a muffle furnace using a maximum temperature of 450 C Do not handle the hot followers with tweezers or tongs as this might damage them by causing distortion or indentation which would render them useless After the followers have cooled brush off the film of ashed polymer using a brass wire brush 52 PET Plus User Manual Finally the followers should be polished until shiny with a Scotchbrite pad available from any super market Do NOT use a file or similar tool to clean the followers because any scratches or similar marks will af
96. tic vacuum tube lever is in line with the vacuum pipe to release the vacuum A slight hissing sound will be heard as the vacuum draws hot dry nitrogen into the sample phial PET Plus User Manual 67 Press the key under GAS OFF to stop the flow of nitrogen gas Unscrew the top cap from the sample phial then carefully pour the powder from the phial into the top of the filling funnel Remove the filling funnel from the top of the barrel Insert a clean follower into the top of the barrel Insert the charging tool into the top of the barrel Immediately press the green GO key to start the test The Charging screen will be displayed 68 PET Plus User Manual 11 0 PRODUCTION DRIER 11 1 TESTING PRINCIPLE The production drier hopper is checked by collecting dried polymer from the bottom of the hopper then testing it WITHOUT FURTHER DRYING to check the drier efficiency This can be used to check the drying temperature drying time and desiccant The polymer MUST be transferred to the PET Plus barrel using a procedure that ensures that the polymer does not come into contact with any external air The Polymer Chip Transfer Vessel is designed for this purpose 11 2 POLYMER CHIP TRANSFER VESSEL This is a metal cylinder containing a central dispensing mechanism that splits the cylinder into 2 chambers Nitrogen is passed through the two chambers to purge any air from the device One chamber has a Schrader quick release inlet with
97. ue a warning message will be displayed Press the key under OVERWRITE POINT to accept this new calibration point Press the ENTER key to return to the Probe Calibration screen Set the calibration micrometer to 25 000mm Check that the measured probe is 25mm 0 01mm If the measured probe is not 25mm 0 01mm press the key under CAL POINT to display the cal point screen True Probe 25 000mm Measured Probe 24 829mm Change Clear True Accept Points Cancel The true probe should automatically display 25 000mm If it does not show 25 000mm press the key under CHANGE TRUE then enter 25mm The display will now show 25 000mm for the true probe Press the key under ACCEPT to correct the zero probe reading True Probe 25 000mm Measured Probe 25 000mm Change Clear True Accept Points Cancel PET Plus User Manual 89 If a calibration point had already been entered at 25mm or approx this value a warning message will be displayed Press the key under OVERWRITE POINT to accept this new calibration point Press the ENTER key to return to the Probe Calibration screen Reset the calibration micrometer to 0 000mm Check that the measured probe is Omm 0 01mm If the measured probe is not Omm 0 01mm enter a new calibration point overwriting the previous point Reset the calibration micrometer to 25 000mm Check that the measured probe is 25mm 0 01mm If the measured probe is not 25mm 0 01mm e
98. uld not be required if the barrel is cleaned immediately after each test Put the cleaning tool through the loop in the wire brush handle then move the brush up and down the length of the barrel to remove the traces of polymer Use another cleaning cloth until the barrel is completely free from polymer and the inner bore is shiny Do NOT use the brush until after the barrel has been cleaned using one or more cleaning clothes otherwise the brush will become clogged with polymer PET Plus User Manual 51 7 12 CLEAN THE DIE BORE The die bore can only be cleaned by blowing through with high pressure nitrogen Do NOT try to clean the die bore by pushing wire etc through it If the wire breaks inside the die then a new die may be required Always clean the die immediately after use even if another test is not going to be performed after wards Place the die into the recess of the die retaining nut with the end containing the O Ring facing up wards Screw the die retaining nut with the die to the bottom of the barrel and hand tighten using the tightening tool Loosen off by about 1 10th of a turn about 30 degrees otherwise it will be very difficult to remove once it has heated up and expanded Fit the top cap to the top of the barrel and tighten securely using the tightening tool to seal the barrel Press the key under FULL to apply the nitrogen gas to the barrel Wait until the gas can be heard flowing freely through the die noting
99. up contains separate results storage so that the statistics for each type of test can be easily viewed so a different test set up should be used for Adifferent polymer m Adifferent production drier or extruder Therefore a different test set up should be used to store the test data for say E Incoming resin m Production Drier number 1 m Production Drier number 2 etc PET Plus User Manual 35 5 2 RENAMING AN EXISTING TEST SETUP Display the Select Test screen to select one of the pre defined test set ups Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Edit Press the key under gt or lt to select the test set up that is to be renamed When the required test set up is displayed press the key under EDIT to display the edit test screen Press a key to select an option 20THOU_284C Rename Global Delete Setup Press the key under RENAME to display the rename test screen Rename Test 20THOU 284C 20THOU_284C Clear All Press the key under CLEAR ALL to delete the existing name then enter the required name using the keypad This name could be a supplier name or a production ID such as drier identification Press the ENTER key to return to the edit test screen 36 PET Plus User Manual 5 3 CREATING A NEW TEST SETUP Display the Select Test screen Select the required test 20THOU_284C 0 Samples Date and Time 01 05 2008 14 44 Select gt Ed
100. valves are automatically switched OFF when any other screen is displayed PET Plus User Manual 9 1 4 EQUIPMENT USE The Incoming or Supplied Resin can be checked before acceptance of delivery The Dried resin can be checked daily from the drying hopper to check the efficiency of the drying heaters and or drying desiccant The preforms can be checked before and after storage to monitor the IV drop in the extruder and also to check the suitability of the storage area humid storage conditions will reduce the IV of the preform and cause problems during the blow moulding stage Note that the drier and preforms CANNOT be checked using the solution method because this checks the IV of the polymer and NOT the changes in IV due to the production process The PET Plus also reports the Thermal Degradation Factor which is a combination of the Thermal Degradation Rate and the Hydrolytic Degradation Rate It is found in practice that the IV drop from polymer chip to preform is usually in the range of 0 02 to 0 03 IV 1 5 MEASUREMENT RANGE The IV measurement range is approximately 0 45 to 1 40 using dies from 0 015 in 0 0381cm to 0 040 in 0 1916cm Every die is machined to be 0 5 in 1 27cm long and has a very accurately defined bore Each die is supplied with a calibration certificate which states the exact size of the die and these values are to be entered into the test parameters The software calculates Intrinsic Vi
101. vessel to the production area If a nitrogen supply is available at the sampling site either 1 Reconnect the nitrogen to the Schrader quick release inlet valve and allow the nitrogen to flow for a minute 2 Have a flexible hose that can be aimed around the chip outlet Remove the top cap and load with the DRY sample as quickly as possible The top chamber should be filled until it is be tween half full and full of polymer The picture above shows a flexible hose assembly connected to the inlet of the extruder IMMEDIATELY replace the top cap Take the transfer vessel containing the dry sample back to the PET Plus The samples do not have to be tested immedi ately because they will be kept dry for several hours if the top or bottom caps are not removed If the samples are to be stored for a time it is recommended that the low pressure nitrogen supply is reconnected to the Schrader quick release inlet valve PET Plus User Manual 71 11 6 TESTING THE POLYMER E NOTE It is very important that the Die the Barrel and the Follower are scrupulously clean gt and have been assembled correctly after cleaning It is also important that the PET Plus is set to the Pre Test screen ready for testing THIS PROCEDURE IS PART OF THE MAIN PROCEDURE SHOWN IN SECTION 7 7 Press the key under PURGE to allow a low volume of nitrogen gas to flow through the barrel to displace any air that may be present Allow the gas to flo
102. w for a few seconds to ensure that the barrel is full of nitrogen Place the standard filling funnel onto the top of the barrel Press the key under GAS OFF to stop the flow of nitrogen gas Remove the bottom cap from the transfer vessel Place the bottom of the transfer vessel onto the top of the filling funnel Turn the dispensing lever until the lever is point ing downwards This will dispense a quantity of polymer into the filling funnel Remove the filling funnel from the top of the barrel Insert a clean follower into the top of the barrel Insert the charging tool into the top of the barrel Immediately press the green GO key to start the test The Charging screen will be displayed Refit the bottom cap to the transfer vessel Turn the dispensing lever until the lever is pointing upwards This allows the polymer to enter the dispensing mechanism ready for the next test It is recommended that the low pressure nitrogen supply is reconnected to the Schrader quick release inlet valve 72 PET Plus User Manual 12 0 MOLTEN EXTRUDATE 12 1 TESTING PRINCIPLE The extrudate from a spinneret or bleed point is checked by collecting molten polymer then testing it WITHOUT FURTHER DRYING The polymer MUST be transferred to the PET Plus barrel using a procedure that ensures that the polymer does not come into contact with any external air The Sample Melt Pot is designed for this purpose 12 2 SAMPLE MELT
103. wn below will be displayed if the barrel is not at the required temperature Set Temp 295 0C Barrel Temp 292 0C 20THOU_295C Waiting for barrel temp to stabilise Suspend This screen will automatically change to the Pre Test screen when the barrel has stabilised at the required temperature Note that the equipment MUST be set to the Pre Test screen BEFORE trying to test a sample PET Plus User Manual 43 7 2 TEST PROCEDURE The test procedure consists of the following actions Check that the barrel is clean Prepare a clean follower and filling funnel Clean the die bore Purge the barrel with nitrogen gas Insert the polymer into the top of the barrel Insert the follower into the top of the barrel Press the GO key Apply pressure to the top of the follower using the charging tool for one minute Fit the probe to the top of the barrel Wait until the test has finished Clean the barrel die and follower 7 3 CHECK THAT THE BARREL IS CLEAN Fold a cleaning patch in two then place over the tip of the barrel cleaning tool Push the cloth into the top of the barrel using the tool and push the tool down completely through the barrel Carefully remove the cloth from the barrel cleaning tool and withdraw the tool upwards Visually inspect the barrel and if necessary use another cleaning cloth until the barrel is completely free from polymer and the inner bore is shiny CAUTION The cloth and barrel cleaning tool may b

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