Dynisco LCR7000 Series Operating Manual Download Page 37

Page: 37 / 116

LCR7000 & RHEOSIGHTS P/N: 974194 |

Rev: A

ECO: 52468

www.dynisco.com

From lab to production,

providing a window into the process

-37-

Plotting and Analyzing your Data

Once a test run is completed you will want to analyze and Plot your data into a graph to

easily analyze your test. You will need click on the "Analyze" button at the top of the

RheoSights Main Operation page.

•

Browse the list of experiments to find the data you want to

plot

•

Highlight

the charges you wish to plot and press the “Plot

Selected” button. This will plot your charges on screen for

you

Plotting

Summary of Contents for LCR7000 Series

Page 1: ...N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 1 Setting the standard for Evaluating Polymer Melt Flow Characteristics Operating Manual Dynisco LCR7000 Series RheoSights ...

Page 2: ...8 RheoSights Reports 47 Formulas Used in Data Analysis 54 Apparent Shear Rate Calculation 54 Apparent Shear Stress Calculation 54 Apparent Shear Viscosity 55 Volumetric Flow Rate Calculation 55 Mass Flow Rate Calculation 56 Introduction to Rheology 57 Simple Shear Deformation 57 Viscosities of some Common Materials 62 62 Pseudoplastic 63 Dilatant 63 Thixotropic 63 Rheopectic 63 Where η is viscosit...

Page 3: ...89 The Non Newtonian Index 89 Troubleshooting 91 Parts List 94 DIES and ORFICES 94 Die Design and Configuration 97 Supplied Hand Tools 98 LCR 7000 SPARE PARTS LIST 100 Navigating the Keypad 103 The Keypad 103 Keypad Definitions 103 Conversion Factors 105 Example Runs 106 Support Vendors 110 RAM Rate Shear Rate Table 112 Reference Books 113 Glossary of Terms 115 ...

Page 4: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 4 ...

Page 5: ...r Italics Rheological items which have defining equations presented in this manual are shown in italics Bold Italics These are parameters that are set from the front panel on the rheometer i e Melt Time Delay Time etc These parameters are entered into the rheometer s control programs via the rheometer keypad BOLD ALL CAPITALS This indicates an actual key found on the rheometer keypad Usage is as f...

Page 6: ... com or https shopeu dynisco com Account registration is required To help us handle your questions as quickly as possible have the following items ready before you call Rheometer name and model number Rheometer serial number on back panel of the unit Computer system make and model Current version of software Found at the bottom on the main operating page of the RheoSights software DYNISCO Customer...

Page 7: ...e factory if necessary Typical laboratory benches are too high for efficient use of the rheometer Cleaning can be difficult and requires awkward hand positions and forces which could lead to carpal tunnel syndrome or back discomfort We strongly suggest a bench height of 29 inches desktop height for an average height operator Place the front of the rheometer flush with the edge of the table This wi...

Page 8: ...r The thickest heaviest of these is used for the rheometer Connect this thickest cord to the back of the rheometer base and into the isolated filter bank 3 in the power box Power to the PC and monitor should connect to the isolated filter bank 1 The printer if used can be connected to any remaining outlet The data processing system consists of an Edge Device and the RheoSights software package Con...

Page 9: ...t using this instrument Install both of the Dynisco PT s into the rheometer barrel and connect the coiled interface cable from the rheometer base to the PT s See Pressure Transducer Installation Section for more details Be sure Sensor 1 is attached to barrel 1 and Sensor 2 is attached to barrel 2 Models 7000 7001 have Load Cell measurement capability The Load Cell is a round blue unit with a 6 pin...

Page 10: ...ntil the sensor you wish to turn off Sensor 1 Sensor 2 or both is shown on the control panel display Press the Edit Smart Key and scroll through the sensor selections until the display reads Device Not Entered and press the Select smart key The sensor that you selected is now turned off After following all the previous steps be sure there is nothing to prevent the crosshead on the rheometer from m...

Page 11: ... been made If still nothing happens proceed to the troubleshooting section An update of the RheoSights software will be automatically pushed to you if your Edge Device is connected to the Internet Please make sure you have good internet connection if you want to receive the update You can also manually download newer version of the Software from our website iot dynisco com Home Download Firmware i...

Page 12: ... firmware IC evenly This will prevent socket damage and bent firmware IC leads Replace the old LSB chip with the new chip labeled LSB Repeat the same procedure for the MSB chip see figure above Replace U3 if supplied with chip labeled U3 v2 0 in the same manner as the USB and LSB chips Confirm proper firmware orientation by replacing the firmware ICs with their notches matching the socket notches ...

Page 13: ...en both Socket Head Cap Screws securely 4 Pivot the Die Swell Laser into operating position If pivot tension is too low the Phillips head screw on the back of the hinge can be tightened to provide the desired pivot tension 5 Install the supplied cable to the Die Swell Laser and connect to any of the USB ports on the Edge Device Configuration of Edge Device to recognize Die Swell Laser 1 Turn the E...

Page 14: ...es Be sure the outlet used to power the rheometer is properly grounded If a thermometer is used to calibrate the temperature on the rheometer it will contain about 8 grams of mercury Every lab with mercury thermometers or equipment containing mercury must be prepared for breakage Note that mercury exposed to air evaporates at room temperature producing an invisible tasteless odorless and dangerous...

Page 15: ...the area between the crosshead and the rheometer swing arm is clear prior to any rheometer movement The large red EMERGENCY STOP button when pressed will stop any rheometer movement and allow the pulley system to be rotated by hand if needed The EMERGENCY STOP button is like a clutch on a car When engaged it disconnects the motor from the driving mechanism when released it re engages any current c...

Page 16: ...he rheometer barrel Repeat the process with fresh patches until the patches come out clean Turn the rheometer power switch ON If you hear a continuous beeping sound turn the rheometer off and be sure you have connected the load cell correctly as described under the Getting Started section If the rheometer s front panel lights up but there is no movement on the crosshead shut the rheometer off pull...

Page 17: ...a comfortable position for you to load the sample Don t be afraid of opening it too far Use the PYREX beaker to scoop pellets from the sample you wish to run Get the phenolic filling funnel and place it directly over the top of the barrel The lip on the base of the funnel will fit onto the top of the barrel insulator Holding the funnel in one hand gently pour about 2 3 of the pellets from the beak...

Page 18: ... the bottom limit switch setting which is located about 3 mm 1 8 above where the piston and die will contact To abort the Purge mode press the QUIT key Pressing the SHIFT than up key will move the ram back to the Park Position Loosen the knob on the swing arm and pull the swing arm and barrel forward for cleaning Put two patches directly over the barrel about 1 2 way overlapped Using the cleaning ...

Page 19: ...e barrel it cools down quickly The longer it is out the longer will be the wait for the temperature to stabilize Minimizing the time the die stays out of the rheometer will help to increase the number of tests you can run When the temperature on the front display is stable you will hear a beep and the display will read READY You can now begin your next test Loading material will cause a small temp...

Page 20: ... run is very simple We ask the rheometer to move at only one speed 35 mm min ca 1 4 min and take measurements at positions in the barrel that are 8 7 mm apart 15 seconds per measurement Additionally we ask the rheometer to pause stop plunger movement for 15 seconds after each data point is taken If RheoSights isn t already running on your Edge Device now is a good time to start it Double click on ...

Page 21: ...d and the plunger guide bushing is in place click the RUN button on the Rheometer Control screen of RheoSights and fill in your test sample information and click on OK to start the test The test will automatically acquire the data purge the barrel of remaining material move back to park position and send the data to the Edge Device What s happening during the run When RUN OK is pressed on the Rheo...

Page 22: ...rnight will do an excellent job of cleaning degraded material off the piston shaft the outside of the die and on the die holder nut Caution Be careful not to breathe in oven cleaner vapors If running at high temperatures 300 oC you may wish to coat the outside of the die and Pressure Transducer with anti seize material prior to placing it in the die holder nut This will make it much easier to clea...

Page 23: ...ecause the connector is not detected by the Edge Device For the second case try rebooting the Edge Device for one or two times If that does not solve the problem your Edge Device may not have the proper driver or you may need a replacement for the connector contact Dynisco for a solution Your RheoSights security protection allows you to add your own password protection for the software When you st...

Page 24: ... it is important not to interrupt the rheometer when it first starts up and finds the HOME position Charge This is the run number the rheometer includes with the data Normally when a new test is started this value should automatically update to the next corresponding number This value is automatically incremented every time a test is done The run number also includes the version of the software e ...

Page 25: ...up icon located in the tool bar the RheoSights Main Operation page The Setup page contains ten preset testing conditions for some standard industry materials Choose the test for the material you are running or change the testing conditions to your liking Select the test you wish to run and click on the Send icon to send the testing conditions to the rheometer and move directly into the Main Operat...

Page 26: ... minimum amount of time the material will be exposed to test temperature in the barrel before the first rate begins Park Position The Park Position is the position where the ram remains idle and the position to which the ram returns after completing a run or sample purge Melt Pause Delay The Melt Pause Delay is the amount of time the plunger will stay idle at the start position For low viscosity p...

Page 27: ...or you may also create your Data Point Setup individually one point at a time To create a new set of data points for your test you can use the Auto Generate function of the toolbar above the datapoints table Type in how many points you want in End Point box start value of point 1 in Start Value box and end value of the last point in End Value box Select the value type Speed Control mm min or Shear...

Page 28: ...ew button to add a data point Remove Last to remove last point and Remove All to remove all data points If you are going to giving each point a Ram Rate you will have to click the Generate Shear Rate button to complete the data point information If you are setting up your data points individually buy Shear Rate you will have to click on Generate Speed Control for each point to complete the data po...

Page 29: ...red from the data and when a steady state algorithm determines that the received data is steady the computer grabs the average force values stores it and proceeds to the next point The Manual mode is also active at the same time with this setting this gives the operator the option to presses the Acquire icon to take the data reading and move onto the next point Four Steady State Algorithms Univers...

Page 30: ...for a specified number of seconds The total delay between two data points will be the delay time plus the actual plunger movement time For example if all rates are 8 mm min and all positions are 8 mm apart then the measurement time is 1 0 minutes plus an additional Time Delay of 180 seconds would make the total time between points 4 0 minutes For thermal degradation runs increase or decrease the T...

Page 31: ...Click on the Auto Calculate button at the top of the page to automatically calculate the information of your new die Once you have filled in all the information for your new die click Select button to select this die for the test Length This is the orifice length or die length It is the length of the capillary region of the die If you know the L D of the die multiply by the diameter to get the len...

Page 32: ... prepared dried mixed check for contaminates Rheometer on 20 minutes Correct Die in rheometer Sufficient anti seize coating on die nut especially at high temperatures 300 C Correct program being run Hand tools in position packing funnel and tool cleaning drill bit etc Are die diameters within spec passed G0 No Go gage ASTM ISO DIN Force calibration and R Cal OK Temperature calibration OK Die lengt...

Page 33: ...er Steady State Universal mode with a 0 second delay between each data point HAMA Laser Micrometer How it works The laser sends out a UV pulse that is picked up by a series of diodes 8188 to be exact When the light is blocked the diode registers no light and the side of and object from edge to edge can be determined If a HAMA LASER micrometer is attached cable connected to the Edge Device with the...

Page 34: ...is can easily be resolved by following the instructions on the alert message For the second case try rebooting the Edge Device one or two times If that does not solve the problem either your Edge Device does not have the proper driver for the Laser or you need a replacement for the connector contact Dynisco for a solution If the Laser is set and values can be seen from the Main Operation page you ...

Page 35: ...eometer sensors to a zero value for the LC Load Cell and or PT Pressure Transducer Show the latest test result report Identify the type of Load Cell and PT sensor Laser settings Park Position The position from which the ram remains idle and the position to which the ram returns after completing a run or sample purge Moves the crossbar to the Home Position When you re ready to start your test press...

Page 36: ...data can be exported to a csv file by clicking Export to File after the test is finished or abort Types of data that can be shown and saved are Loadcell PT sensor data in Newton Loadcell PT sensor data in Pascal Plunger Speed in mm min Loadcell PT shear stress in Pascal Loadcell Force Difference of two consecutive data Shear Rate Temperature in Celsius Plunger Position in mm Loadcell PT shear visc...

Page 37: ...mpleted you will want to analyze and Plot your data into a graph to easily analyze your test You will need click on the Analyze button at the top of the RheoSights Main Operation page Browse the list of experiments to find the data you want to plot Highlight the charges you wish to plot and press the Plot Selected button This will plot your charges on screen for you 1 Plotting ...

Page 38: ... else b Shift an axis Put the mouse on an axis and you will see a two way arrow Drag the axis left right or up down to shift the axis c Select an area of the graph Just like you can select multiple files by holding down the left key and move the mouse you can do the same to select an area of the graph and the graph will focus on only that area d The build in toolbar If you hover your mouse around ...

Page 39: ...m From lab to production providing a window into the process 39 The basic info of the last test you selected will be shown at this section The full report including the data points can be shown by clicking the Show Full Report button 2 Test Info and Full Report ...

Page 40: ...inear and Logarithm Scale on the Graph The default scale for the data on the graph is logarithm scale but you can change it to linear scale on the left right and bottom axises anytime by clicking the button to Lin on the right of the axis data selections and switch back by clicking again 3 Log Values for the Data on the Graph ...

Page 41: ...t to Log Values button logarithm values of the result will be shown on the graph Click the button again and the data will be restored You can choose an algorithm to do curving fitting for the data on the graph by selecting from the list of Fitting Curves The curve will be plotted on the graph and the fitting parameters will be shown on the box above the Show Full Report button 4 Curve Fitting ...

Page 42: ...s designed to predict rheology test result that is not possible or not precise or simply not tested with the actual machine For example if you want to know the shear viscosity of the material at a very low shear rate of 0 01 1 s which is not possible with the LCR7000 you can use Power Law or Modified Cross model or Bird Carreau Yasuda model to fit the data then use the formula given to calulate th...

Page 43: ...lation Mode to switch to interpolation mode and do a curve fitting for the test The power law fitting curve is plotted from shear rate 0 500000 1 s The interval between two points on this curve is 1 which means you can hover on the curve and check the shear viscosity value for shear rate 0 1 2 3 4 5 499999 500000 1 s Notice that more points on the curve takes more processing time especially for co...

Page 44: ...ne tests which meet certain criteria see Appendix for details Furthermore Bagley Rabino corrected Shear Viscosity and Extensional Viscosity Stress Rate can be plotted based on the corrections If a single test is selected Rabino Corrected Shear Viscosity can be plotted Simply select it on for left axis or right axis If two or more tests that meet the criteria of Bagley correction are selected the i...

Page 45: ...ers MFR correlation which calculates melt flow rate of the material based on the test result Select the Test Load and Sensor input the melt density and click CALCULATE There are three types of special graphs First is the Entrance Pressure which shows the process of getting the entrance pressure for bagley correction 7 MFR Correlation 8 Special Graphs ...

Page 46: ...iding a window into the process 46 Second is the Rabinowitch Correction which shows the process of getting rabinowicth correction constants Third is Viscosity Temperature which offers the functionality to predict viscosity for a certain material under a certain temperature under development ...

Page 47: ...e or in the Analyze page On the Main Operation page click on the Report button and the latest test result is shown and it can be printed saved as pdf and saved as csv On the Analyze page the last 20 test reports can be shown based on your selection Click the Print button on the bottom of the popup report window and you will have the options to print it 1 Print Report using Printers including Micro...

Page 48: ...t being used to test apply a light coat of anti seize to the threads to the PT Port Plug and insert into the PT port Only hand tighten the Port Plug until the plug warms up to the barrel temperature Once the PT or the plug has had time to heat snug it tight with a wrench To turn off a sensor or to select another pressure transducer or load cell Press the SETUP button on the front control panel of ...

Page 49: ... Keys scroll Left or Right to locate the proper sensor you wish to install 6 Press the SELECT Smart Key to activate the sensor The Pressure Transducer or Load Cell you selected is now active Insures stability prior to Rate Sweep o It is often convenient to run a time sweep on a material to assess its tendency to degrade at the test temperature before collecting data as a function of rate PVC Examp...

Page 50: ...isco com From lab to production providing a window into the process 50 Note the test at 232 C does not extend much past 13 minutes this is because the test was stopped the die removed and the sample purged before it could degrade any further in the barrel ...

Page 51: ...tes PVC PP PET Example Rate Sweep Data Note the Newtonian like character of the PET at 285 C The PP shows some signs of turning toward a constant viscosity at lower rates but the PVC looks like a powerlaw fluid straight line throughout the sweep Constant Stress vs Constant Rate Constant stress tests on degrading material tested in the non Newtonian region have viscosity vs time curves which fall f...

Page 52: ...s of viscosity vs shear rate to be obtained Extrapolation to viscosity vs rate curves at zero time can also be accomplished with this technique How the viscosities vs rate curves are affected by time at constant temperature can then be evaluated In our in house lab we have found a single rheometer day to day reproducibility of the apparent shear viscosity in shear rate ranges of 10 to 1000 to be a...

Page 53: ...ance cones a matching cone is inserted and the overall length measured Capillary length is back calculated through trigonometry Piston tips and length are checked using hand or laser micrometers Force cells are calibrated using a calibration cell which is calibrated with dead weights that are NIST traceable NIST does provide standard reference materials for melt indexers which can be used on rheom...

Page 54: ...he barrel Dc diameter of the capillary die Example When the plunger moves at a rate of 20 mm min or 20 60 mm sec the Die diameter is 1mm and the Barrel diameter is 9 545 mm then 243 60 1 20 545 9 8 3 2 γ 1 sec Note all length units cancel out Apparent Shear Stress Calculation Formula for Shear Stress c b c p c b c p L D D F L R R F 2 2 2 π π τ Typical Units are Pascals Pa or megaPascals Mpa Where ...

Page 55: ...oise 10poise 1 Pa sec Where Sp speed of the plunger Db diameter of the barrel Dc diameter of the capillary die Example sec Pa 575 20 20 545 9 8 60 800 0 1 4 4 π η Volumetric Flow Rate Calculation Formula for Volumetric Flow Rate Time Distance 4 2 2 b p b D S R Q π π Where Rb radius of the barrel Rc radius of the capillary die Sp the speed of the plunger Db diameter of the barrel Dc diameter of the...

Page 56: ...econds then minutes g 10 111 6 or g min 11 16 or g sec 186 0 120 31 22 MFR NOTE1 Melt Flow also MFR ASTM D1238 is a mass flow rate measurement made at specific conditions of stress die dimensions and temperature which differ from material to material It typically uses units of g 10 minutes Note 2 Strictly speaking all calculation shown above are apparent values since they assume Newtonian behavior...

Page 57: ...ear Stress Force Area Shear Strain Displacement Gap Strain Rate Displacement Rate Gap τ γ γ F A x h x h In the simple shear geometry the gap and area remain constant throughout the deformation process Other definitions are used and depend upon the reference frame chosen for the observation The above definitions are common 1 Geometries of Deformation a Extensional Deformation ...

Page 58: ...the barrel until it is thin enough to fit through the die and you understand the extension aspect of the flow Finally in the capillary die the material immediately adjacent to the walls is stationary more on this assumption later yet the material in the center of the capillary is moving very fast The die wall is like the bottom plate in the simple shear geometry and the center of the stream is sim...

Page 59: ...l yield a straight line as illustrated in the next Figure The slope at any given point on the curve is the viscosity of the material at that shear rate Because the magnitude of the change in viscosity is frequently large it is often more convenient to make a log log plot The Newtonian region for materials on a log log plot of shear stress vs shear rate is where the slope is equal to 1 0 For most p...

Page 60: ...N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 60 Or the same data the precipitous viscosity drop can be displayed more clearly in the log log plot shown in the following ...

Page 61: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 61 ...

Page 62: ...the process 62 Below is a list of some common materials and their viscosities at their typical use temperatures Note that some materials usually considered solid such as glass actually have a very low flow rate even at high stress levels and thus an extremely high viscosity Viscosities of some Common Materials ...

Page 63: ...n of the flow This orientation alignment makes the flow process easier and results in a decrease in viscosity Given enough time after deformation the polymer chains will return to their original random configuration provided the material is stable for that period of time If deformed again the effect of shear rate thinning will then be replicated Dilatant Materials that increase in viscosity with i...

Page 64: ...d to be particularly useful at temperatures closer to the glass transition temperature of the material Suggested test temperatures for various materials are displayed in a table in the ASTM D3835 test method Generally inorganic fillers such as carbon black CaCO3 TiO2 etc increase the viscosity of polymeric materials based on their volume fraction concentration They also tend to reduce extrudate sw...

Page 65: ...lary P pressure drop across the capillary Apparent Shear Rate γ π 32Q D c 3 4R b 2S r c 3 Where γ shear rate S speed of the plunger Q volumetric flow rate Using the above expressions for shear stress and shear rate the viscosity reduces to the equation shown above Physically the viscosity is proportional to the force on the plunger divided by the speed of the plunger As can be seen in the equation...

Page 66: ...ro All of these pressure effects the barrel pressure drop the entrance pressure drop frictional effects and the exit pressure are all part of the total pressure in addition to the pressure drop in the die In the previous equations we assumed that we were only measuring the pressure drop in the die If we use this assumption we over estimate the viscosity because of the extra pressures in the system...

Page 67: ...nents 3 There are no body forces inertial effects etc 4 Viscosity is independent of pressure 5 Isothermal conditions are achieved The Weissenberg Rabinowitsch correction accounts for the fact that most polymeric materials when flowing through a capillary behave like a Newtonian fluid shear stress is directly proportional to shear rate only at very low shear rates For a Newtonian material with a co...

Page 68: ...ange viscosity drop at a fixed shear rate however very rarely exceeds 15 and occurs only in the non Newtonian range of the material The Bagley correction method is used to calculate true stress To obtain the true shear stress perform the following procedure Use a minimum of two dies though preferably three or more having the same entrance angle and same diameter D but with differing capillary leng...

Page 69: ...l still require the Bagley correction If the position of the pressure probe is a substantial distance from the capillary entrance the pressure drop from the pressure probe to the top of the die can be significant Note 2 When using very long dies there may be non linear changes in the pressure vs L D plots due to the effects of pressure or viscous heating on the viscosity In such cases one should u...

Page 70: ...C behaves more like a lightly crosslinked rubber than a true homogeneous melt As a result of this it may exhibit behavior which can be directly opposite to that of most true polymer melts It may show an increase in extrudate swell with temperature and viscosity values that are very dependent upon how temperature and shear history the pellets were formed Though PVC itself is not very moisture sensi...

Page 71: ...e side marked 1 Allow system to boot and self test Press the SYS key located on the keypad Press the CAL key located at center smart key Press SHIFT SYS simultaneously Press once using right side smart key SERIAL SELECT will appear at top of display Press SELECT smart key Press the CLR key Using number keypad at front right side of machine enter the serial 3 digit serial number of the machine and ...

Page 72: ...appear momentarily on the display unit followed by a series of zeros It is now time to enter in the value of the calibration weights Pressing the GROSS NET key will increment the current digit that is flashing Move to the left digits by pressing ZERO and move to the right digits by pressing TARE Enter the value of the calibration weights e g 100 lbs Now place the calibration weights onto the level...

Page 73: ...e into library Press SYS on keypad Press DEVICE smart key Press LC smart key Press until desired LC load cell sensor number is viewed on display Press NEW smart key Press until desired load cell sensor is viewed on delay Press ENTER smart key Press LC UNIT is displayed and should read N Press LC CAPACITY is displayed and should read LC capacity Press LC SCALING is displayed and should read 2 000 m...

Page 74: ...sensors with the sequence character to differentiate them Activate main load cell sensor Note The main load cell sensor is the load cell that is going to be calibrated and tested on the machine Press SETUP key on keypad Press four times Press EDIT smart key Press until load cell sensor of interest is displayed Press SELECT smart key Press ESC key on keypad R CAL Note Step 3 1 4 is an exercise to t...

Page 75: ...ensor with that of the typical value The ID value should be within Κ5 of the typical value Calibrate load cell sensor Press ESC twice on keypad Press SYS on keypad Press once CHAN 1 SENSOR should appear on screen Press SELECT smart key Press SINGLE smart key Press R CAL key on keypad Press ENTER smart key Press CLR key on keypad Enter typical value from Table 3 2 below Locate load cell capacity th...

Page 76: ...he calibration display Connect the calibration load cell to the bronze end of the patch cord Attach phenolic insulators to both sides of the calibration load cell Note The phenolic bobs isolate the calibration load cell from thermal damage due to the heat of the barrel The most accurate calibration will be done at the highest test temperature Press SYS key on keypad Press CAL smart key Press once ...

Page 77: ...The down arrow key alone will cause the crosshead to move at a safe slow speed Zero the calibration unit by pressing TARE on the front of the display This needs to be completed before there is force placed on the calibration load cell Continue lower the crosshead until both load cells come in contact and note the force read on the rheometer display and force read on the calibration display The val...

Page 78: ..._ will appear on display Enter 190 Press CLR keypad button Use the number pad on the right side of the keypad to enter 190 Press ENTER smart key Press ESC key on keypad twice Press SAVE smart key The system will now ramp to 190 C Insert temperature probe into barrel Note Ensure probe is completely seated in the barrel Install die and die holder nut in barrel Insert 12 7 mm 1 2 ceramic spacer Place...

Page 79: ...UBLE Press STABLE smart key Enter reading displayed on the BTP 1000A display Use the number pad on the right side of the keypad to enter the temperature Enter the numbers in order as they appear on the BTP 1000A display also pressing the decimal where necessary NOTE numbers are entered by just pressing the appropriate number key Press ENTER smart key Heat unit to 350 C Press EDIT smart key Press E...

Page 80: ... side of the keypad to enter the temperature Enter the numbers in order as they appear on the BTP 1000A display also pressing the decimal where necessary Note Numbers are entered by just pressing the appropriate number key Press ENTER smart key Record OFFSET and GAIN numbers Press SAVE smart key Temperature calibration verification Allow machine to re stabilize at 350 C for 15 minutes Record tempe...

Page 81: ...s in the need for calibration of the zero point only but it must be at the required test temperature With the addition of the pressure transducer comes an automatic check of its electronics system A precision resistor is placed into the circuit and acts like a known pressure on the system From the systems response to this simulated measurement we can assess the current calibration of the rheometer...

Page 82: ...eypad Press DEVICE smart key Press PT smart key Press until desired PT is viewed on display Press NEW smart key Press until desired PT sensor is viewed on display Press ENTER smart key Press PT UNIT is displayed and should read bar Press PT CAPACITY is displayed and should read PT capacity Press PT SCALING is displayed and should read 3 33000 mV V Press GAIN is displayed and should read 128 Press ...

Page 83: ... machine Press SETUP key on keypad Press five times Press EDIT smart key Press until PT sensor of interest is displayed Press SELECT smart key Press ESC key keypad R CAL Note Step 3 1 4 is an exercise to test that the PT is properly electrically connected Press SYS on keypad Press TEST smart key Press twice and CH2 TEST DISPLAY should appear at top of display Press SELECT smart key Press RCAL smar...

Page 84: ...nal value in the table below The ID value should be within Κ5 of the nominal value CALIBRATE PT SENSOR Press ESC twice on keypad Press SYS on keypad Press twice CHAN 2 SENSOR should appear on screen Press SELECT smart key Press SINGLE smart key Press R CAL key on keypad Press ENTER smart key Press CLR key on keypad Enter typical value from Table 3 4 below Locate PT capacity then enter the typical ...

Page 85: ...pin Bendix female connector of the 7252 56 onto the 8 pin connector of the mounted PT Always use caution Repeat step 3 2 7 3 2 10 The rheometer always performs the ZERO SHIFT and RCAL calibrations together when the R CAL button is pressed on the front panel of the rheometer To be performed correctly the rheometer should be warmed up for at least twenty minutes and locked on to the current test tem...

Page 86: ...into a die The pin should go all the way through the die without being forced Remove the pin and enter through the bottom side of the die as well If the pin will not go all the way through either end of the die it fails to meet the specifications Verify you have the correct nominal dimension and reject the die if it does not pass DO NOT USE THIS DIE CHECK BOTH ENDS OF THE DIE WITH THE PIN If the g...

Page 87: ...ke a long enough extension to the gage so the entire barrel can be checked The barrels are specified at 9 550 0 005 mm leaving the factory Clean the barrel tip with a piece of bronze wool or a like material Use a handheld micrometer to verify the room temperature diameter of 9 515 to 9 520 mm This is on the low side of the ASTM specification but still within barrel plunger tolerance specifications...

Page 88: ...on providing a window into the process 88 The drawing below may be helpful for understanding placement of the die in the barrel 12 Barrel Drawing THERMOM ETER HO LE RTD HOLE 32 GD 1 980 672 C BOREX 625 DEEP 3 4 10 BOTTOM TAP 7 000 005 32 32 TOP VIEW SIDE VIEW BOTTOM VIEW BARREL BORE ...

Page 89: ...ll take four minutes to go from start position to 8 0 inches when the plunger hits 8 0 it will stop Collect all the extrudate that has come out from the start position to the 8 0 inch position Using a balance obtain the mass of this material Let the material cool before weighing as hot material can affect the balance reading 5 The volume extruded from the rheometer is independent of speed 1 82 cc ...

Page 90: ...50oC to that at 190 C 30 2 250 10 2 190 10 2 4 1 4 1 C x C x γ γ 30 2 250 10 24 190 10 24 4 2 4 2 C x C x γ γ Additionally a low stress σ3 is sometimes used along with the higher temperature to avoid melt fracture In this case another correction is made to convert back to the σ2 level Note the 1 83 applies only to the higher stress level 4 3 10 20x σ Pa 30 2 83 1 250 10 20 190 10 24 4 2 4 2 C x C ...

Page 91: ...select the Steady State option in the test setup page of the software By setting the positions you wish the rheometer to collect data or RUN manual and press END when the force values are steady ca 1 3 The temperature used to be very stable on the rheometer now it seems to vary more than 0 2 degrees when just sitting there not loading sample or cleaning barrel The hole that the temperature measure...

Page 92: ...or Once the OVERPACK function is used the machine automatically adopts a park position of 5 0mm To return to the previous park position just press the EDIT key at the machine press the left right arrow until PARK POS is displayed and then press EDIT type in the desired park position press ENTER to accept and then press ESC Now press the up key or HOME in the RUN screen and the ram should return to...

Page 93: ...r is not performing according to previous standards we have always found the answer to be one of the items in the checklist below Force calibration OK Temperature calibration OK The program conditions are exactly the same as before The Force is zeroed correctly Are you using the same die as before Dimensions OK Is the Piston Tip Dimension OK 09 525 Tip OK 9 515 mm Is the die very clean If high tem...

Page 94: ...15 151 X300 15 0 762 11 43 120 0 27 48622441 0 232656667 CX300 1C 519 X300 1C 0 762 0 762 120 0 27 48622441 3 48985 CX300 20 152 X300 20 0 762 15 24 120 0 27 48622441 0 1744925 CX300 25 153 X300 25 0 762 19 05 120 0 27 48622441 0 139594 CX300 30 10 X300 30 0 762 22 86 120 0 27 48622441 0 116328333 CX300 33 22 X300 33 0 762 25 4 120 0 27 48622441 0 1046955 CX300 35 25 X300 35 0 762 26 67 120 0 27 4...

Page 95: ... 0 27 48622441 0 1744925 CZ300 25 203 Z300 25 0 762 19 05 180 0 27 48622441 0 139594 CZ300 30 204 Z300 30 0 762 22 86 180 0 27 48622441 0 116328333 CZ300 33 24 Z300 33 0 762 25 4 180 0 27 48622441 0 1046955 CZ300 40 206 Z300 40 0 762 30 48 180 0 27 48622441 0 08724625 CZ394 10 100 Z394 10 1 10 180 0 12 1613 0 348985 CZ394 15 518 Z394 15 1 15 180 0 12 1613 0 232656667 CZ394 1C 502 Z394 1C 1 1 180 0...

Page 96: ...95 4812273 0 114421311 CZ787 15 564 Z787 15 1 99898 29 9847 180 0 1 522490723 0 232656667 CX825 11 565 X825 11 2 0955 23 0505 120 0 1 321651662 0 317259091 CY295 16 570 Y295 16 0 7493 11 9888 90 0 28 90765109 0 218115625 Note 1 Pin gauges are designed to ASTM or ISO Specifications 0 005 mm They are similar after 98 Previous to 98 ASTM specification was larger Note 2 Full die entrance angles are gi...

Page 97: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 97 Die Design and Configuration ...

Page 98: ...ls The optional power cleaning tool is a reversible drill with a steel shaft topped with a knurled aluminum cap to hold patches This is a battery powered unit that makes barrel cleaning much easier It comes with a rechargeable battery and charging unit and lasts about a week per charge in your average laboratory works great with indexers too ...

Page 99: ...ional power cleaning tool is a reversible drill with a steel shaft topped with a knurled aluminum cap to hold patches This is a battery powered unit that makes barrel cleaning much easier It comes with a rechargeable battery and charging unit and lasts about a week per charge in your average laboratory works great with indexers too ...

Page 100: ... 2052 70DZHV 7052 70HVPT 7252 70HVPT Barrel Heater 230 V W PT 2052 70TZHV N A N A Barrel Insulators Barrel Flange Insulators Upper 8052 142MU 8052 142MU 8052 142MU Barrel Flange Insulators Lower 8052 142ML 8052 142ML 8052 142ML Lower Barrel Insulator 2052 72M 6052 72 7252 72 Upper Barrel Insulator 9052 75M 6052 75 7252 75 Heat Chamber Cover 8052 62M 8052 62M 7252 62M Barrel Plunger Parts Plunger T...

Page 101: ...it GP1410 GP1410 GP1410 Fuse 230 V Unit GP1405 GP1405 GP1405 Exterior Parts Leveling Foot GP3004 GP3004 GP3004 Keypad 7052 110 7052 110 7052 110 E stop Keypad Adder 7052 120 7052 120 7052 120 Front Base Top Plate 7052 01 7052 01 7052 01 Rear Base Top Plate 7052 04 7052 01 7052 01 Load Cells Load Cell 1 5 kN 7052 41 7052 41 N A Load Cell 5 kN 7052 42 7052 42 N A Load Cell 10 kN 7052 43 7052 43 N A ...

Page 102: ...the process 102 Part Description LCR 7000 LCR 7001 LCR 7002 Pressure Transducer 1400 Bar 8052 153MID 8052 153MID 8052 153MID Pressure Transducer 2000 Bar 8052 153MHID 8052 153MHID 8052 153MHID Pressure Transducer Port Cleaning Kit 8052 155 8052 155 8052 155 RTD s Platinum RTD Platinum 7052 13S 7052 13 7052 13 ...

Page 103: ...ough a list of programs by using the UP or DOWN SMART KEY button and then select the desired program by pressing the ACTIVE SMART KEY button 3 SYS SYSTEM Enter self calibration modes or hardware diagnostic modes for testing unit In this mode the user can choose to calibrate test or quit by selecting the appropriate CALIB TEST or QUIT SMART KEY respectively depending on which model you have prompts...

Page 104: ...ed in the EDIT PROGRAM mode EDIT SMART KEY then EDIT SMART KEY again or any text entry The clear key will also clear the PROGRAM number in the VIEW PROGRAM mode EDIT SMART KEY where a new program number can be entered 9 BACKSP BACKSPACE Destructive backspace The BACKSP key performs a destructive backspace function in text editing screens 10 NUMERICAL ALPHA INPUT Allows for numerical and alphanumer...

Page 105: ...o Use Formula C K Tk Tc 273 15 F C Tc Tf 32 1 8 Viscosity To Convert From To Multiply By Poise Pa sec 0 1 centi Poise Pa sec 0 001 centi Stokes m2 sec 1 00E 06 lbf sec ft2 Pa sec 4 79E 01 Pressure or Stress To Convert From To Multiply By Psi Pa 6 89E 03 lbf in2 Pa 6 89E 03 Atm STD Pa 1 01E 05 Atm 1 kgf cm2 Pa 9 81E 04 Bar Pa 1 00E 05 dyne cm2 Pa 0 1 ksi kip in2 Pa 6 89E 06 ...

Page 106: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 106 Example Runs 1 Polyethylene Terephthalate I V Test ...

Page 107: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 107 2 Acrylonitrile Butadiene Polystyrene ABS ...

Page 108: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 108 3 Nylon ...

Page 109: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 109 4 Glass Filled Polyurethane ...

Page 110: ...tact Louise Meyer Gage Company 230 Burnham St South Windsor CT 06074 203 528 6526 Ask for Class X pins ISO specs are 0 0002 of nominal ASTM specs D3835 are 0 0003 of nominal Cleaning Skyline Center Inc POB 3064 Clinton IA 52732 319 243 4065 800 747 4065 Extension 4065 FAX 319 243 9901 Bore Gages nspex Corp 664 Bussee Hwy Park Ridge IL 60068 708 825 2200 Fax 825 0825 Order Diameter Probe 029 Probe ...

Page 111: ...of 1992 cost about 255 for 50 grams SRM Catalog number is NIST Special Publication 260 To order 301 975 6776 Fax 301 948 3730 Hg Spill Kit Mercury Clean Up Spill Kits Mercon Products distributed by Fisher Scientific Unit 8 7551 Vantage Way Delta B C Canada V4G 1C9 Tech Assistance 800 926 8999 604 940 0975 or call Fisher Scientific Thermometers PRINCO Instruments Inc Accepts Hg for Recycle 1020 Ind...

Page 112: ...LCR7000 RHEOSIGHTS P N 974194 Rev A ECO 52468 www dynisco com From lab to production providing a window into the process 112 RAM Rate Shear Rate Table ...

Page 113: ...astics Processing Dealy Wissburn Van Nostrand Reinhold 1990 Modern Plastic Encyclopedia Get Latest Issue McGraw Hill POB 423 Highstown NJ 08520 Has data bank on material lots of good intro articles Polymer Melt Rheology A guide for industrial practice F N Cogswell George Godwin Limited in association with The Plastics Rubber Institute Wiley Sons New York Toronto C 1981 Polymer Engineering Principl...

Page 114: ...ymer Chemistry The Basic Concepts P C Hiemenz Marcel Dekker 1984 Theoretical Computer Programs for Rheologists G Gordon M Shaw SPE Hanser 1994 Properties of Polymers D W Van Krevlen Elsevier New York 1990 Third Ed Viscoelastic Properties of Polymers J D Ferry Wiley Sons 1980 Rheology of Polymeric Systems P J Carreau D De Kee R P Chhabra Hanser 1997 ...

Page 115: ...a 10kN L C or P T and only 5kN is needed to test then the L C SCALING should be set at 50 L C GAIN Rate of voltage to force scale Example 2 5 volts 200n V F RTD Resistive Thermal Detector A device used to measure temperature Sample Length This is the distance over which the speed of the plunger is measured during load control tests Set it to 0 0 if you wish to do runs that control plunger speed It...

Page 116: ...on The terminal force also controls the maximum force allowed during the purging of material from the barrel The speed of purging will be automatically adjusted so that the maximum amount of force applied is half the terminal force if you are having trouble purging the rheometer Normally this value is set just below your load cell capacity e g 1000 LB cell set to 990 LB Test Delay The Test Delay i...

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