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ARES User Manual

1. gt 13 7 gmcm Ay 277 19 Figure 2 6 ARES Front Panel LCD Display ARES User Manual Actuator Bearing Locks Standard Transducers 2K STD and 10K STD The standard transducers do not require a bearing lock FRT without Normal Force 100 FRT and 200 FRT The 100 and 200 FRTs use a bearing lock consisting of an aluminum block Figure 2 7 that is fastened to the transducer by two machine screws The block is machined at an angle that allows the bearing to be locked and unlocked by sliding the block LOCKED POSITION SCREWS 2 UNLOCKED POSITION Figure 2 7 Bearing Lock 100 FRT and 200 FRT Procedure for Locking and Unlocking Air Bearings 100 FRT and 200 FRT Refer to Figure 2 7 while performing the following procedures To Lock the FRT air bearing 1 Read the Caution on page 11 2 Ensure that instrument power is off and air is applied to the FRT 3 Loosen both screws and slide the block to the locked position 4 Tighten both screws To Unlock the FRT bearing 1 Read the Caution on page 11 2 Ensure that instrument power is off and air is applied to the FRT 3 Loosen both screws and slide the block to the unlocked position 4 Tighten both screws ARES User Manual FRT with Normal Force FRTN The FRIN transducers utilize a bearing lock consisting of a steel pin with a clamp on both ends Figure 2 8 that is inserted through the transducer housing On most 2K FRTN1 transducers the pin is installed suc
2. 3 4 Ensure that Orchestrator online indicators do not indicate a problem if so go to 7 Ensure that the commanded temperature is correct and reasonable if not command a suitable temperature Ensure that the SET USER TEMPERATURE LIMIT is set to a reasonable value if not set accordingly Ensure that the temperature reported by Orchestrator is close to actual temperature If the temperature is 650 C the one or both of the PRTs are open Visually inspect PRTs for damage If damaged go to 7 An oven fuse may be open Call Technical Service Ensure that the temperature reported by Orchestrator is close to actual temperature if not change temperature control to Mode 3 If reported temperature is now correct then Tool PRT or upper oven PRT control loop is malfunctioning If reported temperature is incorrect then lower oven PRT control loop is malfunctioning Visually inspect PRTs for damage If damaged go to 4 An oven fuse may be open Call Technical Service Ensure that LN supply pressure is adequate i e 20 30 psi if not check supply lines Ensure that LN filter is not clogged if so go to 5 Ensure that when the LN2 Controller is on vent gas exits from the muffler on the LN2 Controller if not go to 5 Ensure that there is no leaking around dewar Call Technical Service ARES User Manual Table 6 2 Instrument Operation Troubleshooting Guide Continued PROBLEM CORRECTIVE AC
3. Figure 5 11 Setup Instrument Temperature Options Showing the Adjustable Temperature Calibration Table ARES User Manual 225 ARES User Manual Chapter 6 Maintenance General Information This chapter contains the following information e Routine Maintenance Routine maintenance consists of tasks that we recommend you perform on a periodic basis e Special Maintenance Special maintenance tasks can be performed only by qualified electronic technicians e Troubleshooting Guide A troubleshooting guide is supplied to assist you in diagnosing selected problems Routine Maintenance Cable and Hose Inspection Damage to the AC power cords can cause a safety hazard Periodically inspect these items as follows AC Power Cords Remove AC power to the instrument as follows 1 Push the Main Power Switch to the OFF O position 2 Remove the POWER IN plug from the AC main source 3 Inspect all the cords for frayed insulation or exposed bare copper wire especially in the immediate vicinity of the plugs on either end If any damage is found notify TA Instruments Technical Service Apply AC power to the instrument as follows 1 Install the POWER IN plug in the AC main line voltage source 2 Push the Main Power Switch to the ON I position Air Hoses Remove AC power to the instrument as follows Push the Main Power Switch to the OFF O position Remove the POWER IN plug from the AC main line voltage source Lo
4. lg Rig 13 97mm rn INNER CUP DIAMETER 27 94 mm PEL 0 Marry 14 75 mm i INNER BOB DIAMETER 29 50 R 16 00 mm OUTER BOB DIAMETER 32 00 mm R 17 00 mm OUTER CUP DIAMETER 34 00 mm Figure 4 16 Double Wall Couette Original fluid bath set up showing inner and outer cup as well as tool dimensions ARES User Manual Tool Installation Fluid Bath 2 The Double Wall Couette lower tool cup mounts into the Fluid Bath 2 see Chapter 2 to ensure precise thermal control Install the bath on the test station prior to mounting the tool in the bath a CAUTION Never place any lower tool into the bath if the temperature of the lower tool is cooler than that of the bath Placing a tool into a warmer bath will result in expansion of the tool during use After expansion the tool may not be removable without damaging your bath We suggest that you partially insert the tool by placing the tool loosely into the bath Allow the lower tool temperature to match that of the bath then fully thread the lower tool into the bath 1 Select the Set GaplInstrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise the stage to the loading position 2 Verify that the motor is on then mount PRT and lower tool Cup into the Fluid Bath 2 and the upper tool Bob on the transducer shaft 3 Using the Set Gap Instrument Control function in Orchestrator zero the n
5. Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using a specific geometry For each geometry there are specific factors that will affect the operating range for that geometry Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type use the following equation x K A where A Stress Constant for the specific geometry K Strain Constant for the specific geometry and C is computed from the following C for G MAXIMUM C for G MINIMUM 2K FRTN1 2K FRTN1E 7 J 1 15e 06 rad gecm Za see note below Transducer 1K FRTN1 J 4 9 e 06 see note below J 2K STD 10K STD F J 2 60e 06 see note below 100 FRT for 100 J 2 60e 05 200 FRT a ee 100 FRTN1 for 10 J 2 60e 06 200 FRTN1 a see note below NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination ARES User Manual 151 To determine the maximum or minimum complex viscosity 1 that can be measured at a given frequency use the following formula G
6. Raise the stage to provide sufficient room for sample loading Sample Loading Original Fluid Bath The nominal sample volume is 8 ml In general pour the sample into the cup then lower the bob until the gap again reads zero and the sample appears as shown in Figure 4 15C If the gap is set as described in the previous section this will ensure that the nominal bob length is 31 90 mm Note that the upper surface of the bob must be as flush as possible to the upper surface of the cup Tool Maintenance To facilitate cleaning of the lower tool the inner cup can be removed from the outer cup when necessary Inspect the o ring for cuts or other damage and replace it if necessary ARES User Manual STRAIGHT EDGE 1 BRING UPPER SURFACE OF BOB FLUSH WITH UPPER SURFACE OF CUP BY RAISING BOB UP TO STRAIGHT EDGE B UPPER SURFACE OF BOB UPPER SURFACE OF CUP FILL SAMPLE TO HERE UPPER SURFACE OF BOB MUST BE FLUSH WITH a UPPER SURFACE OF CUP BOB T EFFECTIVE BOB LENGTH 31 90 mm WITH SAMPLE LOADED AS SHOWN SAMPLE SAMPLE VOLUME 8 ml cur MAN Ua CUP INNER WALL C Figure 4 15 Double Wall Couette for the Original Fluid Bath Set Up and Use A and B Setting the Gap C With Sample Loaded ARES User Manual THESE TWO SURFACES MUST BE ALIGNED TO OBTAIN EFFECTIVE BOB LENGTH SHOWN MOUNTING SCREW a INNER CUP L 31 90 mm EFFECTIVE BOB LENGTH BOB he OUTER OO CUP
7. THIS DISTANCE IS THE SAMPLE LENGTH SAMPLE LOWER FIXTURE SLIDING CLAMP SAMPLE NOTE Center sample in fixture using Centering Lines as guides Figure 4 11 Torsion Rectangular with Sample Loaded ARES User Manual Torsion Rectangular Original Design Strain Constant Stress Constant 2 T 1 0 378 T 3 18 W K 1000 WT Variables Gc Gravitational constant 980 7 cgs or 98 07 SI T Thickness of sample mm W Width of sample mm L Length of sample mm Options Insets to accommodate thicknesses from 0 76 mm to 6 35 mm Environmental Systems Torsion Rectangular Tool Ambient original design Oven General Information The Torsion Rectangular tool is used for testing solid materials with high modulus including thermosets thermoplastics and elastomers The sample is held in tension between the upper and lower tool Several inserts are provided to accommodate samples of varying thicknesses Sample Dimensions To prepare samples that fit within the physical constraints of the tool use the following guidelines e Maximum Sample Width 12 7 millimeters e Typical Sample Length 45 millimeters e Sample Thickness depends on the size of the insert used INSERT DESIGNATION MAXIMUM SAMPLE THICKNESS MM 184 ARES User Manual Always use the correct size insert for the sample thickness If the sample does not fit tightly in the insert erroneous data may result Shims can
8. 10 A 60 Hz Europe 220 VAC 10 A 50 Hz Japan 100 VAC 10 A 50 Hz 60 Hz with boost transformer Standard Mechanical Chiller 220 VAC 10 A 60 Hz AC PO Option 200 VAC 10 A 50 Hz ARES User Manual Table 1 5 Operating Specifications Environmental Controller Operating Parameter Forced Convection Fluids Bath Oven Temperature Range Standard Ambient to 600 C 10 C to 150 C 30 C to 150 C Optional 150 C to 600 C S a Depends on 30 C min at 20 C empero ramprals OE N Circulator used circulator fluid temp Temperature Stability 05 C 0 01 C 0 1 C at thermal equilibrium o aa a Motor Performance Specifications Table 1 6 Specifications High Resolution Motor HR PARAMETER DYNAMIC MODE STEADY MODE Angular Displacement Range 0 005 to 500 milliradians Not Applicable Frequency Range 1E 5 to 500 rad sec Not Applicable Rotational Rate Range Not Applicable 0 001 to 100 rad sec Table 1 7 Specifications High Torque Motor HT Angular Displacement Range 0 005 to 500 milliradians Not Applicable Frequency Range 1E 5 to 100 rad sec Not Applicable Rotational Rate Range Not Applicable 0 001 to 100 rad sec Table 1 8 Specifications Low Shear Motor LS Angular Displacement Range 0 005 to 500 milliradians Not Applicable Frequency Range 1E 5 to 100 rad sec Not Applicable Rotational Rate Range Not Applicable 1 X 10 to 200 rad sec ARES User Manual Transducer Operating Specific
9. 94 96 150 Strain Controlled Steady Test Methods 116 Strain Controlled Transient Test Methods 121 Stress 93 94 96 Stress Ramp Test 139 Stress Relaxation 100 123 Suspensions 149 y TA Instruments Offices 237 Tan 6 95 Technical Support 14 Temperature Calibration 224 Tensile Strain 93 Tensile Stress 93 Test Tools general guidelines 154 160 upper tool installation 154 Test Modes 100 Test Station 35 Thermal Expansion 160 Thermopastics 149 Thermosets 149 Thermosetting Resins 150 Thin Films 149 Thixotropic Loop 130 Torque Normal Relaxation 132 ARES User Manual Torsion Rectangular New Design test tool constants 177 tool installation 180 general information 177 operating range 178 sample loading 181 Torsion Rectangular Original Design test tool constants 184 tool installation 187 general information 184 operating range 185 sample loading 187 trademarks 5 Transducer description 37 principles of operation 26 Transient Step Strain 123 Troubleshooting Guide 232 V Vane Tool See Couette Viscoelastic 93 Viscosity 93 Viscous Modulus E 94 Viscous Stress t 94 ARES User Manual Appendix A Complex Modulus Limits This appendix provides complex modulus limits for various tools Appendix Table A1 1 Complex Modulus Limits for Parallel Plate 2K FRTN1 and 2K FRTN1E Transducers PLATE DIAMETER mm G Maximum dynes cm G Mi
10. C ARES User Manual Circulator Options The Peltier must be connected to a circulating fluid source Any manually controllable circulator with heating cooling capabilities can be used to operate the Peltier system over its entire specified temperature range This can also be the same circulator used with the Fluid Bath The standard fittings installed onto the ARES Peltier Assembly fluid hoses accommodate computer controlled circulators that are sold by TA Instruments The Peltier Circulator manufactured by TA Instruments is an effective yet inexpensive means of providing non temperature controlled circulating fluid Instructions for use of the Peltier Circulator are printed on the label that is affixed to the circulator If using the Peltier Circulator you must remove the standard fluid fittings from the ARES Peltier Assembly fluid hoses then install the special pair of fittings that are supplied for use with the Peltier Circulator selecting a Thermal Operating Range The temperature of the circulating fluid determines the Thermal Operating Range of the Peltier system To select a thermal operating range fluid temperature must be set in accordance with the following guideline Assuming that the ambient temperature in the vicinity of the heat sink is 20 C a low end differential ATL of approximately 40 C exists between the fluid temperature and the lower limit of the thermal operating range A high end differential ATy of approxi
11. Please refer to the preceding documents as well as this manual prior to and during test setup and execution ARES User Manual 99 Test Modes The ARES is capable of performing dynamic steady and transient time based mechanical tests These are organized in Orchestrator under the following categories e Strain Controlled Dynamic Dynamic oscillatory mechanical measurements where strain is controlled and stress is measured e Strain Controlled Steady Steady mechanical measurements where strain is controlled and stress is measured After the sample is allowed to reach steady state measurements are averaged over a period of time e Strain Controlled Transient Static time based tests where strain is controlled and stress is measured Data are collected rapidly to look at the sample response over time to an applied deformation e Stress Controlled Transient Similar to Strain Controlled Transient tests but where stress is controlled and strain is measured Specific categories and tests are selected from within the Edit Start Test function of Orchestrator The available tests used with the ARES are Strain Controlled Dynamic e Dynamic Single Point Measurement e Frequency Sweep e Dynamic Temperature Step e Frequency Temperature Sweep e Dynamic Strain Sweep e Dynamic Time Sweep e Dynamic Temperature Ramp e Mulitwave Single Point e Multiwave Temperature Ramp Strain Controlled Steady e
12. S PARALLEL PLATE PRT PN 700 03469 BATH 2 COUETTE lower fixture BATH 2 DOUBLE WALL COUETTE lower fixture Figure 2 24 Fluid Bath 2 Lower Tool and PRT options Lower Tool Installation and Removal The lower tool is mounted into the bath well The well is threaded to mate with the threads on the tool The tool should be tightened clockwise by hand only Before installing the lower tool ensure that the correct PRT is installed and operational To remove the tool use the supplied wrenches If necessary to loosen the tool from the bath well The wrench used on the tool is labeled FOR TOOL and the wrench used to hold the bath is labeled FOR COVER Keeping the lower tool and bath well threads clean and free of damage will help ensure easy installation and removal Filling the Circulator Depending on the type of circulator in use and the desired operating range of the circulator fill the circulator with fluid as specified in Table 2 6 The Julabo FS 18 circulator requires about 2 liters of fluid and should be filled to within 5 mm from the top However refer to your actual Bath documentation for specific circulator filling and operating guidelines as well as other bath fluid options for your application Also refer to the bath fluid MSD for guidelines regarding the safe handling of your particular bath fluid ARES User Manual Because of the construction of the Fluid Bath 2 the seals are very delicate It is imp
13. and transducer mount the pulley wheel or hub appropriately Install the calibration tool and pulley as shown in Figure 5 2 a For 10K STD Transducers Two pulleys are supplied Referring to Figure 5 2 insert a pulley into each side of the Test Station frame ensuring that the flat machined into each pulley shaft faces the access hole Please note that Figure 5 2 shows the pulley on the right side only b For all other transducers Insert the pulley into the Test Station frame as shown in Figure 5 2 ensuring that the flat machined into the pulley shaft faces the access hole Secure the pulley s by tightening the setscrew in the access hole Figure 5 2 using a 1 5 mm hex wrench Ensure that the calibration tool and pulley are installed as shown in Figure 5 3 If you have a 10K STD transducer an additional pulley should be installed on the left Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset Torque to Zero buttons Exit the form when finished Prepare the calibration line specified in Table 5 2 depending on the transducer in use Prepare the calibration line s by making a loop at each end ARES User Manual INSTRUMENT ACCESS HOLE TRANSDUCER COVER HUB PULLEY ONE EITHER SIDE CALIBRATION FIXTURE Figure 5 2 Installation of the Calibration Tool and Single Pulley Figure 5 3 Calibration Tool
14. n 4 2 where n Complex viscosity Poise G Complex Modulus dynes cm Frequency rad sec Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 2 Substitute the G MAXIMUM value into equation 4 2 then determine the upper limit of operation by calculating 1 at each O 0 values chosen to be from the lowest to highest frequencies within the transducer operating range 3 Substitute the G MINIMUM value into equation 4 2 then determine the lower limit of operation by calculating N at each 4 Generate an X Y scatter plot of complex viscosity N Y axis versus frequency X axis The region between the upper and lower limits of operation is the range of complex viscosity that can be tested Please note that the values for J above are nominal values and will vary slightly between transducers Accordingly and per good standard practice care should be taken to ensure the data are valid when testing near the upper or lower limits for a given system Possible Sources and Causes for Error This section contains information describing errors that can occur as a result of tool and sample limitations Discrepancies in Sample Geometry The force generated by a sample for a given amount of strain is a function o
15. use the following formula nea 4 2 a 162 ARES User Manual where n Complex viscosity Poise G Complex Modulus dynes cm Frequency rad sec Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 2 4 Calculate G MAXIMUM and G MINIMUM using equation 4 1 Substitute the G MAXIMUM value into equation 4 2 then determine the upper limit of operation by calculating N at each O values chosen to be from the lowest to highest frequencies within the transducer operating range Substitute the G MINIMUM value into equation 4 2 then determine the lower limit of operation by calculating 1 at each Generate an X Y scatter plot of complex viscosity 1 Y axis versus frequency X axis The region between the upper and lower limits of operation is the range of complex viscosity that can be tested Appendix 1 contains tables of G values for some tool combinations transducers and a standard motor Tool Installation Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise the stage to the loading position Verify that the motor is on then mount the upper and lower tools on the actuator shafts Using the Set Gap Instrument Control function in Orchestrator zero the normal force and to
16. 0 C Paints Per one 200 Max 350 Min 20 Zone Number 1 2 4 4 SOWIE TIE ee ceeeeeeeseeeees s or hems 200 i 00 50 200 Extension Value See Mode for Units 0 05 0 007 50 0 50 0 Extension Mode ooo Rate mms Hencky Vis Force am End Test y Options Delay OF Analog Of Ratebiar Ut Options End of Test Save s Help Cancel Figure 3 16 Multiple Extension Mode Test Set up Screen Ok Test Options Multiple Extension Mode Test options are as follows e Delay Before Test e Analog Data Input e Motor Control Gain Manual or Default only for the Constant Force Mode o Proportional Factor gain settings manual or default of 1 0 o Integral Factor gain settings manual or default of 0 1 The motor control gain can be adjusted to change the response of the control loop controlling stress level in constant stress mode ARES User Manual 125 Table 3 4 Summary of Multiple Extension Mode Test Options Extension Description Mode Rate mm s Apply a constant rate of linear Can be used to determine the range of displacement Extension rate in the linear behavior in a material by plotting sample is not constant due to change Force as a function of displacement in sample length Hencky 1 s Apply a constant rate of sample strain Used to measure the extensional modulus Linear displacement rate is adjusted to and properties in samples maintain a constant sample strain rate Rim
17. 02 High range 4 10E 03 Low range 100 FRT Appendix Table A1 10 Complex Modulus Limits for Double Wall Couette Geometry Cup OD 34 mm Cup ID 27 95 mm Bob OD 32 mm Bob ID 29 5 mm G MINIMUM dynes cm TRANSDUCER TYPE G Maximum dynes cm at Frequency rad sec 5 39E 02 5 39E 03 0 100 FRTN1 2 8E 05 9 35E 02 Q 9 3DE 03 1 11E 02 High range 1 11E 03 Low range 5 57E 03 High range 5 57E 04 Low range 100 FRT ARES User Manual 2 8E 05 ARES User Manual
18. 115 G Gap automatic zero 158 enabling the gap control panel 158 manual zero 157 max force allowed option 159 read text tool gap 159 set gap instrument control function 38 setting general 157 Gas input options 53 pressure specifications 53 ARES User Manual H Hastelloy Tool tool installation 171 general information 165 liquid seal 168 operating ranges 165 parallel plate tool 165 use with oven 169 Hencky Strain Rate 125 high voltage warning 207 Hookean Region 93 Hooke s Law 93 Host Computer 35 Humidity Cover 83 84 Instrument Control Panel 36 65 L LCD Display 40 LEDs diagnostic 230 License Agreement 3 Linear Region 93 Linear Strain Sweep 107 LN Controller description 61 location 33 physical specifications 28 Logarithmic Strain Sweep 107 Loss Modulus See Viscous Modulus ARES User Manual Main Power Switch 51 Maintenance cleaning 228 routine 227 special 230 Manual Delay 141 Modulus 93 Motor air pressure requirements 53 description 35 location 34 principles of operation 26 rapid shut off 36 specifications 30 turning on and off 36 Multiple Extension Mode 125 MultiWave Single Point 112 MultiWave Temperature Ramp 112 N Newton s Law 93 O One Cycle Correlation 146 Oven description 58 gas selection 62 location 34 operating requirements 63 operation 65 rapid shutdown 36 signal connection to test s
19. 500 0 Min 1 00e 05 Initial Temp 25 0 PC Max 600 0 C Min 150 0 Strain Limite Mas 312 5000 Min 0 0031 25 one Number 1 E Final Temp occ Peon 00 Ramp Rate PCminlao po Computed Ramp Time hi rr 58 20 Soak Time After Ramp s or hom foo Time Per Measure s or Fires od MM O 2 fi 0 0 PT il Uptions FreShear O Delay Of AutoTens OF Analogi Ot Autost O MeasOps 01 Options End of Test Save As Help Cancel Figure 3 7 Dynamic Temperature Ramp Test Set Up Screen Suggested Uses Suggested uses for temperature ramp tests e To quickly analyze the behavior of samples as a function of temperature and to determine test parameters for subsequent Temperature Step tests e To simulate processing conditions that a material may experience in use by programming the relevant time temperature profile e To study the response of a material to changing strain levels as a function of time and or temperature e The Temperature Ramp test is one of the most flexible of all of the test modes due to its ability to handle complex time temperature strain profiles ARES User Manual Test Options The following test options can be selected for use with the temperature ramp e Steady PreShear e Delay Before Test e AutoTension e Analog Data Input e AutoStrain e Measurement Options o Delay Settings o Strain Amplitude Control ARES User Manual MultiWave Single Point MultiWave Te
20. AC power to the instrument as follows a Push the Main Power Switch to the OFF O position b Remove the POWER IN plug from the AC main line voltage source 2 Apply some cleaning solution onto a cotton cloth then wring out the cloth to discharge excess water the cloth must be damp but not wet 3 While ensuring that excess fluid from the cloth does not enter any crevice of the instrument use the cloth to gently clean the desired external surfaces 4 Ensure that all surfaces of the instrument are dry 5 Apply AC power to the instrument as follows a Install the POWER IN plug in the AC main line voltage source b Push the Main Power Switch to the ON I position ARES User Manual Lifting and Carrying the Instrument Test Station The Test Station weighs 275 pounds 125 kilograms It can be safely lifted and carried only by a fork lift that is rated to carry such weight However since there is no surface that offers adequate contact points for a fork lift the Test Station is designed to be lifted only when it is mounted onto a pallet this is the shipping configuration by placing the forks in the pallet The handles on the side of the test station can be used to slide the test station on the workbench surface You may need to apply some lift while sliding the instrument but do not attempt to completely lift and carry the Test Station by the handles as balancing the instrument is difficult Be careful not to damage the feet on the
21. ARES User Manual Torque Calibration for All Transducers Torque Calibration ensures that the transducer is accurately measuring torque The calibration involves hanging a precision weight on the calibration tool a 2 5 centimeter moment arm that is mounted on the transducer during calibration The applied torque is therefore the product of the weight and the 2 5 centimeter moment For example hanging a 500 gram weight applies a torque of 500 g 2 5 cm 1250 gecm NOTE For this and all subsequent calibration procedures the instructions assume that the Host Computer is connected to the ARES test station and that Orchestrator is running Procedure 1 If calibrating an FRT ensure that the transducer is set to High Range before proceeding To set the transducer to High Range do the following a Access the Set Transducer Characteristics form Figure 5 7 by selecting the Transducer option from the Service function of the Utilities pull down menu b Using the Transducer Selected menu select the high range transducer then Click Ok Remove any test tools Turn on the motor Raise the stage to bring the bottom of the stainless steel transducer cover about 2 inches below the instrument cover Figure 5 2 Determine which calibration tool you have based upon Figure 5 1 Depending upon your tool
22. Calibration form is within the limits for the CALIBRATED FULL SCALE VALUE shown in Table 5 4 Table 5 4 Normal Force Calibration Weights Applied Normal Forces and Calibrated Full Scale Values APPLIED NORMAL CALIBRATED FULL TRANSDUCER WEIGHT NORMAL FORCE SCALE VALUE FORCE VALUE a ay E 1000 grams ont 1000 2 gmf 2100 gmf 5 p n 613 01222 gm 998 to 1002 1995 to 2205 1K FRTN1 100 FRTN1 100 grams 100 gmf 100 0 1 gmf 105 gmf 5 200 ERTN1 p n 613 02060 99 9 to 100 1 99 75 to 110 25 2K STD 1000 grams 00H 1000 5 gmf 1575 gmf 5 10K STD p n 613 01222 gm 995 to 1005 1496 25 to 1653 75 ARES User Manual 13 Select the ACCEPT button Control returns to the Transducer Characteristics form 14 Verify that the Normal Calibration Value now displayed in the form the high range value if the transducer is an FRT is the same as the Current Normal Cal value just displayed in the Transducer Calibration form Press Ok 15 If the transducer in use is an FRT remain in the Transducer Setup form and perform the following step If the transducer is a STD transducer go to step 16 a Access the Set Transducer Characteristics form Figure 5 7 by selecting the Transducer option from the Service function of the Utilities pull down menu b Copy the high range transducer Normal Calibration Value into the column containing the transducer settings for the low range transducer 16 Click Ok This concludes the Norm
23. Controller is currently ready for use In this case the LN level in the Dewar flask is between 50 and 75 of the flask capacity LN2 Off The LN2 Controller is currently disabled 66 ARES User Manual Fluid Bath 2 Description The Fluid Bath 2 offers precise control of sample temperature using a closed fluid re circulant system The operational range of the Fluid Bath 2 is 10 C to 140 C Thermally controlled fluid supplied by a circulator flows through the bath The lower test tool is mounted within the Bath Well and attains thermal equilibrium with the surrounding bath The temperature of the lower tool is measured by the bath PRT which mounts through the Bath Well into the Motor You can choose to control the temperature of either the lower tool or the circulator fluid itself The Circulator regulates the temperature of the bath fluid and pumps the fluid through the Fluid Bath The circulator as supplied by TA Instruments is connected to and is under the control of the test station and software The fluid circulated through the bath is maintained at the temperature selected in Orchestrator The circulator also has its own fluid temperature regulation which can be used as the temperature control loop for the Bath by selecting manual temperature control Orchestrator Presently the standard circulator supplied by TA Instruments is the Julabo FS 18 Installation of Fluid Bath The fluid bath is mounted onto the motor using a
24. Linear Points Per Zone 300 Max 350 Min 20 Shear Rate Limits 1s Max 200 0000 Min 0 007 000 one Mumber 1 2 4 4 Shear Rate Meza foo foo foo Zone Time sor LS o oc o Direction i f Clockwise C Counterclockwise Options Delay OFf Options End of Test Save As Help Cancel Figure 3 14 Step Shear Rate Test Set Up Form ARES User Manual 121 Suggested Uses Step Shear Rate can be used to examine the following sample characteristics e Stress growth and relaxation at constant temperature e Time required to reach steady state flow behavior e Relaxation after steady shear see Shear Rate in the description of Parameters Test Options The following test options are available when using Step Rate with the specified instrument types e Delay Before Test ARES User Manual Stress Relaxation Transient Step Strain Functional Description Stress Relaxation transient step strain monitors sample stress relaxation by taking measurements following a single upward or downward step of the motor to the selected strain Four independent measurement zones with a maximum of 350 data points per zone are available The force response relaxation profile or G t to the step strain is measured in either logarithmic or linear sampling mode Log Logarithmic Logarithmic sampling takes data at logarithmically incremented intervals As an example selecting 5 points per zone during a 100 second zone di
25. Mode Outputs a DC voltage that is proportional to motor strain actual motor angular deflection o Ee Scaling is 9 VDC 0 radians 5 VDC 0 5 radians Steady Mode Outputs a DC voltage that is proportional to transducer normal axial force Scaling is 0 VDC 0 gmf 5 VDC full scale normal force As the instrument is shipped STRAIN NORMAL IN is connected to and outputs STRAIN NORMAL the same signal as STRAIN NORMAL OUT This connector is normally used by IN TA service personel for diagnostic purposes Outputs a DC voltage that is proportional to the selected strain which drives the COMMAND OUT motor in dynamic mode Scaling is VDC 0 radians 10 VDC 0 5 radians As the instrument is shipped COMMAND IN is connected to and outputs the COMMAND IN same signal as COMMAND OUT This connector is normally used by TA service personel for diagnostic purposes Outputs a DC voltage that is proportional to transducer normal axial force Scaling is VDC 0 gmf 5 VDC full scale normal force NORMAL OUT ANALOG 1 IN Accepts a 10 VDC input signal that can be sampled at 1 Hz and stored in the data file This is the input for the Analog Data input feature in Orchestrator LN2 Communications interface between the optional LN2 controler and the instrument Connected to LN2 controller Communications interface between the Host Computer and the instrument Unless you have selected a different port using Orche
26. OF CUP f z COM as mm NO LOWER THAN 5 mm BELOW BOB UPPER SURFACE OF CUP SAMPLE CUP l Figure 4 13 Couette with Sample Loaded Vane Tool The Vane Tool is designed to replace the bob under certain circumstances Itis primarily used with materials that are highly structured such as foams and lotions which may tend to slip with a normal bob This slippage could mistakenly be interpreted as a yield stress using a normal bob For these fluids when using the vane tool the material within the vanes moves as a solid plug However for less shear thinning fluids there will be secondary flows between the vanes which will result in incorrect viscosity shear rate data so it is important to use the correct tool for the material The vane tool is also useful when testing chunky fluids or that contain larger particles Many food items would fall into this category The vane tool is used to do Creep Recovery to measure Yield Stress or low speed Steady shear testing The Vane Tool should only be used for low speed steady testing The vane tool is handled similarly to the standard bob The Couette Geometry should still be selected in Orchestrator The tool dimensions are determined as shown in Figure 4 10 The vane tool is designed for use with the 34 mm cup The vane tool should be lowered carefully into the sample to minimize disturbing the sample ARES User Manual 193 194 Figure 4 14 Vane Tool ARES Us
27. Options Form Used to Input the Fluid Bath System Configuration NOTES 1 Make sure the following are selected e Instrument Setup TEMPERATURE CONTROL e Temperature Control BATH INSTRUMENT CONTROLLED ONLY ARES User Manual NOTES continued 2 Ensure that the maximum and minimum temperatures corresponding to the desired circulator operating range and fluid See the previous topic Filling the Circulator are entered in the Max and Min Temperature fields 3 Select either Temperature Loop Control option using the following information as a guideline e Circulator Temperature When selected the temperature of the fluid in the circulator is maintained at the commanded temperature The lower tool PRT is independent of the circulator temperature and due to its location will report temperatures that are slightly different than the commanded circulator temperature The circulator temperature control should be used when running step or ramp type temperature studies where a controlled steady temperature change or speed is more critical than actual sample temperature e Tool Temperature When selected the temperature of the lower test tool is maintained at the commanded temperature Tool Temperature control is the recommended setting for isothermal and some step testing where controlling the actual sample temperature is most important When the commanded temperature has been achieved wait 20 to 30 minutes at the commanded te
28. STRAIN 100 TEMPERATURE Current ambient temperature Ensure that the phase angle 6 is between 87 and 92 throughout the frequency range If the values obtained from this test are outside this range please contact Technical Services for further assistance This concludes the phase angle check ARES User Manual 219 Strain Calibration Check Strain Calibration Check allows you to determine if actual strain the angular deflection of the motor corresponds to a commanded strain In general this procedure involves selecting the parallel plate geometry then modifying the tool dimensions to achieve a strain constant of 1 This action results in commanded strain being identical to actual motor deflection 1 e if you command 25 strain the motor should deflect 0 25 radians from dynamic zero position While running a Dynamic Time Sweep a calibration pointer attached to the motor allows you to visually examine motor position in relation to calibration marks etched onto the motor cover The calibration marks are graduated in increments of 0 1 0 25 and 0 5 radians from either side of dynamic zero position Additionally you can check the STRAIN reported by the Orchestrator online parameter display which should indicate 25 Procedure 1 Remove any test tools 2 Turn on the motor and ensure that it is in dynamic mode 3 Install the pointer onto the motor as shown in Figure 5 8 4 Use the Strain Offset to align the pointer with
29. Shear 1 s Apply a constant shear rate to the Measure the squeeze flow properties of a sample in squeeze flow material Rate corresponds to the shear rate at the edge of the sample Force gmf Apply and maintain a constant force on This can be used to provide information on the sample the creep behavior of a material End Test Used to indicate that a zone is not used and that the test should end ARES User Manual Arbitrary Waveshape Test Functional Description The Arbitrary Waveshape test allows you to define the strain history used to deform the sample by supplying one or more equations for strain as a function of time Up to four different equations each with a specified time period can be used There are also 4 Zones used for data collection with each Zone capable of sampling over a time interval that is independent of the time specified for the waveform You should first define the time intervals for each of the data collection Zones Figure 3 17 and the number of points samples to collect in each Zone The second part of the form is used to enter equations for the strain as a function of time as well as a playback time Wave Time which determines the period of time over which the equation is to be played back Note that the strain is always given in strain units not percent strain and the limits based on the current geometry are given below the equation fields The waveform cannot be built if the strain v
30. User Manual Lower Tool Installation To install a lower tool into the fluid bath place the tool into the bath Figure 2 36 and apply downward pressure until the tool is seated flush against the bath of the lower tool is cooler than that of the bath Placing a tool into a warmer bath will result in expansion of the tool during use After expansion the tool may not be removable without damaging your bath O CAUTION Never place any lower tool into the bath if the temperature We suggest that you partially insert the tool by placing a phenolic spacer between the upper lip of the lower tool and the surface of the bath Allow the lower tool temperature to match that of the bath then remove the spacer and fully insert the lower tool rem Lower Fixture l a Bath Well Pi ls Fi NOTE install the bath PRT prior to installing the fixture p Fluids Bath Figure 2 36 Installation of Lower tool into Fluids Bath ARES User Manual Circulator Connections Figure 2 37 shows fluid connections between the bath and Test Station The circulator should be positioned on the floor below the work area Make sure all hoses are installed completely onto their respective hose barbs and that the hose clamps are tight Connect the supplied cable between the Circulator RS 232 connector and the Test Station Signal Panel CIRCULATOR connector Inlet Line Clamp A clamp should be installed on the hose running from the c
31. Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 for a sample of fixed length and width and the minimum and maximum thickness the tool can accommodate 2 Generate an X Y scatter plot of sample thickness Y axis versus complex modulus G X axis The region between the upper and lower limits of operation is the range of complex modulus that can be tested ARES User Manual Coefficient of Thermal Expansion a When testing at other than ambient temperatures the coefficient of thermal expansion for Torsion Rectangular geometry is defined as AL 1 At Lo where Coefficient of Thermal Expansion a At Change in temperature C Lo Original length of sample mm AL Change in length of sample mm Positive AL indicates increasing sample length Tool Installation 1 Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise the stage to the loading position 2 Verify that the motor is on and in dynamic mode 3 Mount the upper and lower tools on the actuator shafts 4 Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset torque to Zero bu
32. VALUE is nominally about 5 higher than the maximum force that is measurable by the transducer in use This value should not be zero nor should it be a very large number such as 1E 5 If it is enter the correct full scale value for the transducer in use see nstrument Specifications then repeat the calibration 2 Exit the calibration operation and cycle the instrument main power turn off then on Repeat the calibration 3 Call Technical Service PHASE ANGLE CALIBRATION During Phase Angle Calibration with a steel Repeat the calibration only once sample the phase angle is not within the limits specified in the calibration procedure An eee con echon aie offset are reasonable Ensure sample is loaded correctly Verify static force is correct and in proper direction Remove the sample exit the calibration operation then cycle the instrument main power turn off then on Re load the sample and repeat the calibration Call Technical Service ARES User Manual Operation Table 6 2 Instrument Operation Troubleshooting Guide PROBLEM CORRECTIVE ACTIONS MOTOR Motor does not engage or respond to command Ensure that the motor is on Ensure that the instrument is not in an OVERLOAD condition OVERLOAD is indicated by an online indicator If an OVERLOAD is indicated reset the test using the function END TEST RESET LS Motor Only Ensure that motor air pressure is 60 psi Call Technical Service Moto
33. and Single Pulley Installed ARES User Manual 9 10 11 12 13 14 Table 5 2 Calibration Lines TRANSDUCER CALIBRATION LINE 2K FRTN1 Cut one length monofilament line 2K FRTN1E part number 613 01075 1K FRTN1 2K STD 100 FRTN1 200 FRTN1 Cut one length of thread 100 FRT part number 613 00716 200 FRT Cut two separate lengths of monofilament 10K STD line part number 613 01075 Access the Transducer Characteristics form using the Orchestrator function Calibrate Instrument under the Utilities pull down menu Select the XducerCal button Establish a zero torque reference value by selecting the Zero button Wait about 30 seconds during which time the instrument takes several readings to establish a zero normal reference When zeroing is completed the Transducer Calibration form is displayed Figure 5 4 The zero value displayed in this form should be less than 0 1 of the full scale Torque value If after selecting the ZERO button the TORQUE value displayed is either very high such as 1E 5 or exactly zero refer to the Troubleshooting Guide NOTE Do not hang any weights until after at least one 1 zero reading has been taken Apply a calibrated torque Figure 5 5 depending on your transducer as follows a Place one end of the line over the hub on the calibration tool and place the line in the groove of the pulley b Hang the weight specified in Table 5 3 depending on the trans
34. and cups using various transducers and a standard motor Tool Installation If you are installing the lower tool into either of the fluid baths please refer to the appropriate section of Chapter 2 for your specific bath for additional information before installing the tool into the bath 1 Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise the stage to the loading position 2 Verify that the motor is on then mount the upper tools on the transducer shaft and lower tool into the fluid bath or actuator shaft depending upon which environmental control system is being used 3 Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset Torque to Zero buttons Sample Loading In general pour the sample into the cup then lower the bob until the upper surface of the bob is 1 to 2 mm below the surface of the sample Figure 4 13 Note that the upper surface of the bob must be between zero and five millimeters below the upper surface of the cup If this is not the case adjust the sample volume accordingly Nominal sample volumes are as follows Bob Cup size Sample Volume 16 5 mm 17 mm 25 mm 27 mm 32 mm 34 mm Vane 34mm 192 ARES User Manual UPPER SURFACE OF CUP UPPER SURFACE OF BOB UPPER SURFACE OF BOB MUST BE NO HIGHER THAN UPPER SURFACE
35. are desired Unlike Parallel Plates the gap for a Cone and Plate is fixed and defined by the cone geometry Because of this the Cone and Plate is normally used for isothermal testing only as temperature changes would lead to changes in gap due to thermal expansion For special cases however Invar tools can be used Because of Invar s exceptional thermal expansion properties Invar tools are used for applications where temperature ramps or sweeps are necessary ARES User Manual Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using the cone and plate geometry The following geometry specific factors affect the operating range of cone and plate geometry e Plate diameter strain constant K and stress constant Kz e Cone angle strain constant K Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type using the cone and plate geometry use the following equation E C 41 Y where K Stress Constant K Strain Constant and C is computed from the following C for G MAXIMUM C for G MINIMUM 2K FRTN1 2K FRTN1E l J 1 15e 06 rad gecm a see note bel
36. bottom of the Test Station During installation the Test Station will be removed from the pallet and placed on the workbench Retain the pallet for future use in case the Test Station requires moving To place the Test Station back on the pallet use a forklift to position the pallet flush with the workbench top and slide the Test Station onto the pallet WARNING Do not attempt to lift or carry the Test Station by hand Use a fork lift that is rated to carry the weight of the Test Station Attempting to lift or carry the Test Station by hand can result in serious personal injury or damage to the Test Station ARES User Manual 229 Special Maintenance Service and Repair of the Test Station Other than the routine maintenance listed in the previous section there are no other repairs or service that you as the customer can perform Contact TA Instruments regarding service or repairs as well as the availability of service contracts and plans Diagnostic LEDs Each removable circuit board on the Test Station Mother Board is equipped with a bank of diagnostic LEDs light emitting diodes that indicate the operational status of key electrical signals Figure 6 1 shows the location of the LEDs which can be viewed by opening the access door The electronics are protected by a metal shield that allows inspection of the LEDs during basic troubleshooting The electrical signal monitored by each LED is labeled Except as noted in Figure 6 1
37. calibration menu screens or procedures we provide the following option in Orchestrator for adjusting the ARES for temperature error effects Please note that this option is only available for ARES firmware version 5 xx and above Obtain a table of calibration temperatures relative to PRT temperatures using either a reference thermometer or known samples transition points as described above If using material transition points more than one material should be used for greater precision across a broad range of temperatures Under the Utilities pull down menu select the Instrument Configuration function from the Service function table Select TEMPERATURE CONTROL Figure 5 11 Near the bottom of the form click Adjustable for the Temperature Calibration Table A table will be displayed with up to 20 windows to input the calibration values Enter the measured and theoretical values for each calibration points obtained leaving the remaining windows unaltered The ARES will now adjust temperatures measured by the PRT according to the calibration table linearly interpolating between table values It is recommended that you enter the same commanded and calibrated values for room temperature so that there is no offset at room temperature ARES User Manual Setup Instrument Options Temperature Control e Oven Air Chiller or LW2 Dewar 500 0 150 0 Oven Air Temperature Ea 0 0 100 0 150 0 200 0 3595 0 2 0 101 5 151 0 00 5 3999 0
38. current required to drive back to null position is proportional to the amount of force applied This current is converted to DC voltage and scaled to become the force torque output of the transducer All Force Rebalance Transducers are dual range Selection of range is performed using Orchestrator software Firmware versions 5 00 00 and higher automatically switch ranges during a test FRT transducers are also available with normal force measurement capability For the normal force option the measurement range in tension downward is 60 that of compression upward due to the weight of the transducer shaft being supported by the normal force servo Standard Transducer STD The Standard transducer provides high frequency response with the ruggedness required by QC labs They are generally used for solids and melts testing since they typically lack the low end sensitivity needed for fluids measurements The Standard transducer utilizes a shaft that is supported by a torsion bar Mounted to this is a moment arm A position sensor on each end of the moment arm produces rotational position information In response to rotation in a given direction the output of one sensor increases while the other decreases A torque signal is then derived by taking the differential between these two outputs The torsion bar and moment arm are axially supported by a flat spring allowing axial compliance A third position sensor mounted to the top of the spring assem
39. data gathered over many cycles Strain Amplitude Control Measurement does not begin until the strain that you command during a test is within a certain percentage of the strain actually applied to the sample This feature allows you to specify this percentage Default Does not use strain amplitude control The actual sample strain is simply recorded Adjustable Measurement begins when sample strain is within the entered percentage of initial commanded strain This will increase the test time as the motor movement increases to reach the desired sample strain ARES User Manual ARES User Manual Dynamic Frequency Sweep Test Strain Control Figure 3 29 Measurement Options Set up Screen ARES User Manual Chapter 4 Test Geometries and Formulas Introduction This chapter provides information on the various test geometries and formulas that are used with the ARES instrument The following material is covered e General Test Tool Information e General Test Tool Installation e Zeroing and Setting the Gap e Specific Test Tool Geometries e Test Formulas General Test Tool Information General Recommendations for Geometry Selection Although the physical properties of the sample generally dictate appropriate sample geometry it is sometimes possible to test a given sample using more than one geometry Ideally the test results should be identical in the different geometries However there exist experimental limitations
40. dynamic zero position Figure 5 9 5 Select the parallel plate geometry as the current geometry and enter the following tool dimensions 6 Setup a Dynamic Time Sweep with the following conditions Current ambient temperature 7 Run the Dynamic Time Sweep 8 Ensure that the following conditions exist a The STRAIN value reported is between 24 90 and 25 10 b The pointer deflects 0 25 radians as shown in Figure 5 9 If either condition is not met contact TA Instruments Service group for further assistance 9 Stop the Dynamic Time Sweep This concludes the Strain Calibration Check ARES User Manual POINTER DYNAMIC wo POSITION LS 0 25 RADIANS Figure 5 9 Strain Calibration Check with Pointer ARES User Manual System Check Using PDMS Included in the calibration kit supplied with the instrument is a jar of PDMS PDMS polydimethy siloxane is a rheological reference material that is used to verify the correct operation of the test station A PDMS test should be run periodically to ensure proper operation of the instrument It should also be run as a preliminary diagnostic any time there is a question regarding instrument performance Procedure 1 Turn on the motor and ensure that it is in dynamic mode 2 Ensure that the transducer range is in high range use the Orchestrator function Utilities Service Transducer 3 Install the 25 mm parallel plate test tool see Chapter 4
41. geometry The following geometry specific factors affect the operating range of torsion rectangular geometry e Thickness of sample stress constant K and strain constant K e Width of sample stress constant K and strain constant K e Length of sample strain constant K Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor 178 ARES User Manual To calculate the minimum and maximum G that can be measured by each transducer type using the torsion rectangular geometry use the following equation Ke lc 4 1 r Y where K Stress Constant K y Strain Constant and C is computed from the following Transducer C for G MAXIMUM C for G MINIMUM 2K FRTN1 1 Cz a min 2K FRTNIE C 0 1 F J 1 15e 06 rad gecm a see note below This transducer is not generally recommended 1K FRTN1 for use with this tool However it may be used for some limited applications 2K STD 10K STD 0 1 J 2 60e 06 C see note below 100 FRT ace a These transducers are not recommended 200 FRTN1 for use with the torsion rectangular tool NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination
42. gram centimeter of applied torque Stiffness is the reciprocal of compliance Transducer compliance is the transducer shaft displacement resulting from torque applied to the transducer Shaft displacement is measured by a position sensor on the transducer shaft Sample compliance is sample displacement resulting from force applied to the sample Because the transducer is not an infinitely stiff device both the transducer and sample exhibit compliance Since the transducer is being deformed along with the sample some of the strain that is commanded deforms the sample and some of the strain deforms the transducer This leads to errors in sample moduli which becomes larger as sample stiffness increases ARES utilizes an on line hardware correction scheme to adjust for transducer compliance The system determines sample deformation strain by taking the difference between the measured motor and transducer displacement signals The measurement is sensitive to limits in strain resolution as well as variations in motor and transducer calibration and linearity Under ideal conditions the sample deformation is relatively large and as such the transducer displacement is much smaller than the motor displacement applying the torque The difference between the two deformations which is used to obtain sample displacement is therefore a large number and the relative error associated with the measurement is small However this error becomes significant
43. is not at the limit of its travel if it is adjust accordingly Ensure that the AutoTension Window is set to a reasonable value if not re set Call Technical Service ARES User Manual 235 Table 6 2 Instrument Operation Troubleshooting Guide Continued PROBLEM CORRECTIVE ACTIONS RUNNING A TEST AND COLLECTING DATA Erratic data points or missing data For FRT Transducers Only Ensure that the correct air pressure is supplied to the transducer in use see instrument specifications if pressure is incorrect go to 2 Ensure that AutoTension is functioning correctly if not go to 8 3 Ensure that the oven is not in contact with the upper and lower test tools if so go to 8 4 Ensure that the sample is loaded correctly 5 Cycle the instrument main power turn off then on 6 Ensure on line indicator shows ON TEMP 7 Run confidence check with steel shim 8 Perform a torque calibration 9 Perform a strain check 10 Check force level for overload condition 11 Check that pretension is correct 12 Make sure the sample stiffness dimensions are reasonable for the test tool 13 Call Technical Service ARES User Manual TA Instruments Offices For information on our latest products and more see our web site at www tainst com TA Instruments Inc 109 Lukens Drive New Castle DE 19720 Telephone 1 302 427 4000 or 1 302 427 4040 Fax 1 302 427 4001 HELPLINE U S A For assistance p
44. one of the following depending on the transducer type e 2K FRIN1 or 2K FRINIE delivered after January 2002 see note below Push the pin toward the right of the instrument until the left clamp contacts the transducer housing e 100 FRTN1 200 FRTN1 or 1K FRTN1 Push the pin toward the front of the instrument until the rear clamp contacts the transducer housing To Unlock the FRTN1 bearing 1 Read the Caution on page 11 2 Ensure that instrument power is off and air is applied to the transducer 3 Do one of the following depending on the transducer type e 2K FRTNI1 or 2K FRTNIE delivered after January 2002 see note below Push the pin toward the left of the instrument until the right clamp contacts the transducer housing e 100 FRTN1 200 FRTN1 or 1K FRTN1 Push the pin toward the rear of the instrument until the front clamp contacts the transducer housing NOTE 2KFRTN1 Bearing Lock Orientation During design revisions to the 2KFRIN1 transducer the bearing lock direction was changed Transducers delivered before January 2002 have the bearing lock arranged so that the locked position is with pin pushed to the left and the right clamp touching the transducer housing Transducers delivered after January 2002 approximately are just the opposite the locked position is with the pin pushed to the right and the left clamp touching the housing It is very important to know which locking arrangement your transducer has In general instrum
45. proprietary technology patented by TA Instruments Waters LLC U S Patent No 5 710 426 Thermogravimetric Apparatus describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 5 321 719 Power Compensation Differential Scanning Calorimeter Tzero describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 6 428 203 Differential Scanning Calorimeter Tzero describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 6 488 406 Apparatus and Method for Measuring Viscoelastic Properties of Materials describes proprietary technology patented by Rheometric Scientific Inc acquired by TA Instruments Waters LLC January 2003 U S Patent No 4 601 195 Other Trademarks Windows NT 2000 XP 98 985E Me Microsoft Excel and Microsoft Word 97 are registered trademarks of the Microsoft Corporation Adobe Acrobat Reader are registered trademarks of Adobe Systems Incorporated Oracle and Oracle9i are trademarks or registered trademarks of Oracle Corporation TrueMetrix and Scanning Tip Technology are registered trademarks of ThermoMicroscopes Inc CHROMEL and ALUMEL are registered trademarks of Hoskins Manufacturing Company Teflon is a registered trademark of E I du Pont de Nemours and Company Loctite is a registered trademark of the Loctite Corporation continued on next page 6 ARES User Manual Ot
46. range use the Orchestrator function Utilities Service Transducer 3 Install the Torsion Rectangular tool see Chapter 4 4 Load the calibration steel sample part number 400 02589 that is supplied with the tool see Chapter 4 for details 5 Conduct a Dynamic Frequency Sweep using the following parameters FREQUENCY 0 1 to 100 rad sec log sweep STRAIN 0 02 TEMPERATURE Current ambient temperature Ensure that the phase angle 6 is 0 25 throughout the frequency range If the values obtained from this test are outside this range please contact Technical Services for further assistance ARES User Manual Procedure for 100 FRTN1 200 FRTN1 100 FRT 200 FRT and 1K FRTN1 1 2 Turn on the motor and ensure that it is in dynamic mode In Orchestrator enter the Edit Start Instrument Test function Select Parallel Plate Geometry and then press the Edit Geometry button Select the Options button and enter a fluid density of 1 g cm in the displayed form Ensure that the transducer range is in high range use the Orchestrator function Utilities Service Transducer When checking the 1K FRTN1 only set the transducer to the low 20 gecm range Install the 50 mm parallel plate test tool see Chapter 4 Load the 1000 cP Newtonian Calibration fluid part number 700 01016 with a gap of 1 millimeter Conduct a Dynamic Frequency Sweep using the following parameters p FREQUENCY 0 1 to 100 rad sec log sweep
47. remain constant for the life of the system The phase angle correction is computed and entered into Orchestrator at the factory before the instrument is shipped and should not have to be adjusted under normal operating conditions It is recommended that the phase angle be checked periodically using the following procedures to ensure that the entire system is functioning properly If the values obtained from this test are abnormal please contact Technical Services for further assistance To check the phase angle using the 2K FRTN1 2K FRTNI1E 2K STD or 10K STD Transducer a Dynamic Frequency Sweep is run on a steel sample that is loaded into a torsion rectangular tool Recall that a purely elastic sample has a phase angle of zero degrees The phase angle of steel is near zero If using any of the 100 FRTN1 200 FRTN1 100 FRT or 200 FRT transducers a Dynamic Frequency Sweep is run on a 1000 cP Newtonian fluid calibration fluid that is loaded onto a parallel plate tool Again recall that a purely viscous sample has a phase angle of 90 degrees The phase angle of the Newtonian fluid is near 90 degrees To check the phase angle for the 1K FRTN1 transducer either the steel sample or oil sample may be used Procedure for 1K FRTN1 2K FRIN1 2K FRTN1E 2K STD and 10K STD Transducers 1 Turn on the motor and ensure that it is in dynamic mode 2 Ifthe transducer is a 2K FRTN1 2K FRTN1E or 1K FRTN 1 ensure that the transducer is in high
48. shown in Figure 2 38 Setup Instrument Options Ei Ed Figure 2 38 Setup Instrument Options Form Used to Input the Fluid Bath System Configuration NOTES 1 Make sure the following are selected e Instrument Setup TEMPERATURE CONTROL e Temperature Control BATH INSTRUMENT CONTROLLED ONLY 2 Ensure that the maximum and minimum temperatures corresponding to the desired circulator operating range and fluid See the previous topic Filling the Circulator are entered in the Max and Min Temperature fields 3 Select either Temperature Loop Control option using the following information as a guideline e Circulator Temperature When selected the temperature of the fluid in the circulator is maintained at the commanded temperature The lower tool PRT is independent of the circulator temperature and due to its location will report temperatures that are slightly different than the commanded circulator temperature The circulator temperature control should be used when running step or ramp type temperature studies where a controlled steady temperature change or speed is more critical than actual sample temperature 90 ARES User Manual NOTE continued e Tool Temperature When selected the temperature of the lower test tool is maintained at the commanded temperature Tool Temperature control is the recommended setting for isothermal and some step testing where controlling the actual sample temperature is most importa
49. step increases in strain while holding frequency and temperature constant Two types of strain sweeps can be executed Figure 3 6 as follows Logarithmic Strain Sweep The logarithmic strain sweep uses the entered strain values in dimensionless strain units as the upper and lower strain limits of the sweep An increment or step size also in strain units must be entered Increments are performed in logarithmic steps The number of points per decade includes the initial strain but excludes the final strain As an example consider a sweep conducted over a single decade of strain between 10 and 100 Selecting five data points to be measured per decade divides the difference of the endpoint logarithms into five equally spaced fractional exponents so that six discrete strains are generated e Initial Frequency 10 e Decade Frequencies 15 9 25 1 39 8 63 1 e Final Frequency 100 One data point is measured at each of the strains Up to 500 data points can be measured per each decade of strain Logarithmic strain sweeps can be run in ascending or descending order and can begin or end at any strain within the range of the instrument Linear Strain Sweep The linear strain sweep uses the entered strain limits The test starts at the initial strain and continues until the final strain is reached adding the strain increment to each subsequent strain if the final strain is greater than the initial value or subtracting the incre
50. suggest that you partially insert the tool by placing a phenolic spacer between the upper lip of the lower tool and the surface of the bath Allow the lower tool temperature to match that of the bath then remove the spacer and fully insert the lower tool ARES User Manual 197 Assemble the lower tool cup by installing the inner cup into the outer cup using the mounting screw provided Figure 4 16 Make sure the o ring is present clean and free of defects Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise the stage to the loading position Verify that the motor is on then mount the upper tool on the transducer shaft and lower tool and PRT into the properly installed fluid bath Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset Torque to Zero buttons Using the manual stage control buttons lower the stage until the upper surface of the bob is below the upper surface of the cup Figure 4 15A Place a straight edge across the upper surface of the cup While monitoring the normal force raise the stage slowly until the upper surface of the bob touches the straight edge There will be a visible increase in normal force when the bob contacts the straight edge Figure 4 15B Zero the gap using the Zero Indicator button in the Set Gap Instrument Control function
51. test station input or air dryer and purge the lines before re powering your instrument To quickly determine if there is an interruption in the air supply we have found that it is helpful to install a pressure gauge before the air dryer Pneumatic Connections Figure 2 15 shows the location where all the pneumatic connections are made Connections are made using standard fittings The connections to the air supply MAIN and N2 GAS ports use quick disconnect fittings Table 2 3 identifies and describes Pneumatic connections on Pneumatics Panel necessary for test station operation ARES User Manual Connector AIR SUPPLY MAIN AIR SUPPLY N2 GAS GUN HEATERS OVEN PRESSURE SENSOR ARES User Manual Table 2 3 Pneumatic Connections Connected to the external air dryer Connected to an external nitrogen or other gas supply Connected to the oven Connected to the oven Connected to the oven Pneumatic input to the Test Station Used to supply air to the oven and throughout the Test Station Supply pressure should be 80 psi Pneumatic input to the Test Station Supplies nitrogen or other gas to the oven thus allowing Nitrogen gas to be used as the heating medium Supply pressure should be 60 to 70 psi Pneumatic output from the Test Station to the oven Supplies the oven with air or N gas depending upon position of Gas Supply to Oven selector switch black knob below pressure gauges Pne
52. the sine of the phase angle gives the out of phase component of the stress G which is proportional to the amount of energy lost to viscous dissipation 9 ARES User Manual Data Correlation All dynamic mechanical data correlation is performed on between 1 and 64 cycles of oscillation depending upon the testing frequency as shown in Table 3 3 Table 3 3 Single Point Measurement Data Correlation Frequency rad sec Cycles of Correlation The control computer samples 2 048 data points regardless of the test frequency The number of cycles of correlation determines the number of data points sampled per cycle For example at frequencies less than 2 rad sec the computer samples all 2 048 data points during one cycle of strain and force At 500 rad sec only 32 data points are sampled At higher frequencies fewer points per cycle are used however the data is collected over multiple cycles so the actual number of data samples still totals 2048 At least one complete cycle is required for correlation resulting in measurement time being inversely proportional to frequency This is an important consideration when observing materials that change rapidly over time such as cures involving gels and thermosets where sample material properties may differ dramatically between test start and completion ARES User Manual 4 SE REFERENCE SINE WAVE X REFERENCE 90 Y B FORCE S ANN SZ STRAIN A Dynamic Measureme
53. threaded collar Three screws fasten the rotating Shaft of the Fluid Bath Figure 2 21 to the Test Station Motor Anvil A threaded collar secures the Fluid Bath Body to the Test Station Motor Housing Two hoses supply fluid between the Fluid Bath and the fluid source which is typically a computer controlled circulator Prior to mounting the Fluid Bath perform the following actions on the ARES instrument e Raise the Stage to maximum height e Remove all Upper and Lower Test Tools and loosen the Anvil Tightening Knob on the Motor Anvil e Thoroughly inspect the Test Tool mounting surfaces i e the transducer anvil and the motor anvil and clean off any material that may interfere with the mounting of the Fluid Bath This is essential to ensure proper mechanical mating between the bath and the instrument e Turn off the Motor using the Instrument Control Panel Figure 2 22 while performing the following steps to install the bath 1 Remove the protective plastic base from the Fluid Bath Threaded Collar by placing the two pins on the Threaded Collar Spanner Wrench provided into two of the holes machined into the Collar and rotating the wrench counterclockwise 2 Gain access to the Shaft by sliding the cover of the Fluid Bath fully upward 3 Hold the Fluid Bath above the ARES Motor Anvil with the Bath Hoses facing toward the right of the instrument ARES User Manual 4 Rotate the Fluid Bath Shaft to align the flat portion of th
54. transducer x WARNING This is a high torque motor Turning on the motor while in Never turn on the motor while a sample is loaded Keep hands clear of the motor ARES User Manual Motor On Off Control Power to the Motor is controlled using the Instrument Control Panel function available in Orchestrator software To turn the Motor on or off open the Instrument Control Panel by either clicking the Control Panel button Figure 2 3 which appears on the Tool Bar or from the Control pull down menu Choose either MOTOR POWER ON or OFF then select the Ok button l Control Panel Button Instrument Control Panel ki E4 Environmental Control Settings Temperature i 00 0 PC Max 500 0 C Min 1 50 0 Temperature Control f Oyen Air Chiller or LN2 Dewar Environmental Controller 1 Off On Motor Control Settings Ok Help Cancel Figure 2 3 Instrument Control Panel NOTE If the Environmental Controller option is set on the Control Panel will appear as in Figure 2 20 Motor Oven Stop The Motor Stop and Oven Stop Buttons on the front panel of the Test Station will quickly and unconditionally power down their associated component To turn the motor or oven back on use the normal software controls ARES User Manual Transducer The transducer Figure 2 2 measures force generated by the sample during deformation by the motor The sample is mounted between the motor and tr
55. 13 01222 4980 to 5020 9975 to 11 025 ARES User Manual Normal Force Calibration for All Transducers Normal Force Calibration ensures that the transducer is properly measuring normal force The calibration involves hanging a precision weight on the calibration tool which is mounted on the transducer during calibration The applied normal force is the amount of weight applied to the calibration tool For example hanging a 1000 gram weight applies a normal force of 1000 gmf Normal Force Calibration Procedure 1 If calibrating an FRT ensure that the transducer is set to High Range before proceeding To set the transducer to High Range do the following a Access the Set Transducer Characteristics form Figure 5 7 by selecting the Transducer option from the Service function of the Utilities pull down menu b Using the Transducer Selected menu select the high range transducer then click Ok 2 Turn on the motor 3 Raise the stage to maximum height and remove any test tools 4 Install the calibration tool as shown in Figure 5 2 the pulley need not be installed 5 Using the Set Gap Instrument Control function in Orchestrator zero the normal force on the motor using the Offset Normal Force to Zero buttons 6 Access the Transducer Characteristics form using the Orchestrator function Calibrate Instrument under the Utilities pull down menu 7 Select the XducerCal button Establish a zero torque reference value by selecti
56. 170 degree C activates the absorbent qualities of the getters NOTE Operate the LN2 controller for 15 minutes at least once every 60 days to maintain the insulating properties of the LN2 transfer line Oven Gas Selection Either gaseous nitrogen N or air can be flowed through the heaters during a test To switch between N and air use the Gas Supply to Oven Selector Switch located below the pressure gauges on the Pneumatics side panel Figure 2 15 Rotate the valve to the desired position positions are labeled When using the optional LN2 Controller you can select to flow gases through the heaters in either of the following two ways through software control 1 Use evaporated liquid nitrogen LN at all times 2 Use liquid nitrogen until a specified temperature is reached then use either nitrogen gas or air thereafter depending upon which gas input port is selected with the Gas Supply to Oven Selector Switch 3 When using the gas switching option the input temperature for switching from LN to Gas should be approximately 10 degrees higher than the input to switch from Gas back to LN This will prevent the system from switching back and forth between the two sources at the switch temperature since when switching from liquid nitrogen to gas there is a momentary change in temperature as the switch takes place Enable the Gas switching option and set the switch point temperatures using the Set Test Conditions function in
57. 34 93 600 93 00 Fax 34 93 325 98 96 SWEDEN NORWAY Waters Sverige AB TA Instruments Division PO Box 485 Turebergsvagen 3 SE 191 24 Sollentuna Sweden Phone 46 8 59 46 92 00 Fax 46 8 59 46 92 09 AUSTRALIA TA Instruments C O Waters Australia Pty Ltd Unit 3 38 46 South Street Rydalmere NSW 2116 Australia Phone 613 9553 0813 Fax 61 3 9553 0813 ARES User Manual A AC Power main power switch 51 specifications 28 Air See Gas input options Air Dryer 33 54 55 228 Air Quality 54 Analog Data Input 125 144 Arbitrary Waveshape Test 127 AutoStrain 145 AutoTension 142 B Bearing Locks FRT with normal force 42 FRT without normal force 41 low shear LS motor 45 standard motors 45 Standard Transducer 41 Boltzmann Superposition Principle 112 C Calibration normal force 215 phase angle check 218 strain check 220 temperature 224 torque 210 Calibration Intervals 208 calibration procedures 207 ARES User Manual Index Chiller description 59 diagram 60 electrical specifications 29 physical specifications 28 circulator 27 30 48 67 70 77 88 Cleaning the Instrument 228 COM Port 48 Complex Modulus E 94 Compliance definition 150 determination of operational range 151 Cone and Plate test tool constants 173 tool installation 175 general information 173 operating range 174 sample loading 176 Constant Stress Test 137 Corre
58. 4 Load the PDMS part number 700 01011 using a gap of 2 millimeter 5 Conduct a Dynamic Frequency Sweep using the following parameters 5 for 100 or 200 FRT FRTN1 use 1 STRAIN SWEEP MODE Log INITIAL FREQUENCY 0 1 rad s FINAL FREQUENCY 100 rad s 6 Set up the plot to show G G viscosity and phase angle The displayed data should look similar to that shown in Figure 5 10 7 At the completion of the test select the GG Crossover function from the Analysis pull down menu The frequency and value where G and G cross crossover point is computed and displayed Compare the computed frequency and G G crossover to the values labeled on the PDMS jar Please note that on the PDMS jar crossover frequency in rad s is labeled Wc and the crossover value is labeled Gc no exponent is shown The computed crossover point should be within the error limits provided on the jar Press the Stamp button to place the computed crossover data on the plot This concludes the PDMS test ARES User Manual ARES User Manual Dynamic Frequency Sweep of PDMS G G Crossover Point 4 9045 2 438x10 Error 1 54 for Freq 6 94 for G Freq rad s Figure 5 10 Typical Results of PDMS Tests 90 0 80 0 30 0 20 0 ajbuyaseyd Temperature Calibration The temperature of the ARES is monitored by a Platinum Resistance Thermometer PRT which is automatically calibrated upon power up This calibration is
59. 6 5 mm bob 17mm cup for fluid bath or fluid bath 2 Enviromental Systems O D Ambient BATH MOUNT Oven Fluid Bath Fluid Bath 2 see Chapter 2 for more details regarding lower tool Couette Tool General Information The Couette tool is used for testing lower viscosity fluids that would not generate enough torque using parallel plates Itis also used where containment of the fluid would be difficult using other tools Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using the Couette The following geometry specific factors affect the operating range of the Couette e Length of bob stress constant K e Radius of bob strain constant K and stress constant K e Radius of cup strain constant K ARES User Manual Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type using the Couette use the following equation Ks o 4 1 cx Y where K Stress Constant K Strain Constant and C is computed from the following C for G MAXIMUM C for G MINIMUM 2K FRTN1 1 c Minin 2K FRTN1E C 0 1 E J 1 15e 06 rad gecm a Transducer see n
60. 76 D Ea T a iria E E A A did 76 C tor OPTIONS ore ira E o A N A T nase E EE E E EO A 77 esqui a Thermal Opera Fe NS Ao E o A 77 Tiss alla ork Pee and cena E AE dues E 78 Caireculator Cone cons ii tios 80 iaa o EE 80 Peltier Configuration in Orchestrator cocine 81 a AAA Po O e ee ee 82 Ester Op ra CCU CICS pri S 83 PCO ceca sees o E sonia eaennssescuesun E E E 83 Lei e A e o E em enn en ner rn A ee tel er eee te 83 A A A 85 TESS CUM a e A E A T E E E T E 85 ERO I A EA Ea EEA E II EAN TE 85 Lowe Toole aa Oaa E ee 87 S Een a era 88 Mc PP A TT E T T A A A T 88 AAA e o 88 Fluid Bath Configuration in Orchestrator cscsssssssssssssssssssssssssscsssecssssessssscssssesssseessnecessscsssnecssnecessecesseeseaneessn 90 A o rer re tere nee eee eee eer ee eee 91 Marl Bat OPeratie INCA UU ete in 6S enero inn pta a i 97 P Datl Operan oia 92 Chapter Test DescOpuoAS AAA AA 93 Iba Vago e hULeiaLo q A o Pre o O ter er ee ee ee 93 Sesso Hal a a Viscoclas uc sad is ceo 93 DS ciao ho al aa e T o Tee err ee ee ee 93 Hooke sand IN GW LOM e LAWS israel NN 93 PCAC SIN FOS UUM T A e CE A 94 Dinamme Meenanical TESTO pato 94 Pe in OTA oi Wi el NS APA OO pcan nasa E EET E S aceecunyeadeenestoe 94 Measurement MeMO paar odo 96 DET Ae ay PU a EE O O or PEI E E E E EE N gents 97 ARES User Manual Documents Describing Instrument Software Opera On sins 99 TET M 016 hc e e E E EE E E A E E E 100 Stran Controlled Dynamic Test Memo dsp 101 Dynamic Sin
61. ARES Rheometer PN 902 30026 Rev D June 2003 1999 by Rheometric Scientific Inc 2003 by TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Notice The material contained in this manual and in the online help for the software used to support this instrument is believed adequate for the intended use of the instrument If the instrument or procedures are used for purposes other than those specified herein confirmation of their suitability must be obtained from TA Instruments Otherwise TA Instruments does not guarantee any results and assumes no obligation or liability TA Instruments also reserves the right to revise this document and to make changes without notice TA Instruments may have patents patent applications trademarks copyrights or other intellectual property covering subject matter in this document Except as expressly provided in written license agreement from TA Instrument the furnishing of this document does not give you any license to these patents trademarks copyrights or other intellectual property TA Instruments Operating Software as well as Module Data Analysis and Utility Software and their associated manuals and online help are proprietary and copyrighted by TA Instruments Purchasers are granted a license to use these software programs on the module and controller with which they were purchased These programs may not be duplicated by the purchaser without the prior written cons
62. Analogli Df Autost OF MeasOps 04 Ok Options End of Test Save As Help Cancel Figure 3 3 Dynamic Time Sweep Test Set up Screen Suggested Use Time sweep provides a means of monitoring the time dependent behavior of a material for example thermal degradation at temperature curing in thermosetting systems or the build up or breakdown of network structure Test Options The following test options can be selected for use with the time sweep e Steady PreShear e Delay Before Test e AutoTension e Analog Data Input e AutoStrain e Measurements Options o Delay Settings o Strain Amplitude Control 102 ARES User Manual Frequency Sweep Functional Description The Frequency Sweep test takes successive measurements at selectable frequencies while holding a constant strain and temperature Ideally the selected strain should be within the linear viscoelastic region of the sample The time it takes to complete the test is highly dependent on the low end frequency selected For example a frequency sweep from 0 1 to 100 rad sec taking 10 data points per decade will take approximately 12 minutes Changing the range to 0 01 to 100 rad sec increases the test time to around 2 hours and running the test from 0 001 to 100 rad sec may take over 20 hours Three types of frequency sweeps can be executed Figure 3 4 as follows Logarithmic Frequency Sweep The logarithmic frequency sweep uses the entered frequency values as the upper
63. C Min 20 0 C Temperature Control Bath Instrument Controlled Only Motor Control Settings Motor Power Off tf Or Cancel Figure 2 40 Instrument Control Panel Showing Fluid Bath Control Options ARES User Manual Chapter 3 Test Descriptions Introduction Stress Strain and Viscoelasticity Definition of Terms Elasticity is the ability of a material to store deformational energy and can be viewed as the capacity of a material to regain its original shape after being deformed Viscosity is a measure of the ability of a material to resist flow and reflects the ability of the material to dissipate deformational energy through flow Material will respond to an applied force by exhibiting either elastic or viscous behavior or more commonly a combination of both mechanisms The combined behavior is termed viscoelasticity In rheological measurements the deformational force is expressed as the stress or force per unit area The degree of deformation applied to a material is called the strain Strain may also be expressed as sample displacement after deformation relative to pre deformation sample dimensions Sample deformations can be in the form of either simple shear where the material is deformed in a plane while confined between two surfaces or linear deformations where the material is either compressed or extended Hooke s and Newton s Laws Hooke s law describes the mechanical behavior of an
64. Commanded stress which is maintained by varying shear rate Positive Stress results in clockwise rotation Negative Stress results in counterclockwise rotation Time Duration that shear stress is commanded unless Max Allowed Strain see previous item is reached first When either Time or Max Allowed Strain is reached zero rate and zero stress is commanded Constant Stress Test El x Estimated Viscosity f3 00e 05 Pas Max Allowed Strain 1 00e 06 Points Per Zane 200 Max 350 Min 20 fea Stress Limits Pa Max tbs929 42 Min 6 392942 ht ee Zone Number 1 2 de Ed ao Ses ee Palfso0o foo ooo o ae sais ore Time sor homes EM lo E ee intense Options Delay Off MotorPID On ae E ee E Hien a Options End of Test Save As Figure 3 22 Constant Stress Test Set Up Screen ARES User Manual 137 Suggested Uses This test is used to measure the creep response of materials which provides transient information of the measured strain as a function of the commanded stress Options The following test options can be selected for use with the Constant Stress test e Delay Before Test e Steady PreShear e Motor PID ARES User Manual Stress Ramp Test Description Stress Ramp commands a steady stress level from an initial to a final stress at a selectable linear rate that is based upon zone time Positive Final Stress values result in clockwise rotation of the actuator stress head negativ
65. D SPECIFICATION 10K STD Measurement Range 0 2 to 2000 gecm 1 to 10 000 gecm Maximum Operating Frequency 500 rad sec 80 Hz NORMAL FORCE SPECIFICATION 2K STD AND 10K STD Measurement Range 2 to 1500 gmf 2 1500 gmf ARES User Manual Chapter 2 Instrument Components Identification and Operation Component Identification and Placement The base system Figure 2 1 consists of the Test Station with oven and Host Computer Additional optional components include LN2 Controller and an air filter dryer Figure 2 1 shows the recommended arrangement WARNING If this instrument is used in a manner not intended or specified in this manual the protection provided by the instrument may be impaired AIR DRYER Mount to wall behind test station LN2 CONTROLLER From Your Compressed Air Supply From Your LN2 Supply ARES TEST STATION HOST COMPUTER Figure 2 1 Base System ARES User Manual FRONT PANEL LCD DISPLAY STAGE TRANSDUCER OVEN OPTION MOTOR ACTUATOR MOTOR OVEN STOP BUTTONS MANUAL STAGE CONTROL FLUID BATH OPTION PELTIER OPTION Figure 2 2 Test Station Front View Including Environmental Control System Options ARES User Manual Host Computer The Host Computer allows the human operator to control the test station and to monitor display and analyze data during the test Control is achieved through Orchestrator software While some basic references to the software will be
66. Duration 2600 h m Figure 3 21 Steady Step Rate Temperature Ramp Set Up Screen ARES User Manual 135 Suggested Uses Steady Step rate Temperature Ramp can be used to examine the following e Process simulation e Transient material response to changing shear rates and temperatures Options The following test option is available when using Steady Step Rate Temperature Ramp e Delay Before Test ARES User Manual Stress Controlled Transient Test Methods Constant Stress Test Functional Description Constant Stress is a transient test that applies a stress in a selected direction for a specified time period in up to two zones In each zone rate is varied to maintain stress until either a strain or time limit is reached at which time zero stress is commanded When setting up the Constant Stress test the desired temperature to conduct the test and the sample estimated viscosity calculated by dividing the shear stress by the shear rate are first entered Figure 3 22 Then the Maximum Allowed Strain which is the maximum displacement of the actuator throughout the test is entered When either the maximum allowed strain or time see next item is reached zero rate and zero stress is commanded The estimated viscosity value is used to modify the gain term in the closed loop control algorithm which adjusts the motor s rotational rate to generate the desired stress level For each zone the following are entered Stress
67. ES User Manual Delay Before Test Manual Delay A manually entered Delay Before Test is the time period between the start of the test and the first measurement 1 through 65 000 seconds The time period selected in Delay Before Test Figure 3 25 allows the instrument to equilibrate or the sample to relax prior to imposing the deformation Apply AutoTension The Apply AutoTension at the End of Delay check box determines the point at which AutoTension is applied If left unchecked AutoTension is applied at the start of the Delay period Checking the box causes it to not be applied until the delay period has ended Automatically Start Test When On Temperature When checked the start of the test is delayed until the Environmental Control System has stabilized at the Commanded Temperature Figure 3 25 Delay Before Test Options Set Up Screen ARES User Manual 141 Auto Tension Adjustment AutoTension maintains a specified axial static force on the sample AutoTension can apply tensile force to keep the sample taut prevent sample buckling or compressive force to maintain a compressive load and prevent loss of test tool contact During dynamic testing using the Torsion Rectangular test tool AutoTension can be used to compensate for the change in sample length that occurs as a result of thermal expansion Using AutoTension with tools such as Parallel Plate can prevent loss of contact between sample and tool Following is a
68. Gap in millimeters b Max Allowed Force Enter the maximum Normal Force in grams force that will be generated while the sample is being compressed during the gap setting operation When Normal Force exceeds this value the stage stops descending until Normal Force drops below this value Stage movement then resumes 3 Click Set Gap An information form appears indicating the time elapsed since the button was clicked The Stage should descend relatively quickly typically 5 mm sec until the Upper Tool is 3 mm from the Commanded Gap Position at which time it will slow its rate of descent until the Gap is achieved The gap is set when the information form is no longer displayed Comments Concerning the Gap Control Panel Enabling the Gap Control Panel The Gap Control Panel function can only operate if the Stepper Motor and Remote Gap Monitoring options are enabled These options have been enabled at our manufacturing facility and should require no modification However for your reference these options are set by using the Instrument Configuration function located under the Service function of the Utilities pull down menu Set the Stepper or Linear Motor and Remote Gap Monitoring options to yes as shown in Figure 4 3 ARES User Manual Read Test Tool Gap Checkbox The Read Test Fixture Gap checkbox is located in the form used to edit a specific geometry accessed by clicking the Edit Geometry button in the Edit Start Test dialog bo
69. Member States relating to electrical equipment designed for use within certain voltage limits EN 61010 1 1993 Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General Requirements Amendments EN 61010 2 010 1994 Particular requirements for laboratory equipment for the heating of materials Amendments Electromagnetic Compatibility Standards For the European Economic Area In accordance with Council Directive 89 336 EEC of 3 May 1989 amended by Council Directive 93 68 EEC on the approximation of the laws of the Member States relating to electromagnetic compatibility Immunity EN 50082 1 1997 Electromagnetic compatibility Generic immunity standard Part 1 Residential commercial and light industry Emissions EN 55011 1998 Class A Technical Support For technical support concerning TA Instruments Rheometric Series please call 1 302 427 4070 8 a m to 5 p m USA ET Monday through Friday For technical support concerning Microsoft Windows please call Microsoft Corp at 1 206 635 7000 USA 6 a m to 6 p m USA PT Monday through Friday In other countries call the relevant Microsoft international subsidiary office ARES User Manual Table of Contents TA Instruments End User License Ac eC in iit erpressen a E a E E AS 3 Traiasmarksiand Pati A E Ie reer 5 TA Instruments Trademarks ai 5 SUE EEE E AAA a A O E TEE 5 Otier Trademarks ern rey ee TOT Re Tm ais apta T
70. N2 Controller The main power cord 220V IN must be disconnected from the Power Panel to completely remove AC power from the system ARES User Manual WARNING HIGH VOLTAGE is used in the operation of this instrument DEATH ON CONTACT may result if operating personnel fail to observe safety precautions Learn the areas of high voltage connections and exercise care not to contact these areas when performing instrument calibration Prior to working inside the instrument remove all jewelry turn off the power and ground points of high voltage before touching them Make adjustments using an insulated electronic adjustment tool Do not make physical contact with any component inside the instrument while power is applied to the instrument Instrument Labels Label found on the Rear of Power Chassis WARNING FOR CONTINUED PROTECTION AGAINST FIRE HAZARD REPLACE ONLY WITH SAME TYPE AND RATING OF FUSE Label found on the Front of Transducer FRT only INSTALL REMOVE LOCK WITH AIR PRESSURE ON Label found on the Front of Motor Mount WARNING KEEP HANDS AND LOOSE OBJECTS AWAY FROM MOTOR DURING TURN ON AND OPERATION Label found on the Front of Oven DANGER HOT TOOLS AND SURFACES ARES User Manual Regulatory Compliance Safety Standards For the European Economic Area In accordance with Council Directive 73 23 EEC of 19 February 1973 amended by Council Directive 93 68 EEC on the harmonization of the laws of
71. O Ao A 115 TEO EE O 115 Strain Controlled Steady Test MethodS eeseeeeeseseesesesersrsesesesereeseseserersesereseseeseseseseseressesesesessesesesesseseseseseeseseseseee 116 oead iomele Pola E E E 116 EUncuona DES 0 O en E A E E E tre 116 Pi o o E E seas yseeennanstosetssacateaaenins 116 Sa a A E E E N T E E sen stsecenae 117 OPONE A o e o o E EA OO AES 117 SPE WE oa 118 Puncuona DESEO erasmo ita olaa 118 Data Coleco MOS api E EE E A E E EAE E E 118 Dato A E E RO 119 roses de 6 US ata 119 OPUS o 120 Stralm Controlled Transient Test Methods eiiean a S 121 AP Ea 1 AE a o E E E E eco aceenue ae 121 ARES User Manual Funcional ISSO MOM nata tencia 121 BN OC SOS O nantes E EA O E E E E E E osa anaeees 122 TESCOP HONG eieae a a A N E rr rere E 122 Stress Relax ton Iransieni Step Stali ni pelo AAA EEA 123 Funciona CS iON r E E st cantecsansteo wuiaeeeadsaunsanedesnedemarcancsesoer 123 BS 0 IN IE OP O o E octet ep A E E E T 124 TES TOPS ie 124 PATO Te SiO MOS aaa 125 Funcuona FEDO ET PO iS 125 AREE ONO 11S AEA EEE E EEE E E E O E E E 125 oa AAA PO ee ee 127 ancora DESC D O a E A E T E E E E E O E 127 PCa OO yay ida 128 T D a E A E N E E E E E E E E E S 128 Topo 1G Loop Rale Ramp a oes a een ee 130 B el alle asa A A NA tne een rrerTe 130 ES Se Usas 130 OIA PP pease E ASS 131 Torque Normal Relato senti aia oia 132 Funcional Peger pO ienien E 132 Sre e O MN EU y EPR O E E E E E E E ses errno ees 132 dano erorii a E S E E sea
72. O nee erty E mre rn ny rr 187 rote Laat EOR AAA e ee iO O N E 187 A A II PUNA E E T EE seu emia 190 Cial dal Ml Sauces earn LO qee OR PUN A 190 dera AAA in A o 190 Took llo A e E Terr A ne rere irerrrre terre rrsr errr rere ery re 192 Sample LOIS anti toas 192 Va Vol is 193 TOM ca LO a AP o E A ETE 195 Eire EO AON AAA o e E a aE OENE 195 Opera NS KINE OS srr o ices inane re tinsaue i ntessaied E ous tuietegnatsotghescea nennes mmattentestiess 196 ToolInstallation Original WC Dri 197 sample Loading Orie mal Fluid Dalton oio ae eins 198 dio Melia iaa A o A 198 Tool installation Fluid Dat Zas TEE 201 Sample Oa End Dalila pops 201 Tool IV ar bees Elda Dat 2 eere EA eactessiersadscoesseaes 202 A o o E PE UU O O ere a ener rer oi 204 Dynamic Measurement Portas pistas 204 steady and Transient Measurement FOU AS sesspreicseneai ici 205 Chapters all Dra Mrs 207 A O reer N eter 207 A A 208 Calbraton Intel E E T A AE EE A E 208 Torque Calibration Or All Trans Quecers Muspnirain ita 210 IXOCS O so 210 Normal Force Calibration for All Transducers cccccscccccssssecesessececeesseceeessseeeecseseeeecsseeesessseeeeeneesees 215 ARES User Manual Normal Force Calibration Procedure c ccccccccccceccccccccccccccucccccccausceusceuesccucceuucceusccauseecscesceeseauseeeecens 215 A e o eee eee eee ee eee 218 I TOMY WI CAPA Po ie E A ve secede T A O 218 Procedure for 1K FRTN1 2K FRTN1 2K FRTNIE 2K STD and 10K STD Tra
73. Ops Oft Options End of Test Save As Help Cancel Figure 3 10 Frequency Temperature Sweep Test Set up Screen Suggested Use Frequency temperature sweep combines the frequency and temperature step methods to generate a group of curves which can be shifted using time temperature superposition TTS along the frequency axis to extend the range of frequency characterization beyond that which is experimentally practical at the chosen reference temperature From TTS data a master curve can be generated for the sample Test Options The following test options can be selected for use with the frequency temperature sweep e Steady Preshear e Delay Before Test e Analog Data Input e AutoTension e Measurements Options o Delay Settings o Strain Amplitude Control ARES User Manual 115 Strain Controlled Steady Test Methods Steady Single Point Functional Description Steady Single Point takes a single measurement while applying a steady shear deformation at a chosen shear rate Data are taken at the commanded shear rate and temperature Figure 3 12 Data can be collected using either of two modes Time Based Time Based data collection takes a single measurement Following the start of the test the Delay Before Measure is the time period between the beginning of motor motion and the beginning of data collection This allows time for the material to reach steady state The Measurement Time is the period during which data are actual
74. ROLLER uses the COMMAND signal and the SERVO SPEED and SERVO DISPLACEMENT feedback signals to drive the motor SERVO DRIVE applying deformation to the sample A feedback displacement signal SERVO DISPLACEMENT is derived from a sensor on the motor shaft SERVO DISPLACEMENT is conditioned and sent to the A D input as the strain deformation signal STRAIN Transducer The FRT Transducer is also configured as a position servo The transducer shaft moves as a result of the sample deformation that is applied by the motor A feedback displacement signal is derived from a sensor on the transducer shaft The torque applied to the transducer is proportional to the energy required to hold the transducer shaft at a known position This energy TORQUE RESPONSE is conditioned and sent to the A D input as the force applied to the sample FORCE The Standard transducer not shown in Figure 1 1 generates a signal proportional to the movement of the internal torsion bar without any active feedback control ARES User Manual Environmental Control System This instrument can subject the sample to a number of thermal environments using several different environmental systems When using the forced air convection oven two resistive heater guns mounted on the left side of the oven are used to control the sample test temperature An optional liquid nitrogen controller allows testing at sub ambient temperatures The power to the heaters is directed and moni
75. RTN1 1 92E 02 Low range 200 FRTN1 Appendix Table A1 8 Complex Modulus Limits for Cone and Plate FRT Transducer CONE ANGLE G MAXIMUM dynes cm G MINIMUM rad at Frequency rad sec dynes cm PLATE DIAMETER 9 22E 04 9 22E 05 4 79E 07 1 84E 04 1 84E 05 9 59E 06 3 69E 04 3 69E 05 1 92E 07 100 w 10 w lt 10 100 w 10 w lt 10 100 w 10 w lt 10 2 31E 03 w 2 31E 04 w 1 20E 06 4 61E 03 w 4 61E 04 w 2 40E 06 9 59E 01 High range 100 FRT 1 92E 00 High range 200 FRT 9 59E 02 Low range 100 FRT 1 92E 01 Low range 200 FRT 1 92E 01 High range 100 FRT 3 84E 01 High range 200 FRT 1 92E 02 Low range 100 FRT 3 84E 02 Low range 200 FRT 3 84E 01 High range 100 FRT 7 68E 01 High range 200 FRT 3 84E 02 Low range 100 FRT 7 68E 02 Low range 200 FRT 2 40E 02 High range 100 FRT 4 80E 02 High range 200 FRT 2 40E 03 Low range 100 FRT 4 80E 03 Low range 200 FRT 4 79E 02 High range 100 FRT 9 58E 02 High range 200 FRT 4 79E 03 Low range 100 FRT 9 58E 03 Low range 200 FRT ARES User Manual Appendix Table A1 9 Complex Modulus Limits for Couette geometry 2R 34mm 2Rg 32mm L 34mm TRANSDUCER TYPE G Maximum dynes cm at Frequency rad sec 100 FRTN1 3 94E 03 w 3 94E 04 w 2 05E 06 3 94E 03 w 3 94E 04 0 2 05E 06 G MINIMUM dynes cm 8 19E 02 High range 8 19E 01 Low range 4 10E
76. Rapid Cooling is displayed on the form Oven Pressure Source Selects the gas input to the oven Selecting Gas supplies either air or gaseous Nz Selecting LN2 supplies evaporated LN from the LN2 Controller LN2 Rapid Cooling Turns on off rapid cooling which evaporates LN2 at the maximum possible rate Rapid Cooling is always on at temperatures lower than 124 C Oven System Status Indicators Two special purpose neon lamps located on the front of the oven cover inform you of the status of the two gun heaters The top lamp shows the output level of the top heater When the lamps are at their brightest the heater guns are full ON Orchestrator Online Help provides instructions for choosing Online instrument status Indicators to be displayed along the bottom of the screen The following indicators can be displayed which show the status of the oven environmental system Environment On Off Oven Open Oven Open The oven is not closed This condition disables the oven environmental system Env On The oven environmental system is currently enabled Env Off The oven environmental system is currently disabled Gas LN2 Status Oven Only Gas Gas Either air or gaseous N2 is currently input to the oven LN2 Fill The LN2 Controller Dewar flask is currently filling with liquid nitrogen and the LN level is less than 50 of the flask capacity Temperature control will not be active while the Dewar flask is filling LN2 Ready The LN2
77. Reps Miri k Help Cancel Figure 2 39 PID setup form showing Fluid Bath settings The values listed in Table 2 11 should be used as guidelines and will work for most applications However you may need to experiment somewhat to determine their baths best PID settings for their system or specific applications The Orchestrator Online Help has a complete description of how to determine and tune the PID coefficients ARES User Manual Table 2 11 PID Values for Various Circulators and Fluids Circulator Julabo Julabo NesLab V5 NesLab V4 or FS 18 FS 18 firmware below firmware 50 Water Bath Fluid 100 Water 50 Ethylene Glycol 100 Water 100 Water Fluid Bath Operating Requirements The Fluid Bath can operate only if the following conditions are met e The Fluid Bath is selected as the current environmental system e The circulator must be filled on and circulating fluid through the bath e The circulator must be connected to the test station via the correct RS 232 cable e The clamp is set properly Fluid Bath Operation The Fluid Bath is operated using the Instrument Control Panel Figure 2 40 The desired temperature is set in the Temperature input field When testing at higher than ambient temperature the circulator set point must always be set to a temperature greater than the desired bath temperature Instrument Control Panel Ei E Environmental Control Settings Temperature 5 0 CC Max 150 0
78. S Oven Operation 3 RAA Oven Oven PRTs Lower Oven Oven gas temperature is maintained as in Mode 1 Air Temp both upper PRT Temperature is reported using the lower Oven PRT and lower Designed for use when lower tool does not support a The oven is operated using the Instrument Control Panel Figure 2 20 The options displayed on the Instrument Control Panel will be a reflection of the Environmental System Configuration entered using the Instrument Configuration function Table 2 5 describes the features of each option Instrument Control Panel ix Environmental Control Settings Temperature 100 0 PC Max 500 0 C Min 150 0 C Temperature Control Oven Sir Chiller or LN2 Dewar Environmental Controller off On Liquid Nitrogen Dewar Off On Oven Pressure Source C Gas LN LN2 Rapid Cooling C Off Or Motor Control Settings Motor Power Off On Figure 2 20 Control Panel showing Environmental Control Options ARES User Manual 65 Table 2 5 Description of Oven Control Options in the Instrument Control Panel OPTION DESCRIPTION Temperature Desired temperature to conduct test commanded temperature Temperature Control Selects the environmental system oven bath in use Set this to Oven Air Chiller or LN2 Dewar Environmental Controller Turns on off the oven environmental system Liquid Nitrogen Dewar Turns on off the LN2 Controller If on LN2
79. STION Figure 2 9 Bearing Lock Orientation 2K FRTN1 FRTNTE The view shown is looking from the front of the instrument A Systems delivered before January 2002 B Systems delivered after January 2002 ARES User Manual High Resolution HR and High Torque HT Motor The HT and HR motor do not require a bearing lock Low Shear LS Motor The LS motor bearing lock Figure 2 10 consists of a formed metal plate that is fastened to the motor anvil with 3 machine screws and one Phillips head screw To install this lock the motor cover must be removed Procedure for Locking and Unlocking Air Bearings LS Motor Refer to Figure 2 10 while performing the following procedures To Lock the LS Motor air bearing 1 oy PTA ly Read the Caution on page 11 Ensure that instrument power is off and air is applied to the Motor Remove the Motor cover Figure 2 21 page 68 retaining 1 of the Phillips head screws for the lock Place the lock on the motor aligning the 4 screw holes Inset the 3 machine screws and the Phillips head screw and tighten Retain the Motor cover and remaining Phillips head screws for re installation when the lock is removed To Unlock the LS Motor bearing i oS Read the Caution on page 11 Ensure that instrument power is off and air is applied to the Motor Loosen and remove the 3 machine screws and the Phillips head screw Remove the lock Install the Motor Cover NOTE the Phillips head screw re
80. Steady Single Point e Steady Rate Sweep Strain Controlled Transient e Stress Relaxation e Arbitrary Waveshape e Step Shear Rate e Thixotropic Loop e Force Gap Test e Torque Normal Relaxation e Multiple Extension Mode o Constant Force mode Creep Recovery o Strain Rate mode o Hencky Strain Rate mode o Rim Shear Squeeze Flow mode e Steady Step Rate Temperature Ramp Stress Controlled Transient e Constant Stress Test e tress Ramp Test ARES User Manual Strain Controlled Dynamic Test Methods Dynamic Single Point Measurement Functional Description The Single Point Measurement test makes a single measurement at a fixed frequency strain and temperature Dynamic Single Point Ei Ed Frequency fi 0 0 rads Max 500 0 Min 1 00e 05 SUMP fo Max 312 5000 Min 0 003125 Temperature 25 0 CE Mas 600 0 C Min 150 0 C Options PreShear 0f Delay Df Analoga O MeasOps Oft Options End of Test Save 4s Help Cancel Figure 3 2 Dynamic Single Point Test Set Up Screen Suggested Uses Suggested uses for single point measurement are as follows e Determination of unknown range response limitations of a new sample material e Determination of parameters for the design of new tests e Determination of force generated at various conditions and temperatures for the purpose of keeping force within the range of the transducer during sweeps Test Options The following test options can be selected for use with the sing
81. T WFL 1 00 G 1 8756TR l 00 G 1 8756TW Couette 1000XG 2TL R Y Double Wall Couette 1000 G 27L R Y t R Variables length mm W width mm T thickness mm R radius mm H height mm Ge gravitational constant 980 7 cm s cone angle Rpg radius of the bob Rc radius of cup For double wall Couette refer to Figure 4 16 for definition of Ry R2 R3 R4 ARES User Manual Chapter 5 Calibration Introduction This chapter contains calibration procedures that you can performed Do not attempt any calibration procedure unless you are thoroughly familiar with the operation of both the instrument and Orchestrator software Calibration procedures are given for Orchestrator version 6 5 6 which is the software released with the instrument at the time of this manual publication However menu and function names may change without notice during subsequent software releases WARNING HIGH VOLTAGE is used in the operation of this instrument DEATH ON CONTACT may result if operating personnel fail to observe safety precautions Learn the areas of high voltage connections and exercise care not to contact these areas when performing instrument calibration Prior to working inside the instrument remove all jewelry turn off the power and ground points of high voltage before touching them Make adjustments using an insulated electronic adjustment tool Do not make physical contact with any component i
82. TIONS TRANSDUCER Torque or Normal Force either does not respond Applies to FRT transducers only or is beyond full scale when no force is applied 1 Ensure that the correct air pressure is supplied to the transducer in use see instrument specifications if pressure is incorrect go to 3 Ensure that the transducer is unlocked Call Technical Service Stage does not move NOTE Manual AutoTension is activated by selecting the HOLD button see Orchestrator Online Help for details 1 Make sure the stage is not at its limit of its travel 2 Ensure that there is not a force overload condition 3 Ensure that manual AutoTension functions correctly if not go to 5 4 Ensure that manual AutoTension is not on when trying to move stage using the Stage Control if it is on turn it off 5 Ensure it is activated in firmware 6 Cycle the instrument main power turn off then on 7 Ensure that the oven is all the way to the left or all the way to the right 8 Call Technical Service Stage moves in only one direction when Ensure that a Normal Force Overload AutoTension is not in use condition does not exist if it does determine the cause Ensure that the stage is not at the limit of its travel if it is adjust accordingly Cycle the instrument main power turn off then on Call Technical Service Stage moves in only one direction when During sample loading ensure that the stage AutoTension is in use
83. Ts to ensure that they do not collide with the tool causing potential damage to the PRT To adjust the oven clearance do the following 1 Mount the lower tool and try and slide the oven past to tool 2 Note any clearance problems 3 Shave the foam using a razor knife or fine rasp Cover the motor with a paper towel or cloth to keep the shavings from getting into the motor 4 Slide the oven past the tool and again note any clearance problems 5 Continue shaving the oven until it slides past the tool Once the oven clears the tool close the oven almost all the way while noting the position of the lower PRT relative to the tool If the PRT will contact the tool adjust its position There is a mounting bracket that holds the PRT located on the top of the oven under the outermost cover Remove the outer cover to access the bracket Loosen the two screws and adjust the PRT position as necessary ARES User Manual 169 170 FLUID SEAL SAMPLE OVERFLOW WELL GLASS CHAMBER SAMPLE O RING LOWER TOOL PRT LOWER TOOL Figure 4 6 Cross Section Showing Fluid Seal Adjust PRT Position if needed using 2 Screws on PRT Top Mounting Plate OVEN INSULATION FOAM Shave Down This Edge As LOWER Needed OVEN PRT Figure 4 7 Oven Modifications ARES User Manual Tool Installation Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise
84. User Manual 201 Tool Maintenance Fluid Bath 2 To facilitate cleaning of the lower tool the inner cup can be removed from the outer cup Unscrew the inner cup mounting screw and remove the inner cup and O ring Figure 4 17 Clean the cup as necessary Reassemble the lower tool cup by installing the inner cup into the outer cup using the inner cup mounting screw Before reassembling the tool inspect the O ring for cuts or other damage and replace it if necessary Inner Cup Mounting Screw 1mm Gap i AN Gap must be 1mm to obtain A Effective Bob Length Outer Cup A L 32 mm Effective Bob Length Bob rf tm i Inner Cup ii F m l iit a rae 1 T Me i la R gt 2R INNER CUP DIAMETER 13 97mm 1 R 2R INNER BOB DIAMETER 14 75mmi R3 a 2R OUTER BOB DIAMETER 16 00mm I Ry p k OUTER CUP DIAMETER 17 00mm A cu Figure 4 17 Fluid Bath 2 Double Wall Couette Setup Showing Inner and Outer Cup as Well as Tool Dimensions 202 ARES User Manual Zero the Gap F Set Gap to 1mm Raise Stage and Fill Cup with Sample Lower Stage Back to 1mm Gap Sample Should Slightly Over Flow Lip Sample Volume 8 to 9 ml PA Minimum Sample Fill Level D Figure 4 18 Fluid Bath 2 Double Wall Couette Sample Loading Procedures A Zero the gap B Set the gap to 1 mm C Raise the stage and fill the cup D With sample loaded ARES User Manual 203 Test Fo
85. Zone 200 Max 350 Min 20 Zone Humber 1 J 3 4 Zone Time s or kmp Eo m m Direction ian Clockwise ote Options Preshear Of Delay Of Analogln Oft Options End of Test Save As Help Cancel Figure 3 19 Torque Normal Relaxation Test Set Up Form Suggested Uses e Determination of time required for a sample material to relax after a deformation as in sample material loading e Analysis of time dependent behavior of a sample ARES User Manual Options The following test options are available when using Stress Relaxation e Delay Before Test e Steady PreShear ARES User Manual Force Gap Test Description Executing the Force Gap test adjusts the sample gap to a specified value over a specified time Data can be collected during the time that the gap is changing The following parameters are set through the Force Gap Test Set Up Screen Figure 3 20 Force Sample Gap to In this field enter the sample gap that is desired at the end of the Force Gap test The test concludes when this gap is reached regardless of the Gap Adjustment Time next item Gap Adjustment Time This field determines the rate at which the gap command changes Enter the time period during which the gap will change from initial position at the start of the test to the gap specified in the Force Sample Gap to field Save Test Data When checked saves data that have been collected while the gap was changing The data are repo
86. accomplished by switching in precision resistors in place of the PRT and using the known resistance to adjust the offset and gain of the electronics However some errors can still exist due to PRT errors or temperature gradients that exist within the oven which cause the temperature at the PRT to truly be different than the temperature at the sample Although these errors are generally small they can lead to discrepancies between the temperature measured by the PRT and the actual temperature of the sample at any given time For studies that require the most exacting temperature accuracy it can be helpful to input a temperature calibration table to account for differences in measured temperature versus actual sample temperature However keep in mind that performing the calibration incorrectly could actually make the errors worse than doing nothing Of prime consideration is providing a temperature reference that is of sufficient accuracy to be used as a calibration reference One option is to mount an accurate thermometer in place of the sample and compare its output to that of the PRT at several temperature steps Another method used is to run a temperature ramp study on a material with well defined and well known thermal transitions such as the glass transition point and using the reported values to adjust the PRT temperatures Temperature Calibration using Orchestrator While temperature calibration is not handled under the standard instrument
87. al Force Calibration Remove the weight and calibration hook from the transducer and store both in the calibration kit Low Range High Range Set Transducer Characteristics E Transducer Selected a lTransducer Transducer 3 Transducer Description NN Maximum Torque lacmlf200 fio000 Mo Minimum Torque lg cm 0 004 ho oo Do o Torque Calibration Value 1 20 42 1021 0 loo 80 Torque Compliance J6 50e 06 650e06 00 Inertia Constant lger lf 160 po 80S Phase Adjust Constant rads rad 1 086 04 1 08e 04 00 w Maximum Normal Force lalf2000 0 f2o000 foo foo Minimum Normal Force uwus O20 f20 oo foo Normal Calibration Value faro 2101 56 foo foo SC Normal Compliance umkg 0 0 fo foo foo Phase Offset ccs sense fred 0 0 fo bo Joao OK XducerCal Help Cancel Figure 5 7 Set Transducer Characteristics Form Shaded windows show input cells for Torque and Normal Calibration values ARES User Manual 217 Phase Angle Check Principle The phase angle correction compensates for possible phase shifts that may be added to torque and strain due to A D filtering by the instrument electronics It is a function of the electronics and not the Motor or Transducer Once the correction is determined it should
88. alue exceeded the limit at any point If the sum of the wave times is less than the sum of the data collection times then the motor will remain stationary once the entire wave has been played Arbitrary Waveshape Test ki Temperature 25 0 PC Max 0 0 Min 0 0 C Points Per Zone 200 Max 350 Min 40 Aone Number 1 2 3 4 Time or hms jp oo ct ct ct Wave Time Wave Equation straini Ft where t ig time ze El Isnt l2 El BO ze El int fz ial Isnt Strain Limits Max 0 008905 Min 0 000000 Options Delay Of Options End of Test Wave Save Ag Help Cancel Figure 3 17 Arbitrary Waveshape Test Set up Screen In evaluating each equation the time for each equation is based on the running time since the start of the first equation For example if two equations are used each 2 seconds in length the time variable is evaluated from 0 2 seconds for the first equation and 2 4 seconds in the second If there are discontinuities in the strain value between the end of one equation and the start of another a jump in position will occur during measurement If this is not desired then the strain value should be contiguous from equation to equation in order to avoid such transients ARES User Manual 127 Once the strain equations and sampling times have been specified the waveform must be sent to the instrument The Wave button is used to compute the resulting waveform display the results g
89. ample Loading esmero olor onneani si ia Sa a aN 160 ROTC HG lme eae A E E 160 A e Beene E ere E e IU E E A E 161 E A na D o tai A E E A A N N 161 OPen Ene TN a A A ES 161 oa i o o A 163 pee aa LI 07 10 T 0 OCIO o O ee 163 Hlastelloy POOL tara lle Rates portones tino aaa cel 165 General Mora ON reo ocaciones 165 Uperitns NOS tia 165 Mts Re AAA A E E E EA once E E O aa eee ey apeteyecuiases 168 Sy AE Ue Vea adas 169 A OA 171 ARES User Manual Sample LOMO cesar 171 EP A soe 173 General doo iio 173 perane Nao iitis 174 i Deve Miatie 0l ciate q sip S A A Teer TTS 175 Oa OS a OCA E T e ate secu Er cose E A T 175 Testing at Other than Ambient Temperatures ocooconococcnonnnnnnnnananinonnnnnancnnononanononcnnnnnnanononnnnnann conc na nonncnnancanos 175 noe 1 Ak 6 Cal 8 2 6 o a pms ore eee E eR ener re E ee ee rere ee re ee eee 176 Torsion Kectansular New Destinos 177 A re tea UIT OT VAL ees a Go oaceamerp EE ease ssacetcuded atecneseeaiesadieoenshecteradaueet spe 177 sample DINOS catas 178 Clip TU an 178 Operas lea acia 178 Coefficient of Thermal Expansion O PP PI e o iaia aea nn aa aai 180 AAA E A E Un E errr E mn Ter arr 180 Sample GO io 181 Torsion Rectansulas Diana DE pandeo 184 Sanar o AAS Po mE ener earn ener ee sere ene et ene errr rere ererenn terrae 184 Dat Plo Pe MeO esa pi tee anes 184 da suit CEE o e in EE E 185 Costicientor Thermal Expansion osa anotaron ope nipona poi 186 dle ratio hala a OOOO o Ue
90. an illuminated LED indicates proper operation ARES User Manual FRI BENDIX SPRING 15 15y pr HOTCRON SLAVE STEPPER BD SLAVE TEMP 1 BD A D FUNC GEN 2 BD LS MOTOR E Blinks at 1Hz On when link to Host Computer is active All other LEDs are 15V 15V PHASE LOCK 5V 0000 INDUCTOSYN amp O000 0000 Figure 6 1 Location of Diagnostic LEDs ARES User Manual Troubleshooting Guide Table 6 1 and Table 6 2 list some problems that may arise during instrument calibration and operation and offers the corresponding corrective actions Each corrective action is listed by number Each action constitutes a single troubleshooting operation For example first try corrective action 1 If the problem persists try 2 and so on until you reach Call Technical Service Before calling technical service have the following information ready e The instrument model and serial number e The software version you are running e Any troubleshooting steps you followed to diagnose the problem Calibration Table 6 1 Calibration Troubleshooting Guide PROBLEM CORRECTIVE ACTIONS NORMAL FORCE CALIBRATION During either Torque or Normal Force 1 Exit the calibration operation and enter the Calibration the first value of force that is TRANSDUCER SETUP UTILITIES SERVICE displayed is either very high such as 1E 5 or TRANSDUCER The TORQUE or NORMAL exactly zero CALIBRATION
91. and lower frequency limits of the sweep Logarithmic frequency sweeps can be run in ascending or descending order They can begin or end at any frequency from 1x10e to 80 Hz with a maximum of 500 data points measured during each decade of frequency Frequencies are selected by specifying initial and final frequencies and the number of data points to measure between each decade of frequency points per decade The number of points per decade includes the initial frequency but excludes the final frequency As an example consider a sweep conducted over a single decade of frequency between 10 and 100 radians per second Selecting five data points to be measured per decade divides the difference of the endpoint logarithms into five equally spaced fractional exponents so that six discrete frequencies are generated e Initial Frequency 10 rad sec e Decade Frequencies 15 9 25 1 39 8 63 1 rad sec e Final Frequency 100 rad sec One data point is measured at each of the frequencies Linear Frequency Sweep The linear frequency sweep uses the entered frequency limits The test starts at the initial frequency and continues until the final frequency is reached adding the frequency increment to each subsequent frequency if the final frequency is greater than the initial value or subtracting the increment if the final frequency is less than the initial value As an example a linear sweep from 10 to 50 rad sec in increments of 10 rad sec g
92. aneously That is the collar should be tightened a small amount then the screws started then the collar some more to ensure that all components are aligned and mating properly If at any time a part does not seem to fit well or tighten easily stop and ascertain the reason for the problem Do not force anything ARES User Manual 6 Tighten the Peltier Assembly Collar by placing the two pins on the spanner wrench provided into two of the holes machined into the Collar and rotating the wrench clockwise until the Collar is snug do not overtighten 7 Tighten the three screws in the Peltier Assembly Shaft using the supplied 5 5 mm open end wrench do not overtighten ame WE a PELTIER or BATH HOUSING CROSS SECTION SHOWN FOR VISIBILITY Figure 2 30 Peltier Alignment Pin Circulator Connections Connect the Circulator hoses to the Peltier Assembly as follows Fluid Output from Circulator Lower Hose of Peltier Assembly Fluid Input to Circulator Upper Hose of Peltier Assembly The circulator should be positioned on the floor below the work area Make sure all hoses are installed completely onto their respective hose barbs and that the hose clamps are tight Filling the Circulator Regardless of the type of circulator used we recommend that the fluid used be a mixture of 50 water and 50 ethylene glycol Use of pure water or any other mixture will ultimately result in damage to the Peltier Assembly specifically
93. ansducer using the various test tools described in Chapter 4 CAUTION Force Rebalance Transducers contain a precision air bearing that is equipped with a bearing lock which prevents movement of the air bearing when no air is applied To avoid damaging your transducer familiarize yourself with the operation of the bearing lock see the next topic and observe the following cautions Do not apply power to the instrument when the bearing is locked Do not unlock the bearing unless air is applied to the transducer If the air supply must be intentionally interrupted turn off instrument power and lock the bearing prior to removing air If the air supply is interrupted while the bearing is unlocked do not touch the anvil until air is restored Maintain air flow to the transducer at all times to prevent contamination of the air bearing Failure to observe these cautions will result in damage to the transducer Stage The stage Figure 2 2 is a motorized platform that supports the transducer The stage can be raised and lowered to facilitate sample loading using either the manual stage control buttons on the right side of the test station or through Orchestrator software control The rate at which the stage moves can be adjusted through software Manual Stage Control The Manual Stage Control uses 3 push button actuators located on the lower right side panel of the Test Station Figure 2 2 It allows movement of the stage during op
94. anvil and insert the tool into the anvil pulling apart the retainers if necessary Hand tighten the knob do not over torque Lower Tool Installation Fluid Bath Mount To install a lower tool into either of the Fluids Baths please refer to Chapter 2 for specific installation instructions For either bath the correct lower PRT should be inserted first followed by the tool ARES User Manual RETAINERS _ KNOB UPPER FIXTURE NX 1 HOLD FIXTURE HERE WHILE INSTALLING OR REMOVING RETAINER ANVIL a KNOB FIXTURE 2 PUSH FIXTURE FULLY UPWARD INTO ANVIL AND HOLD FIXTURE IN PLACE 3 TIGHTEN THE KNOB 4 FIXTURE INSTALLED Figure 4 1 Upper Tool Installation ARES User Manual 155 LOWER FIXTURE TOOL PRT Sareea ee e id Ce Va ALIGNMENT KEY KNOB Figure 4 2 Lower Tool Installation Motor Mount ARES User Manual Setting the Gap Zeroing the gap between upper and lower test tools is a prerequisite to setting the gap during sample loading Zeroing the gap requires lowering the stage until the upper and lower tools touch then setting the GAP value to read zero millimeters After that moving the stage results in an accurate gap indication as displayed by the GAP value The following procedures are general for all test tools Specific details regarding each tool are described under that tool s individual section Two methods are available for zeroing and setti
95. as expressly set forth in this LICENSE 3 OTHER RESTRICTIONS This LICENSE is your proof of license to exercise the rights granted herein and must be retained by you The following also apply to the software described above as covered by this LICENSE a You may not rent or lease this software but you may transfer your rights under this LICENSE on a permanent basis provided you transfer this LICENSE this software security key s and all accompanying written materials and retain no copies and the recipient agrees to the terms of this LICENSE Any transfer of this software must include the most recent update and all prior versions continued ARES User Manual b You may not reverse engineer decompile or disassemble this software except and only to the extent that such activity is expressly permitted by applicable law notwithstanding this limitation c This software is licensed as a single product and its component parts may not be separated for use on more than one computer d Without prejudice to any other rights TA Instruments may terminate this agreement if you fail to comply with the terms and conditions of this agreement In such event you must destroy all copies of this software and all of its component parts 4 NOWARRANTY The software described above and documentation are provided on an as is basis and all risk is with you TA Instruments makes no warranties express implied or statutory as to any matter whatsoeve
96. ated by a viscoelastic material can be separated into two components an elastic stress T that is in phase with strain and a viscous stress T that is in phase with the strain rate AY dt but 90 out of phase with strain The elastic and viscous stresses are sometimes referred to as the in phase and out of phase stresses respectively The elastic stress is a measure of the degree to which the material behaves as an elastic solid The viscous stress is a measure of the degree to which the material behaves as an ideal fluid By separating the stress into these components both strain amplitude and strain rate dependence of a material can be simultaneously measured The viscous and elastic stresses can be related to material properties through the ratio of stress to strain or modulus Thus the ratio of the elastic stress to strain is referred to as the elastic or storage modulus G which represents the ability of a material to store energy elastically The ratio of viscous stress to strain is referred to as the viscous or loss modulus G and is the measure of a material s ability to dissipate energy The complex modulus G is a measure of the overall resistance of a material to deformation If these measurements are made using a linear geometry instead of a shear geometry then the letter E is used to represent the modulus instead of G ARES User Manual In some cases it is useful to define the ratio of sample strai
97. ations Table 1 9 Specifications Force Rebalance Transducers 2K FRTN1 and 2K FRTN1E TORQUE Measurement Range High Range 2 to 2000 gecm Low Range 0 02 to 200 gecm 500 rad sec version V8 x and above Maximum Operating Frequency 100 rad sec older than V8 x Measurement Range 2 to 2000 gmf Table 1 10 Specifications Force Rebalance Transducer 1K FRTN1 Jp TORQUE SPECIFICATION Measurement Range High Range 1 to 1000 gecm Low Range 0 002 to 20 gecm 200 rad sec versionV8 x and above Maximum Operating Frequency 100 rad sec older than V8 x NORMAL FORCE SPECIFICATION Measurement Range 2 to 2000 gmf Table 1 11 Specifications Force Rebalance Transducers 100 FRTN1 and 200 FRTN1 SPECIFICATION 100 FRTN1 SPECIFICATION 200 FRTN1 Measurement Range High Range 0 04 to 100 gecm High Range 0 08 to 200 gecm Low Range 0 004 to 10 gecm Low Range 0 008 to 20 gecm ml perang 100 rad sec 16 Hz Frequency SPECIFICATION 100 FRTN1 AND 200 FRTN1 Measurement Range 0 1 to 100 gmf ARES User Manual Table 1 12 Specifications Force Rebalance Transducers 100 FRT and 200 FRT TORQUE SPECIFICATION 100 FRT SPECIFICATION 200 FRT Measurement Range High Range 0 02 to 100 gecm High Range 0 04 to 200 gecm Low Range 0 002 to 10 gecm Low Range 0 004 to 20 gecm Maximum Operating Frequency 100 rad sec 16 Hz Not Used for Measurement Table 1 13 Specifications Standard Transducers 2K STD and 10K STD SPECIFICATION 2K ST
98. be used for very thin samples with the stipulation that an identical number of equally sized shims must be used on either side of the sample NOTE Loading soft samples or samples that do not properly fit the inserts can result in inaccurate data Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using the torsion rectangular geometry The following geometry specific factors affect the operating range of torsion rectangular geometry e Thickness of sample stress constant K and strain constant K e Width of sample stress constant K and strain constant K e Length of sample strain constant K Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type using the torsion rectangular geometry use the following equation x K where K Stress Constant K Strain Constant and C is computed from the following ARES User Manual 185 C for G MAXIMUM C for G MINIMUM 2K FRTN1 2K FRIN1E This transducer is not generally recommended 4K FRTN1 for use with this tool However it may be used for some limited applications 2K STD B 10K STD A J 2 60e 06 r see n
99. bly is used to sense axial force Environmental Control Options This instrument can be configured to subject samples to various thermal environments These options are a Forced Convection oven a re circulating fluid bath or a Peltier system See Chapter 2 for details ARES User Manual HOST COMPUTER kk RS 2320 TRANSDUCER SUBSYSTEM TORQUE RESPONSE I I l I I ETTE TRANSDUCER A ss SIGNAL TORQUE eae oe CONDITIONER CPU AND RAM eee m FUNCTION MOTOR GENERATOR CONTROLLER TEMP CONTROLLER ee A ee ee ee ee ee ee ee A A ee ee ii TEMP CMD TOOL TEMPERATURE AND MEASURE eee eee i i TEMP CONTROL gt A ooann nnn i ee ance ENVIRONMENTAL CONTROLLER e ARES I scan e TEST STATION TEMP ae CONTROLLER Mee TERT UN a from CPU BOARD TEMP CMD AND CIRCULATOR MEASURE TEMP CONTROL ANG FEEDBACK PELTIER OPTION TOOL TEMPERATURE FLUID BATH OPTION Figure 1 1 ARES Functional Block Diagram ARES User Manual Principles of Operation Figure 1 1 is a simplified block diagram of the ARES The following discussion offers a brief explanation of ARES operation using Figure 1 1 for reference In Figure 1 1 terminology printed in upper case refers to the various components or subsystems and the signals generated by the system are printed in italics The ARES consists of the following subsystems e Contro
100. ceptacle Do not use excessive force if resistance is encountered while lowering as this may damage the PRT Plug and Receptacle In this case raise the Peltier Assembly check the alignment described in the next step and try again ARES User Manual UPPER HOSE FLOW my COVER RAISED POSITION SHAFT SCREWS 3 at serio COLLAR p i LOWER HOSE q FLOW PRT PLUG Oq RED DOT VIEW FACING FRONT OF INSTRUMENT Figure 2 29 ARES Peltier Assembly 5 Slowly lower the Peltier Assembly onto the ARES Motor Housing ensuring that e The three screws in the Peltier Assembly Shaft align with the three threaded holes machined into the ARES motor anvil e The Pin Figure 2 30 machined into the bottom of the Peltier Assembly is seated into the notch in the ARES Motor Housing the Pin and notch should be located toward the rear of the instrument It may be necessary to rotate the Peltier Assembly back and forth until the Pin falls into the notch e The threaded Collar of the Peltier Assembly rests in the threaded portion of the ARES Motor Housing e Ensure that the spring Figure 2 29 is positioned behind the Anvil Tightening Knob on the ARES Motor Rotate the Motor Anvil to gain access to the Anvil tightening knob then tighten the knob a flat head screwdriver may be used if you do not overtighten While the next steps are listed sequentially they should be performed more or less simult
101. chined into the Collar and rotating the wrench clockwise Do not overtighten the Collar 2 Tighten the three screws in the Shaft using the supplied 5 5 mm open end wrench Again do not overtighten the screws VIEW FACING FRONT OF INSTRUMENT UPPER HOSE FLOW ml COVER RAISED POSITION SHAFT SCREWS 3 COLLAR E LOWER HOSE T Figure 2 21 Fluid Bath 2 Lower Portion Details 68 ARES User Manual LOWER FIXTURE LOWER FIXTURE WRENCH Fixture Removal Only BATH WRENCH Lower Fixture Removal Only COVER RAISED POSITION THREADED COLLAR SPANNER WRENCH UPPER HOSE FLOW OUT LOWER HOSE FLOW IN THREADED COLLAR a Y a Ps MOTOR COVER a MOTOR ANVIL KNOB Figure 2 22 Fluid Bath 2 Components and Installation ARES User Manual Circulator Connections Connect the circulator to the bath using the supplied connectors The lower hose on the bath is for flow into the bath out of the circulator and the upper hose is for flow out of the bath Figure 2 21 The circulator should be positioned on the floor below the work area Make sure all hoses are installed completely onto their respective hose barbs and that the hose clamps are tight Connect cable 707 00750 between the Circulator RS 232 connector and the Test Station Signal Panel CIRCULATOR connector PRT Installation There are two PRIs available Figure 2 24 each designed to be used with a specific lower too
102. ck the Transducer and Motor bearings Remove Air supply to instrument Po ES ARES User Manual 227 Inspect the air hoses for cracks and other damage that could result in leaks especially in the vicinity of the bend radii If any damage is found notify TA Instruments for service There are also internal filters inside the test station that should be inspected and serviced on an approximately 6 month to 1 year basis Only qualified service personal should perform this maintenance If no leaks are found apply AC power to the instrument as follows 1 Establish airflow through the air dryer but do not connect the air output to the test station Allow the air to purge for 3 to 5 minutes Connect the air supply to the test station Unlock the transducer and motor bearings Install the POWER IN plug in the AC main line voltage source Push the Main Power Switch to the ON I position a ly Verify that the air pressure to the motor transducer and oven are correct Note to check the oven air pressure the oven must be all the way to the right and closed Air Dryer Inspect and service the air dryer according to its manual This should include draining and cleaning the pre filters Replace them if necessary Cleaning the Instrument If the exterior plastic or metallic surfaces of the instrument require cleaning use only a solution consisting of a non abrasive household dish detergent and water Clean as follows 1 Remove
103. complex viscosity N Y axis versus frequency X axis The region between the upper and lower limits of operation is the range of complex viscosity that can be tested ARES User Manual 167 COVER UPPER COVER CLIP TOOL SEALING FLUID WELL UPPER PLATE GLASS CHAMBER SAMPLE OVERFLOW LOWER WELL PLATE O RING LOWER TOOL Figure 4 5 Hastelloy Tool Liquid Seal The upper tool is designed with a liquid seal The upper plate has a well machined in it that holds the sealing fluid When the upper cover is slid into place on top of the glass chamber a lip on the under surface of the cover extends into the fluid completing the seal Figure 4 6 The bottom of the glass chamber is sealed with a special O ring During use the lower tool glass chamber and cover move as one piece effectively one large lower tool The liquid provides a good seal without the drag associated with conventional seals To ensure optimal performance the sealing fluid should be of low viscosity The sealing fluid should also be chemically appropriate for the sample material to avoid any dangerous reactions or interactions between the sample and sealing fluid For the best and most consistent results the volume of sealing fluid should be kept constant for each sample run Some experimentation may be necessary to determine the optimal fluid volume for a particular tool gap and sample A pipette or other accurate fluid delivery system should be u
104. concerning the operation of Orchestrator software see the Orchestrator Online Help Description of Instrument The Advanced Rheometric Expansion System ARES is a mechanical spectrometer that is capable of subjecting a sample to either a dynamic sinusoidal or steady shear strain deformation and then measuring the resultant torque expended by the sample in response to this shear strain Shear strain is applied by the motor torque is measured by the transducer Strain amplitude and frequency are set by the operator with the actual sample deformation determined by the measured motor and transducer displacement Motors There are 3 basic motors available for use in ARES The High Resolution HR motor is a ball bearing direct drive motor It provides very precise and accurate motion in both dynamic and steady modes The applied strain is essentially instantaneous The High Torque HT motor is similar to the HR Motor but is designed to deliver much higher torque The HT motor is intended for use in conjunction with the 10K STD transducer The Low Shear LS is most commonly used for fluids testing The motor shaft is supported axially by a precision air bearing This minimizes axial runout providing the smoothest normal force data It also has a special controller that allows extremely low shear rates to be applied during steady shear tests ARES User Manual Motor Modes In Dynamic Mode the motion is oscillatory The mot
105. ctive zone The Ramp Rate is the Rate of thermal change that the sample material undergoes during the test Orchestrator reports the difference between the Initial Temperature and Final Temperature setpoints divided by the Ramp Rate that you specified as the computed Ramp time Ramp direction is set using the Initial and Final Temperatures in a zone The Ramp Rate is in units of C per minute C min and the entry field accepts any value within the range of the instrument with a display resolution of 0 1 C If temperature control is not needed and the deformation is the only desired change the Ramp Rate should be set to O C min A Ramp Rate of 0 C min makes the test a time sweep hence this test is sometimes referred to as a time cure sweep Following the Ramp the Soak Time After Ramp is the time period during which temperature is held at the Final Temperature Orchestrator reports the total time required to run the test including all zones and soak times as the Computed Test Duration Steady Step Hate Temperature Ramp Test Ea Ed Initial Temp 25 0 PC Ma 500 0 Min 150 0 sampling Mode Log Linear Points Per Zone 200 Max 350 Min 20 Shear Rate Limits 1 s Max 400 5737 Min 0 004005 Zone Number 1 2 3 4 Final Temp cono Poo foo foo fo Ramp Rate oe PCAmin yao lao ooo po 8 foo Computed Ramp Time ms 230 pza Soak Time After Ramp s okma fo Mo fo O Mero Poo no foo o Computed Test
106. d Orly Li Instrument Control Panel Showing Fluid Bath Control Options Peltier Description The Peltier environmental control system utilizes a solid state heat pump thermopile to control the temperature of the lower tool which is an integral part of the Peltier Assembly In general the solid state heat pump consists of multiple semiconductor devices in series alternating P type and N type The devices are placed between the lower tool and a heat sink Figure 2 28 e ELECTRICAL INSULATOR HEAT CONDUCTOR gt a ELECTRICAL CONDUCTOR N N TYPE SEMICONDUCTOR P P TYPE SEMICONDUCTOR Figure 2 28 Solid State Heat Pump Peltier Element Schematic DC voltage is applied across the semiconductors to either heat or cool the lower tool depending on the polarity of the voltage The semiconductors transfer thermal energy between the lower tool and the heat sink which is essentially a heat exchanger through which fluid typically water is circulated The fluid temperature determines the amount of thermal energy that the heat sink can source to or sink from the lower tool The fluid temperature thereby modifies the actual operational temperature range within the overall System Specifications Table 2 8 Table 2 8 Peltier System Specifications 30 C to 150 C depending on circulator fluid temperature 30 C per minute from 0 C to 100 C at 20 C circulator fluid temperature 0 1
107. d appears at the top seam between the bath cup and body Figure 2 35 the clamp should be tightened immediately Filling the Circulator Depending on the type of circulator in use and the desired operating range of the circulator fill the circulator with fluid as specified in Table 2 10 Refer to your Bath documentation for specific circulator filling and operating guidelines as well as other bath fluid options for your application Also refer to the bath fluid MSD for guidelines regarding the safe handling of your particular bath fluid Table 2 10 Circulator Operating Ranges Using Various Bath Fluids Desired Operating Range of Circulator Fluid bath temperature range is slightly less 20 C to 30 C 100 Dow Corning Syltherm XLT 1 C to 99 C 100 water 5 C to 100 C 50 ethylene glycol 50 water 20 C to 150 C Julabo Thermal H10S 40 C to 110 C 100 ethylene glycol ARES User Manual LABEL ACCESS PORT BATH OUTLET Q EN N Figure 2 37 Fluid Bath Fluid Connections ARES User Manual Fluid Bath Configuration in Orchestrator When you command a temperature the Orchestrator software uses the Instrument Configuration to determine the environmental system currently in use and establish operating conditions Prior to operating the fluid bath access the Instrument Configuration function located under the Service function of the Utilities menu and set up the instrument using the guidelines
108. d temperature When the Peltier system is used temperature control and monitoring is accomplished through the lower tool PRT connector TOOL TEMPERATURE and special electronics in the ARES Test Station ARES User Manual Specifications Table 1 1 Physical Specifications Chassis Width Depth Height Weight Test Station 26 in 21 in 36 in 275 lbs LN Controller 11 in 9 5 in 22 in 38 lbs Mechanical Chiller 29 in 20 in 46 in 260 lbs Fluid Bath Circulator 12 in 17 in 295 in 74 lb Table 1 2 Test Station Operating Specifications Operating Parameter Specification 180 to 264 VAC 20 A 50 60 Hz single phase Transient Over Voltages Installation over voltage category II Temperature Range Ambient 5 to 40 C Relative Humidity 80 up to 35 C then decreasing linearly to 50 at 40 C ARES User Manual Table 1 3 Pneumatic Ratings AIR INLET RATINGS AIR PRESSURE FLOW AIR QUALITY Instrument quality air having the with Oven following characteristics 5 5 scfm 156 l min e Any particles present in the air Instrument 80 psi 5 5 bar must be smaller than 5 microns in without Oven diameter 3 scfm 85 l min e Relative humidity 35 to 70 Dewpoint 10 C with Oven 7 5 scfm 213 l min mea Air Dryer 100 psi 6 8 bar without Oven 5 scfm 142 l min Table 1 4 Accessories Power Specifications NOMINAL RATED COMPONENT VOLTAGE CURRENT AND FREQUENCY USA Fluid Bath Circulator 115 VAC
109. d valve to control liquid nitrogen flow into the Dewar and hardware to control the boiling of the liquid nitrogen to produce very cold nitrogen gas within the flask A second solenoid valve regulates the flow of the cold nitrogen gas out of the Dewar flask for use by the Test Station Dewar Flask A Dewar flask is a container specifically designed to efficiently store liquid nitrogen Dewar flasks help prevent evaporation due to their double wall construction Within the Dewar flask a heater immersed in the LN provides controlled boiling The Dewar is equipped with a pressure relief valve to prevent damage to the system It is common for the relief valve to open loud pop several minutes after the LN2 controller is shut off as the residual liquid nitrogen in the Dewar evaporates to gas Connection The LN2 output connects to the Forced Convection Oven Connect the signal cable from the LN2 controller to the LN2 port on the Signal Panel Figure 2 12 All connections to the ARES are normally made during system installation by a TA service technician Connect the LN2 controller filler hose to your liquid nitrogen source The external liquid nitrogen tank should have a low pressure lt 30 psi valve The hose between the nitrogen tank and the LN2 controller should be kept as short as possible to maximize the LN2 controller performance Software Configuration The LN2 operates using Orchestrator software Chapter 2 discusses the set up and operatio
110. description of the AutoTension parameters that must be set in the AutoTension Adjustment Set Up Screen Fig 3 26 AutoTension Direction When Tension is selected tensile static force is applied When Compression is selected compressive static force is applied Initial Static Force This is defined as the static force that is maintained throughout the test AutoTension Sensitivity Minimum change in normal force that results in an adjustment to maintain the Initial Static Force Switch AutoTension to Programmed Extension When Sample Modulus When sample modulus decreases below the value entered in this field the last valid coefficient of thermal expansion 0 of the sample is used to determine an AutoTension static force that best maintains the sample length The coefficient of thermal expansion 01 is given by AL am AT where AL change in sample length L sample length AT change in sample temperature This feature is useful when running temperature sweeps to prevent excess sample stretching with increasing temperature It is important to apply this adjustment when sampling through the glass transition point where there will be a significant rapid drop in G Without this adjustment the now softer sample beyond the glass transition point would rapidly stretch and ultimately be pulled part A test run may be necessary to determine where the glass transition point occurs before setting this value 142 ARES User Manua
111. ducer WARNING Do not attempt to lift or carry the Test Station alone Attempting to lift or carry the Test Station can result in serious personal injury or damage to the Test Station CAUTION Never place any lower tool into the bath if the temperature of the lower tool is cooler than that of the bath Placing a tool into a warmer bath will result in expansion of the tool during use After expansion the tool may not be removable without damaging your bath We suggest that you partially insert the tool by placing a phenolic spacer between the upper lip of the lower tool and the surface of the bath Allow the lower tool temperature to match that of the bath then remove the spacer and fully insert the lower tool WARNING Fuses must be changed by a qualified electronic technician only WARNING Prior to changing a fuse ensure that AC power to the Test Station is OFF Changing a fuse on a live electrical circuit can cause serious personal injury or death WARNING For continued protection against fire hazard replace only with a fuse of the same type and rating WARNING The following procedure must be performed only by a qualified electronic technician WARNING Ensure that AC power to the Test Station is OFF before attempting the following procedure see step a Changing a fuse ona live electrical circuit can cause serious personal injury or death WARNING The Main Power Switch does not remove power to the oven or L
112. ducer in use from the loop in the line c Ensure that the weight s is are free to hang without obstruction and that the weight is steady not swinging from side to side Select the Torque Cal button The Torque Calibration form is displayed Enter the Calibration Torque specified in Table 5 3 depending on the transducer in use Select the Calibrate Now button When calibration is complete the Transducer Calibration form is again displayed ARES User Manual Transducer Calibration Figure 5 4 Transducer Calibration Form Figure 5 5 Applying Torque Using the Calibration Weight ARES User Manual 213 15 Verify that the Torque value displayed on the Transducer Calibration Form Figure 5 4 is within the limits for the TORQUE VALUE shown in Table 5 3 depending on the transducer in use Verify that the Current Torque Cal value displayed in the Transducer Calibration Form is within the limits for the CALIBRATED FULL SCALE VALUE shown in Table 5 3 If the Torque values are not within the specified limits contact TA Instruments Service 16 Select the Accept button Control returns to the Transducer Characteristics form 17 Verify that the Torque Calibration Value displayed in the form the high range value if the transducer is an FRT is the same as the Current Torque Cal value just displayed in the Transducer Calibration form Press Ok 18 If the transducer in use is an FRT perform the following step If the tran
113. dulus Limits for Cone and Plate 2K and 10K Standard Transducer PLATE DIAMETER CONE ANGLE Gx MAXIMUM Gx MINIMUM mm rad dynes cm dynes cm 0 1 9 22E 05 9 59E 01 2K 4 80E 02 10K 1 84E 05 1 92E 01 2K 9 60E 01 10K 3 69E 05 3 84E 01 2K 1 92E 02 10K 0 02 2 31E 04 2 40E 00 2K 1 20E 01 10K 0 04 4 61E 04 4 79E 00 2K 2 40E 01 10K ARES User Manual Appendix Table A1 7 Complex Modulus Limits for Cone and Plate FRTN1 Transducer PLATE DIAMETER CONE ANGLE G Maximum dynes cm Gx MINIMUM mm rad at Frequency rad sec dynes cm 9 22E 04 9 22E 05 4 79E 07 1 84E 04 1 84E 05 9 59E 06 3 69E 04 3 69E 05 1 92E 07 wm 100 w 10 w lt 10 100 w 10 w lt 10 100 w 10 w lt 10 2 31E 03 w 2 31E 04 w 1 20E 06 4 61E 03 w 4 61E 04 w 2 40E 06 1 92E 00 High range 100 FRTN1 3 84E 00 High range 200 FRTN1 1 92E 01 Low range 100 FRTN1 3 84E 01 Low range 200 FRTN1 3 84E 01 High range 100 FRTN1 7 68E 01 High range 200 FRTN1 3 84E 02 Low range 100 FRTN1 7 68E 02 Low range 200 FRTN1 7 67E 01 High range 100 FRTN1 1 53E 00 High range 200 FRTN1 7 67E 02 Low range 100 FRTN1 1 53E 01 Low range 200 FRTN1 4 79E 02 High range 100 FRTN1 9 58E 02 High range 200 FRTN1 4 79E 03 Low range 100 FRTN1 9 58E 03 Low range 200 FRTN1 9 59E 02 High range 100 FRTN1 1 92E 01 High range 200 FRTN1 9 59E 03 Low range 100 F
114. e Tighten the lower and upper collars Raise the stage until a force of approximately 10 of full scale is generated Please note that this tension level is a general recommendation only and you should set the tension level according to the sample characteristics When using the AutoTension feature adjust the stage so that the normal force is Zero Using the Motor Position Offset slider in the Set Gap Instrument Control function in Orchestrator adjust the motor position until the displayed torque is zero DO NOT use the Offset torque to Zero button Read the gap and record this distance as the sample length 2K FRT transducers only Use Hold function under the Control pull down menu when changing temperature ARES User Manual UPPER FIXTURE NON y ya A 4 A Wau 6 05 A SAMPLE ENTER THIS DIMENSION AS INSERT SAMPLE LENGTH ONE EACH UPPER AND LOWER COLLAR S ONE EACH UPPER AND LOWER v E l N 4 N F A a STOP PIN LOWER FIXTURE Figure 4 12 Torsion Rectangular with Sample Loaded ARES User Manual Couette Strain Constant Stress Constant 1000 G on L Rg MOTOR MOUNT Variables ambient testing Ge Gravitational constant 980 7 cgs or 98 07 Sl L Length of bob mm Rp Radius of bob mm Rc Radius of cup mm Options 25 mm bob 27 mm cup ambient testing only 32 mm bob 34mm cup for fluid bath or fluid bath 2 1
115. e PID loop settings Figure 2 32 affect how the Peltier settles at a set point temperature As the Peltier reaches a setpoint there will typically be a few degrees of overshoot after which the temperature will oscillate a few times and then stabilize The Peltier will typically reach stabilization within a few minutes By modifying the Proportional Band P coefficient less overshoot can be achieved but there will typically be more oscillations before the bath stabilizes so the overall stabilization time will be longer PID Setup Form ki Ei PID Temperature Control Setup Peltier Proportional Band 2 5 4 peset o ae i 0 87 Reps Mmin cle eae 0 01 F Miri Ok Help Cancel Figure 2 32 PID Setup Form Showing Peltier Settings Table 2 9 Default PID Loop Values for Various ARES Firmware Versions PID Loo Version 4 Version 5 and 6 P Firmware Firmware Proportional 5 2 5 Band Reset 10 67reps min 10 67reps min Ras osm CI ARES User Manual Peltier Operating Requirements The Peltier can operate only if the following conditions are met e The Peltier is selected as the current environmental system e The environmental system is turned ON in the Instrument Control Panel e Fluid must be flowing through the Peltier pumped through it At all times while operating the Peltier system ensure that the circulator is connected to the Peltier Assembly and the circulator pump is ON Failure to heed this warning w
116. e Shaft with the flat portion of the ARES Motor Anvil both flats should be facing toward the right as you face the instrument 5 Slowly lower the Bath onto the ARES Motor Housing ensuring that e The three screws in the Shaft align with the three threaded holes machined into the ARES motor anvil e The Pin Figure 2 23 machined into the bottom of the Fluid Bath is seated into the notch in the ARES Motor Housing the Pin and notch should be located toward the rear of the instrument It may be necessary to rotate the bath back and forth until the Pin falls into the notch e The Threaded Collar of the Fluid Bath rests in the threaded portion of the ARES Motor Housing e Ensure that the Spring Figure 2 21 is positioned behind the Anvil Tightening Knob on the ARES Motor Rotate the Motor Anvil to gain access to the Anvil tightening knob then tighten the knob A flat head screwdriver may be used if you do not overtighten While the next steps are listed sequentially they should be in practice performed more or less simultaneously That is the collar should be tightened a small amount then screws started then the collar some more to ensure that all components are aligned and mating properly If at any time a part does not seem to fit well or tighten easily stop and ascertain the reason for the problem Do not force anything 1 Tighten the Threaded Collar by placing the two pins on the spanner wrench provided into two of the holes ma
117. e optional LN2 controller operation to 150 C or the mechanical air Chiller operation to 60 C can be used to extend the operational range of the oven The air convection oven is recommended for polymer melts and solids and can accommodate Cone and Plate Parallel Plate Torsion Rectangular and Torsion Cylindrical geometries The recirculating Fluid Bath 2 or original Fluid Bath is appropriate for liquid samples that may evaporate under the influence of circulating air The temperature range of the bath is approximately 20 to 140 C depending upon the Circulator and bath fluid used and can be used with Parallel Plates Cone and Plate Couette and Double Wall Couette geometries Our patented rotating oscillating Peltier system has a temperature range of 30 to 150 C with heating rates as high as 30 C min The Peltier system can be used with Cone and Plate or Parallel Plate geometries Refer to the following sections for information regarding each specific environmental option OVEN OPTION FLUID BATH OPTION ARES User Manual Oven The oven is a forced air convection environmental chamber that encloses the sample Mounted in the oven are two resistive heaters gun heaters that are used to control the temperature of the gas that is input to them During testing at or above ambient temperature either air or nitrogen gas can be input to the heaters If test temperatures must be extended to below ambient the input to t
118. e or negative that the sample material undergoes during the test Ramp direction is set using the starting and final temperatures in a zone The ramp rate is in units of degrees minute The entry field accepts any positive value for ramping rate The actual maximum ramping rate that can be accurately maintained is a function of the size and thermal properties of the sample If temperature control is not needed and strain or sampling rate is the only desired change the ramp rate should be set to 0 C min Time Per Measurement Time Per Measurement establishes the sampling rate When entering this value consider the time per measurement cannot be shorter than the physical time required to make a dynamic measurement If the time entered is less than physical time required to make a dynamic measurement the instrument will sample as fast as it can ARES User Manual 109 Strain Strain can be set to any value within the range of the instrument as shown in the boundary window but should not exceed the linear viscoelastic region of the sample material If a value of zero is entered then this zone inherits the strain level from the previous zone Note also that this value can be overridden if the AutoStrain function is being used Soak Time After Ramp Following the Ramp the time period during which temperature is held at the Final Temperature before proceeding to the next zone Dynamic Temperature Ramp Test Ei Ed Frequency f 0 0 rad s Max
119. e regulator if necessary to achieve 60 psi by turning the knob clockwise to decrease the pressure and counterclockwise to increase pressure During extended use parts of the Chiller may freeze inside blocking gas flow To help prevent damage to the gun heaters due to insufficient gas flow the Chiller is equipped with an emergency shut off that will shut down the compressor and turn off the heaters if the airflow through the Chiller drops If this happens turn off the Chiller and allow it to thaw before continuing Freezing will generally happen if the dew point of the input gas is greater than 80 C The air dryer is designed to provide dry gas with a dew point sufficient to prevent freezing The Chiller should be turned off when it is not actually in use and the air dryers should be properly maintained and inspected Maintenance There are no user serviceable parts inside the refrigeration unit The compressor and condenser are lifetime lubricated and do not require oiling The condenser fins and grill should be kept clean to ensure good airflow Clean them as needed by vacuuming or blowing with compressed air The air filters should be inspected and cleaned as necessary Also any moisture should be drained from the filter housings regularly Refer to the air dryer air filter and refrigeration unit documentation that came with the Chiller for further maintenance information The balance pressure should also be periodically monitored as d
120. e values result in counterclockwise rotation In each zone the data can be sampled at a logarithmic or linear interval Figure 3 23 Logarithmic sampling takes data at logarithmically incremented intervals resulting in equally spaced data points when plotted as a function of logarithmically scaled time the number of points taken is inversely proportional to zone time Linear sampling takes data at linearly incremented intervals resulting in equally spaced data points when plotted as a function of linearly scaled time This technique is useful for relatively short zone times where linear time scaling is practical The estimated viscosity value is used to modify the gain term in the closed loop control algorithm which adjusts the motor s rotational rate to generate the desired stress level Stress Ramp Test ki E3 Temperature 25 0 PC Max 600 0 C Min 150 0 sampling Mode Log Linear Paints Per Zone 200 Max 250 Min 20 Stress Limits Pa Max tb3929 42 Min 6 392942 Estimated Viscosity i coon Pers one Number 1 2 3 4 Final Stress Palfiooo foo foo foo Zone Time s or homes 300 a COM CI Options La omis ndortest_ Saveds tee coce Figure 3 23 Stress Ramp Test Set Up Screen suggested Use Stress Ramp is used to determine material hysteresis by deforming the material by linearly accelerating or decelerating the shear stress command The test is similar to the thixo
121. ed ooo f No ves Help Cancel Figure 4 3 Instrument Configuration Function Instrument Options Set the Stepper or Linear Motor and Remote Gap Monitoring options to yes to enable the Gap Control Panel functions ARES User Manual 159 Test Tool Installation and Sample Loading General Guidelines The next several sections contain specific procedures to install the test tools used in each geometry Specific sample loading guidelines are given for each tool However the following general sample loading guidelines pertain to all tools e Make sure the tools are clean and free from damage e Install the tools correctly as described In general the tools should be easy to install Having to use undue force is a sign that something is wrong Stop and ascertain the problem before continuing e Make sure the tools align with each other properly and that the Gap is properly zeroed e When using the oven close the oven door carefully to ensure that the sample or tool does not interfere with the oven door While loading the sample onto the tool ensure that the sample is centered as well as is possible between the tool mounting surfaces Off center loading may cause misalignment of the transducer motor shafts Additionally misalignment may also affect the accuracy of the data If misalignment does occur the sample should be removed from the tool and carefully reloaded When testing at temperatures below ambient temperatu
122. ee errr Torre 6 y en CON UB UO np 8 e o O 10 Kequiea axe iae apoco rat n loo aio 10 ANCL N UIC So dono oro 10 iae Gr enn PA CIS APP In e E E AE E A EAEE ET 13 Resulatory E e E E A ica 14 E T e E E E E A OEE 14 Electromagnetic Compatibility Standards concnicnncnncnnnnnoncnnnnnaninonacanoncannannnonncnconannononnonccnncnonan cr nannc nac nn nan ncncns 14 Technical 16 0 POR paa eer ene eee ree ae 14 Lable alg OIE S reer Me TTT NT Ree A ii cad 15 Ch pler e Ntro dic austin imine anisinn ha arenes 23 AL Y LE POCA O nn o E T IE slg val pda urns cena saad uae gn se ET A ben eo oem canes ners 23 Pesci nonoke N a aos 23 DVN WOM q CA o OE OO EEE mm 23 la APP Cen eee ee ee ee 24 Pii ee a A Teen Over or rene ete E A A nr A ET Tere eer Ree rer oer rrr ttn errr er rrr rt err re 24 Force Rebalance Transducer with Normal Force FRTN1 cee cccesscccesesseeeeeseseeeeeeeaeeeeeseseeeeseeeeeeesaes 24 Standard Transducer STD 2ss ccsapsonacsannsasonssasussonsatand neekin r oran E insi nieki 24 Environmental ControboOpuodns traes titi 24 earar de a aD e E T E E E A E E E 26 CI E p ads 26 Aa 07 a E E E E E E E E E A E E T 26 Tran de e A E E E E E S 26 FE POU aE oo Ea een oe EE A 27 See E O E O O E 28 Motor Tr OL aCe OPECIN aOR S Ns 30 Transducer Operant Speci nea GONS ai 31 Chapter 2 Instrument Components Identification and Operation e seesssesseosseesseessossseeseoessesssessseesesssseesess 33 Component Identification and Place
123. een Test Options The following test options can be selected for use with the temperature ramp Steady PreShear Delay Before Test AutoTension Analog Data Input Measurement Options o Delay Settings o Strain Amplitude Control ARES User Manual Frequency Temperature Sweep Functional Description The Frequency Temperature Sweep takes successive measurements over a range of selected frequencies at a series of constant temperature steps At each temperature step a frequency sweep is run while the temperature is held constant The temperature is then changed to the next step allowed to equilibrate and the frequency sweep is run again In a frequency temperature sweep entry fields for strain value and initial temperature are displayed on the host computer Figure 3 10 You can select either a linear logarithmic or discrete frequency sweep then enter the frequency parameters Thermal step size and soak time are also selectable Frequency Temperature Sweep Test i x Strain 0 1 Maz 1 2 5000 Min 0 003125 Sweep Mode cy Log O Discrete 0 Linear Initial Frequency 0 1 rads Max 500 0 Min 1 00e 05 Final Frequency fi 00 0 rads Points Per Decade 5 Max 500 Initial Temp 25 0 PC Max 600 0 C Min 150 0 Final Temp 35 0 E Temp Increment 2 0 PC Soak Time fi 00 e or him Options PreShear Of Delay Of AutoTens Off Analogin Of Meas
124. enerates frequencies of 10 20 30 40 and 50 rad sec One data point is measured at each of the frequencies Discrete Frequency Sweep The discrete frequency sweep takes a measurement at each of up to ten selected frequencies Discrete frequency sweeps can be run in any order and can begin or end at any frequency within the range of the instrument ARES User Manual 103 Dynamic Frequency Sweep Test Strain Control Figure 3 4 Frequency Sweep Test Set up Screen Suggested Use The frequency sweep is used to analyze frequency and time dependent behavior of samples In general high frequencies correspond to short time scales and low frequencies correspond to long time scales Test Options The following test options can be selected for use with the frequency sweep e Steady PreShear e Delay Before Test e Analog Data Input e AutoStrain Adjustment e Correlation Measurement Options 104 ARES User Manual Dynamic Temperature Step Functional Description The Temperature Step test takes successive measurements at selected temperatures while holding a constant frequency and strain Temperature is automatically incremented or decremented from selected lower and upper temperature limits by user selected steps A unique set of test conditions can be entered in up to four temperature ranges or zones A selected thermal soak time at each temperature ensures temperature equilibrium prior to measurement When setting up a tem
125. ent of TA Instruments Each licensed program shall remain the exclusive property of TA Instruments and no rights or licenses are granted to the purchaser other than as specified above ARES User Manual TA Instruments End User License Agreement This License Agreement is your proof of license Please treat it as valuable property IMPORTANT READ CAREFULLY This is a legal agreement between you either an individual or an entity and TA Instruments for this TA Instruments instrument control and or data analysis software product By breaking the seal on your disk CD ROM package and or installing copying or otherwise using this SOFTWARE you agree to be bound by the terms and conditions of this agreement Failure to comply with the terms of this license terminates the agreement and your rights to use this software TA Instruments Software License 1 GRANT OF LICENSE This TA Instruments End User Software License Agreement LICENSE grants you the following rights a Instrument Control Software This LICENSE permits you to use one copy of the specified version of the TA Instruments instrument control software provided this software is in use on only one computer at any time If you have multiple LICENSES for this software then at any time you may have as many copies of this software in use as you have LICENSES If the anticipated number of users of this software will exceed the number of applicable LICENSES then you must have a reasonable mec
126. ents delivered before January 2002 should have the older locking pin alignment When locking and unlocking the bearings on these instruments the directions described above should be reversed as shown in Figure 2 9 If you are unsure as to which locking orientation your system has the following procedure will help you determine it 1 Turn off the power to instrument Ensure that air is supplied to the transducer 2 Holding the upper tool mount manually try to move the transducer both axially up and down and rotationally 3 Move the bearing lock to the opposite position and try to move the transducer again Note how each orientation feels as you try to move the transducer In the locked position there will be no movement axially or rotationally In the unlocked position you should feel some movement in both directions Make a note in your manual as to the locked and unlocked positions for future reference ARES User Manual F LEFT CLAMP 2K FRTN1 or 2K FRTN1E RIGHT CLAMP __ BALL PLUNGER Factory Set ONE EACH SIDE LOCKED POSITION UNLOCKED POSITION Bearing Lock orientation for ARES SHIPPED BEFORE JANUARY 2002 A po LEFT CLAMP 2K FRTN1 i or ZK FRINIE RRR BERS See MES RIGHT CLAMP E E BALL PLUNGER Factory Set i ee M Oi E ai 5 Pin a Ome Each SIDE i a t UNLOCKED POSITION Bearing Lock orientation for ARES SHIPPED AFTER JANUARY 2002 LOCKED PO
127. er Manual Double Wall Couette Strain Constant Stress Constant 1000 G qe 2 2 27 L R Rs Variables Ge Gravitational constant 980 7 cgs or 98 07 Sl L Length of bob mm R1 R2 R3 R4 equal the following radii BOB gt CUP lt gt Options CUP BOB 34 mm OD 27 95 ID 32 mm OD 29 5 ID Enviromental Systems Fluid Bath Fluid Bath 2 Double Wall Couette Tool see Chapter 2 for more details regarding lower tool General Information The double wall Couette tool is used for testing lower viscosity fluids that would not generate enough torque using parallel plates It is also used where small sample volumes are necessary ARES User Manual 195 Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using the double wall Couette geometry The following geometry specific factors affect the operating range of the double wall Couette e Inner diameter of cup R strain constant K e Outer diameter of cup R strain constant K e Inner diameter of bob R stress constant K and strain constant K e Outer diameter of bob R stress constant K and strain constant K e Length of bob stress constant K_ Additionally the following instrument specific factors affect the operating range of all geometries e M
128. er limits of operation is the range of complex viscosity that can be tested Appendix 1 contains tables of G values for some tool combinations transducers and a standard motor Tool Installation Install a tool as follows 1 Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to raise the stage to the loading position 2 Verify that the motor is on then mount the upper and lower tools on the actuator shafts 3 Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset torque to Zero buttons 4 Using the stepper control buttons lower the stage to a point where the tools are close but not touching 5 Use the Zero Fixture button in the Set Gap Instrument Control function to determine the zero point for the test tools 6 Raise the stage to provide sufficient room for sample loading Gap and Cone Angle The actual gap setting and cone angle for each cone and plate tool is stated on the Certificate of Calibration that is included in the tool kit If no Certificate of Calibration is available contact our Technical Service department ARES User Manual Testing at Other than Ambient Temperatures Use the standard cone and plate tools for isothermal testing only Transitions to elevated temperatures cause expansion of the tool For example with a 50 micron nominal gap settin
129. erations such as sample loading The movement of the stage is defined by the following modes of operation 1 Step When stepped the stage moves very slowly in single steps of the stage motor To step the stage downward press and hold the bottom button To step the stage upward press and hold the top button 2 Slew When slewed the stage moves very quickly and smoothly To slew the stage downward press and hold both center and bottom buttons To slew the stage upward press and hold both center and top buttons ARES User Manual Software Stage Control Movement of the stage can also be controlled from the Set Gap Instrument Control function in the Orchestrator software Click the Set Gap button Figure 2 4 located on the tool bar The Set Gap Instrument Control function can also be opened from the Control pull down menu The Set Gap Instrument Control function has displays that show Torque Normal Force and the current Gap In addition there are several buttons that control instrument features The Send to Top button can be used to move the stage all the way to the top of its motion The Set Gap button can be used to move the stage to the entered commanded gap The force used to move the tools together while setting the gap will not exceed the value entered in the Max Allowed Force box The Zero Fixture button is used to bring the tools together to establish a zero gap reference from which the gap is then set EE Set Gap Inst
130. erative that a mixture of 50 ethylene glycol 50 water be used in the bath Alternatively Julabo Thermal H10S can be used Using pure water is not recommended as it will significantly reduce the lifetime of the seals In the event of a seal failure the bath must be returned to TA Instruments for service and repair Table 2 6 Circulator Operating Ranges using Various Bath Fluids Desired Operating Range of Circulator Fluid bath temperature range is slightly less 5 C to 100 C 50 ethylene glycol 50 water 40 C to 110 C 100 ethylene glycol 20 C to 150 C Julabo Thermal H10S Fluid Bath 2 Configuration in Orchestrator When you command a temperature Orchestrator software uses the Instrument Configuration to determine the environmental system currently in use and establish operating conditions Prior to operating the fluid bath access the Instrument Configuration function located under the Service function of the Utilities menu and set up the instrument using the guidelines shown in Figure 2 25 Setup Instrument Options fx Instrument Testing Limits Intr mem S MUD eeaeee neeaae aeaee etene Temperature Control Temperabure Conto ee Bath Instrument Controlled Only Ma aa fi 50 0 fe MEMO GMa terete eee A 20 0 E Temperature Loop Control Ji pe Temp Calibration Table Default C Adjustable Cancel Figure 2 25 Setup Instrument
131. es in the opposite direction 3 The data are averaged to supply the single data point that is reported by Orchestrator Using two directions per measurement can give more accurate results at low rates ARES User Manual Steady Single Point Test Figure 3 12 Steady Single Point Test Set Up Screen Suggested Uses Steady Single Point can be used to determine the following e Unknown range response limitations of a new sample material e Parameters for the design of new tests e Time required for a sample material to reach steady state at a given shear rate when torque stress signal is manually monitored e g with an external strip chart recorder Options The following test options are available for use with Steady Single Point e Delay Before Test e Analog Data Input ARES User Manual 117 Steady Rate Sweep Functional Description Steady Rate Sweep applies varying magnitudes of steady shear deformation the magnitude of each deformation depending on selected shear rates Figure 3 13 Shear rates can be generated as follows Logarithmic The logarithmic rate sweep commands rates that are logarithmically incremented resulting in equally spaced data points when plotted as a function of logarithmically scaled shear rate in reciprocal seconds 1 s Shear rates are selected by specifying initial and final rates and the number of data points to measure between each decade of rate As an example consider a sweep conducted ove
132. escribed in the Polycold documentation included with your Chiller Upon receiving the instrument you should note and record the pressure reading on the suction gauge This gauge is located on the opposite side of the refrigeration unit as the air dryer air filter and J box The Chiller should be off for 24 hours before taking a balance pressure reading The initial reading should be over 100 psig Subsequent reading should be within 7 psig of the original value If the balance pressure drops more than 7 psig it would indicate a leak in the refrigeration system ARES User Manual 59 NOTE 0 Polycold suction gauge and on off switch are located on this panel l INPUT TO REFRIGERATION UNIT COLD AIR OUT PRESSURE REGULATOR ADJUST TO 60 PSI AIR DRYER AIR INPUT SEPARATOR ah rt AIR FILTERS a ia TO CUSTOMER FURNISHED a AIR FLOW oe Rea CONTROLLER o CONDENSER 1 i ON OFF GRILL SWITCH I I J BOX SIGNAL CONNECTION i to TEST STATION I LN2 CONNECTOR i AC POWER IN i I I I i I AC POWER IN Y J BOX SIDE PANEL Figure 2 17 Chiller Showing Various Components 60 ARES User Manual LN2 Controller The LN2 controller extends the lower range of the oven to 150 C using liquid nitrogen The LN2 controller is connected between an external liquid nitrogen source and the Test Station Figure 2 1 Controlled by the test station through Orchestrator software the LN2 controller consists of a Dewar flask a solenoi
133. f the material s modulus and the size of the sample Therefore discrepancies in sample dimensions will obviously affect the accuracy of test results Referring to the equations for each geometries strain and stress constants note the dependence of compliance on each of the dimensions Due to this dependence a small error in sample dimension may propagate into a large error in compliance and therefore modulus Testing outside the Linear Region Most of the tests available are designed to be conducted within the samples linear region Conducting tests outside the linear region may result in erratic or incorrect data It is critical that for a given material the linear region is determined first and then subsequent test performed based on the findings To determine a materials linear region typically a Dynamic Strain Sweep is run as a preliminary test 152 ARES User Manual Temperature Variations Changes in sample temperature during measurement can have a significant effect on the measured dynamic data particularly in the loss component of stress and in tan As a result temperature steps where temperature is held constant during a measurement may yield better tan resolution when studying the temperature dependence of a material as opposed to a temperature ramp where temperature is changing during a measurement Also make sure that sufficient equilibration time is provided for the entire sample to reach the test temperature Some sample
134. g for a 50 mm cone and plate geometry thermal expansion can cause contact between tools resulting in erroneous test data The system should be equilibrated at the desired working temperature and then the final gap set For special applications Invar tools can be used Invar has a coefficient of thermal expansion that is 10 times less than steel between 0 and 230 C Outside this range Invar s thermal expansion properties are similar to steel s If temperature ramps or sweeps must be performed using cone and plate tools Invar must be used sample Loading 1 ze 3 176 Ensure that the gap has been zeroed Place the sample on the lower plate Ensure that the sample is centered on the tool Using the stepper motor buttons on the right side of the test station adjust the sample gap until the upper plate is close to the specimen Set the gap using the Set Gap Instrument Control function entering the appropriate parameters The initial gap should be set approximately 0 05 mm above the final gap to facilitate sample trimming For softer materials using the normal force limits helps to avoid damaging the sample as the sample may be rapidly compressed in a manual loading procedure with insufficient time for sample relaxation Trim the sample flush with the edges of the plates Lower the stage to achieve the gap specified on the Certificate of Calibration Again this can be done manually or using the Set Gap Instrument Control function chan
135. ging the entered gap to the specified final value The sample should bulge slightly as shown in Figure 4 9 Allow samples to relax before beginning testing by monitoring the force and waiting for it to decay to close to zero Enter the sample dimension in the Orchestrator Test Geometry screen Note that if the tools were correctly zeroed the actual sample gap can either be read from the Gap real time parameter or measured automatically at the start of the test by selecting the Read Test Fixture Gap check box in the Geometry screen UPPER FIXTURE SAMPLE LOWER FIXTURE Figure 4 9 Cone and Plate with Sample Loaded ARES User Manual Torsion Rectangular New Design Strain Constant Stress Constant K TOTO COW TT J WAL 3 18 K 1000 WT Variables Gc Gravitational constant 980 7 cgs or 98 07 Sl T Thickness of sample mm W Width of sample mm L Length of sample mm Options Clamps to accommodate thicknesses up to 6 5 mm Environmental Systems Ambient Torsion Rectangular Tool Oven new design General Information The re designed Torsion Rectangular tool is used for testing solid materials with high modulus including thermosets thermoplastics and elastomers The sample is held in tension between the upper and lower tool Three setting anvils Figure 4 10 are provided to accommodate samples of varying thickness Each setting anvil is designed to provide clamping for two different
136. gle RomtMeasure enana 101 FCO IND Eee o e EA e En o UU oo O E E E N eae 101 U Usas 101 TOPON PAP E E E E E S 101 Byna E N O a a E E A E I E EE re rer eee 102 Funciona Dese O a E E E R E E 102 Seea O E E T eRe E EE E E ner ere een ae eee eer 102 MS NO a E A A ES o A AOE E E 102 FOC SIN E E A o A cesar conn eceeosaueacsuace cece yerrameradeas 103 Funciona I DOSCH AON oa EEE A A 103 pro io UL AAA 5 o In 104 iO a ahs AP o Pe A O eres 104 aria io a qshabia do 1 OR ER A o ce ee TE 105 Functional Descritores 105 er O AP Ei o A e doneaacenamnnea eaeenaueupye 106 MSS ori o o gts 0 o nn o no E O T N E ETE 106 Basa tea eo q 10 ro y e lt a OOO PA Un e A 107 Funciona TICS CHOI O I nta r R E EEE A 107 Sue 24 chet 216 Usos E ee ere 108 ici A o E E eee 108 Dynamic Temperature Raimi p gt Lest sisiisstasvsansnisvincaasansisnansacvasiasiansdiaansasueieiiiwanesabiagasesenasnanndyermaaslsinwetaansabacaaanens 109 PU COMA Descrip o AAA o oe stcgestipenses scaenatvacauaneiants 109 pe ORS 24 etc S16 il Okc PO OR o eC eee o o O oe et ere ar ere eer Tee 110 MSS INO A o o o O eo masa siagetatoaecounebanses 111 MultiWave Single Point MultiWave Temperature Ramp occoooonncnnccncnioninnnonanncnnanininannanccnnancnnn non nnnnanncnnanannnnso 112 Funcion WB ccs git OE a eceener re eee treme ne cer err ty eter ren rea rere eee ee reer 112 TES COPIE pcia 114 Frequency Temperature Sweet 115 tiale corn Sei 0 510 q E OPE OP UE E E O A E A N A E 115 oe a
137. h that it points toward the left front corner of the instrument However some 2K FRTN1 transducers may be equipped with a pin that is rotated slightly from this position The bearing locking and unlocking instructions for these transducers directs you to push the pin toward the left or right Regardless of the orientation of your pin left means toward the left hemisphere of the transducer as viewed facing the front of the instrument On low range transducers 100 FRTN1 200 FRTN1 and 1K FRIN1 the pin is installed so it points toward the front of the transducer housing as shown in the lower half of Figure 2 8 LEFT CLAMP RIGHT CLAMP BALL PLUNGER Factory Set ONE EsncH SIDE PIN UNLOCKED POSITION 2K FRTN1 or 2K FRTNIE LOCKED POSITION LOCKED POSITION a UNLOCKED POSITION FRONT CLAMP Rear CLAMP IS ON OPPOSITE S 0 BALL PLUNGER 100 FRTN1 Factory Set or nents 200 FRTN1 Figure 2 8 Bearing Locks 2K FRTN1 FRTN1E and 100 200 FRTN1 The view shown for the 2K FRTN1 transducers is looking from the front of the instrument The lock on the 1K FRTN1 is similar to that shown for the 100 200 FRTN1 transducer ARES User Manual Procedure for Locking and Unlocking Air Bearings FRTN1 and FRTN1E Refer to Figure 2 8 while performing the following procedures To Lock the FRTN1 air bearing 1 Read the Caution on page 11 2 Ensure that instrument power is off and air is applied to the transducer 3 Do
138. hanism or process in place to assure that the number of persons using this software concurrently does not exceed the number of LICENSES You may also store or install a copy of the TA Instruments instrument control software on a storage device such as a network server used only to install or run this software on your other computers over an internal network however you must acquire and dedicate a LICENSE for each separate computer on which this software is installed or run from the storage device A LICENSE for this software may not be shared or used concurrently on different computers b Data Analysis Software TA Instruments Thermal and Rheology data analysis software is not restricted to use on only one computer These programs may be installed on multiple computers for use provided it is for analysis of data generated by the LICENSED instrument control software 2 OWNERSHIP RIGHTS The software described above is owned by TA Instruments or its suppliers and is protected by United States copyright laws and international treaty provisions TA Instruments and its suppliers own and retain all right title and interest in and to this software including all copyrights patents trade secret rights trademarks and other intellectual property rights therein Your possession installation or use of this software does not transfer to you any title to the intellectual property in this software and you will not acquire any rights to this software except
139. he following C for G MAXIMUM C for G MINIMUM 2K FRTN1 2K FRTN1E i J 1 15e 06 rad gecm TA see note below 1K FRTN1 l J 4 9 e 06 see note below 2K STD 10K STD 0 J 2 60e 06 see note below 100 FRT for 0 100 J 2 60e 05 200 FRT 100 ERTN1 for 0 10 J 2 60e 06 E 200 FRTN1 a see note below for w lt 10 see note below NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Pick the correct values for your specific transducer and motor combination ARES User Manual To determine the maximum or minimum complex viscosity N that can be measured at a given frequency use the following formula nea 4 2 q where n Complex viscosity Poise G Complex Modulus dynes cm Frequency radians second Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 2 Substitute the G MAXIMUM value into equation 4 2 then determine the upper limit of operation by calculating N at each O 0 values chosen to be from the lowest to highest frequencies within the transducer operating range 3 Substitute the G MINIMUM value into equation 4 2 then determine the lower limit of operation by calculating N at each 4 Generate an X Y scatter plot of
140. he heaters must be evaporated liquid nitrogen LN supplied by the optional cryogenic LN2 Controller or very cold gas supplied by the optional Chiller Upper Gun Heater ata fe Upper Lower Oven PRT Oven PRT Lower Gun Heater Figure 2 16 Oven Chamber Showing Gun Heaters and PRTs Oven Temperature Control Oven temperature is maintained by a control loop that is closed around a Platinum Resistance Thermometer PRT The ARES has two control loops Oven PRTs to minimize vertical temperature gradients each of which is located in front of the respective gun heater being monitored The control system determines actual oven temperature by supplying a constant current to the PRT and measuring the voltage developed across it The difference between commanded and actual oven temperature is continuously driven to minimum You can choose to control the temperature of either the oven environment or in some cases the lower tool The choice is made using Orchestrator software The temperature of the lower tool can be monitored using the lower tool PRT which is mounted on the motor Installation of the lower tool PRT is covered as part of the lower tool installation in Chapter 3 Under normal operating conditions the oven PRTs are used to control oven temperature and the tool PRT is used to report sample temperature However the tool PRT can be used to control the oven temperature as well Figure 2 16 shows the inside of the oven chamber and the l
141. he measurement by clicking either the Toggle Steady Measure button Figure 3 11 on the toolbar or the Toggle Steady Measure function accessed from the Control pull down menu e When desired stop the measurement by clicking either the Toggle Steady Measure button on the toolbar or the Toggle Steady Measure function Direction For positive Rate values Direction specifies the rotational direction of the actuator at the first commanded shear rate Selecting Directions per Measurements of One results in data collection while the actuator rotates in the specified direction Selecting Directions Per Measurement of Two results in the following sequence of events 1 Data are collected while the actuator rotates in the specified direction 2 Data are collected while the actuator rotates in the opposite direction 3 The data are averaged to supply the single data point that is reported by Orchestrator Using two directions per measurement is necessary if the transducer changes range during the test Steady Rate Sweep Test El Ei Temperature 25 0 PC Mas 600 0 C Min 150 0 Sweep Mode icy Log f Discrete Initial Rate f 0 123 Maz 525 0000 Min 0 006250 Final Rate fi 00 0 ls Points Per Decade E Mas 500 Data Collection Mode amp Time Based Manual Delay Before Measure 20 Measurement Time 30 z Director ooo eee eres Clockwise C Cou
142. heaters in the oven It is very important that good quality air is supplied to the ARES test station at all times during use otherwise significant damage to the instrument can result The optional N2 GAS input is available for using other gases as the oven heating medium when the sample being tested would react with normal air Nitrogen is commonly used in this case Use the Gas Supply to Oven Selector Switch black knob below gauges to choose which gas input port is used to supply gas to the oven Gas Pressure Specifications Air should be supplied to the ARES at 5 5 scfm 156 1 min at a pressure of 80 psi 5 5 bar Gas connected through the N2 GAS port should be supplied at 60 to 70 psi 4 8 bar The gas supplied to the various components is regulated using the Air Pressure Adjust Knobs on the backside of the panel Pull the knob out and rotate it clockwise to increase the pressure to the desired component Pressure is monitored using the associated gauges on the side of the Pneumatics panel Pressure to the various components should be adjusted as follows REQUIRED COMPONENT PRESSURE Transducer 35 psi 40 psi with oven on Oven ARES User Manual Air Quality Specifications It is critical that high quality clean dry air is supplied to the test station at all times Any particles present in the air must be smaller than 5 microns Since the motor and transducer use air bearings larger particles in the air can easily damage
143. her Trademarks continued Swagelok is a registered trademark of the Swagelok Company Inconel is a registered trademark of Inco Alloys Special Metals X acto is a registered trademark of Hunt Corporation TYGON is a registered trademark of NORTON Co TA Instruments Q Series modules contain proprietary embedded operating system software copyrighted by Mentor Graphics SILICON SOFTWARE 1989 97 Mentor Graphics Corporation Microtec Division All rights reserved Unpublished rights reserved under the copyright laws of the United States RESTRICTED RIGHTS LEGEND Use duplication or disclosure by the U S Government or a U S Government subcontractor is subject to the restrictions set forth in the license agreement provided with the Software pursuant to DFARS 227 7202 3 a or as set forth in subparagraph c 1 and 2 of the Commercial Computer Software Restricted Rights clause at FAR 52 227 19 as applicable MENTOR GRAPHICS CORPORATION MICROTEC DIVISION 880 RIDDER PARK DRIVE SAN JOSE CA 95131 2440 ARES User Manual System Configuration This table should be filled out during system installation with assistance from the TA Instruments service installation engineer Please refer to the information below when contacting TA Instruments for customer support or service fnstument faes OO S ICC In Cres S S mesoi O AA INS IO EE AA O on oo S soionmental Control Tag Bata Peltier EN2conroer a chile oo S S Cds Crua
144. ideal solid Hooke s law for shear deformations states that if a shear strain T is applied to an ideal solid a shear stress Y develops in the material in direct proportion to the strain T GY The proportionality constant in equations for shear G is known as the modulus of the material The modulus of a material is a measure of its stiffness or ability to resist deformation Linear stress strain behavior is characterized by the modulus remaining unchanged as strain is varied The region where the modulus remains constant as strain is changed is called the linear region The linear region is also called the Hookean region of the material Newton s law describes the mechanical behavior of an ideal viscous fluid When a fluid moves by virtue of being pushed through a pipe or dragged through a screw in an extruder etc the movement is termed shear Newton s law relates the shear stress T to the rate of strain or shear rate dy dt T nit where N coefficient of viscosity A fluid is said to be Newtonian if the viscosity does not depend upon the strain rate An analogous equation can be written for tensile testing where the tensile stress 0 is related to the tensile strain e by ARES User Manual sa dt In a non Newtonian fluid the viscosity is not constant but is a function of strain rate Many polymer solutions are non Newtonian in behavior because their viscosity decreases as shear rate is increased This is called shear th
145. ighly corrosive or noxious materials such as sulfuric acid The tool is made form Hastelloy which is highly resistant to corrosion The tool is designed with a sealed glass chamber surrounding the sample The top tool and cover are designed to provide a liquid seal for the top After the sample is loaded the cover is put in place and an appropriate liquid is poured into the well on the back of the top plate This seals the chamber containing any sample fumes during testing Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using the parallel plate geometry The following geometry specific factors affect the operating range of parallel plate geometry e Plate diameter strain constant K and stress constant Kx e Gap between plates strain constant K e The viscosity of the sealing fluid may also affect the operating range ARES User Manual 165 Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type using the parallel plate geometry use the following equation i K lc 4 1 OTK Y where Kz Stress Constant K Strain Constant and C is computed from t
146. iia a endesa etc 51 Mant Ower WC AAA T POE o II N 51 Enecumaties Tinei ri EE S ii EA 53 E T anes E N A E A T A A E E T E 53 Cas Prenu cae 9 216 602 MON Sansa 53 Ae ahy OCC iga ON e n E E E N 54 Focumauc k onnec hona cracca aaa 54 Environmental Control Systends usais 57 a E EE E A E A AO 58 Oven Temperature COn Ora 58 l E E E E EE T T T E I 59 CS a E Mm o y ene eee ae 59 S LE TT L E T E EE E T E O E ee ee 59 AO o E CAPA A TT A A T E E O E 59 MAIN E EE ta aa E E N E E E 59 EN OTO E na E ENE O A T T E T are ren 61 Dew T E epa n rasta vd E E IE E A E E E EE E EEE oncia 61 CO O E E T E E E 61 OBES CONC Ura LION spinanie E EE E E 61 ENSEon tolera 61 Mie INC sitio dpto 62 RC CUO IO OPIO E E E T E A E T 62 Oven Operatine Requirements surrender R E A 63 Oven Configuration in Orchestrator sccssssscsssssssssesssssesssscssssssssnscsssscsssscsssnsessnecssssesssneesssecsssesssecessneessneesseeee 64 ARES User Manual Si o UI A 65 dio berto oo lolo Lars 1 101 N E E O A E E RT 66 FNC Me ke ia a e A oo o E E A A E A a AR 67 Descrip MOM AAA EAEE E E E E EOE A E 67 lstallation of Fhud oy A A oO E Ena an rr 67 Circula lor COMMS CHIOIS sario tii 70 el Bal bg Yo A O PORO E E eee er ener eee err re 70 Lower Tool installation and Removal persia ina 71 iras o E o 71 TM Elia bat 2Conteuration ln Orchestrator ctricos pere a EN AREA aereas Te PID Loop Cp PEPPER 73 Pid Ban Oporne Requirements oi 74 Pe Tani z Or Oi paa 74 Poe ae tc lee RN
147. ilities pull down menu to reflect the correct COM port You must tell the software the correct COM port you are using in order for communication with the Test Station to take place If you have a serial mouse more than likely it is using COM1 and you will need to use another serial port COM2 for example to communicate with the test station The oven position and temperature sensors are connected to the test station through the OVEN connector The optional LN2 Controller is interfaced to the LN2 connector if cooling option is required If the Fluid Bath is used connect the RS 232 output from the circulator to the CIRCULATOR connector Many of the connectors are not used under standard operation of the ARES However they are available for more customized applications when needed Examples might be to plot applied strain on an external strip chart recorder or to input an external voltage to be digitized with the test data Table 2 1 contains more detailed information regarding these additional connectors Figure 2 12 Test Station Signal Panel ARES User Manual Table 2 1 Signal Panel Connectors TORQUE OUT Outputs a DE voltage that is proportional to transducer output torque Scaling is Q VDC 0 g cm torque 5 VDC full scale torque As the instrument is shipped TORQUE IN is connected to and outputs the same TORQUE IN signal as TORQUE OUT This connector is normally used by TA service personel for diagnostic purposes Dynamic
148. ill result in rapid evaporation of fluid trapped in the Peltier Assembly hoses causing hose rupture damage to the Peltier Assembly and possible personal injury ES WARNING Do not operate the Peltier system unless fluid is being Peltier Operation Turn on the Circulator and set it to the desired temperature The Peltier is operated using the Instrument Control Panel Figure 2 33 Set the environmental control option to On The desired temperature is set in the Temperature input field Humidity Cover After you have loaded the sample you may install the two piece Humidity Cover Figure 2 34 by simply placing each half of the Cover onto the top of the Peltier Assembly and pressing the halves together The Humidity Cover helps to create a thermally isolated chamber thus insuring that the Peltier specifications are met It also prevents sample evaporation during testing The pads on the inside of the cover should be saturated with sample before each use to minimize evaporation WARNING During and after testing at other than ambient x temperature the sample test surface can reach temperatures that cause personal injury Allow the Peltier System to return to ambient temperature BEFORE you touch the sample test surface or the sample ARES User Manual Instrument Control Panel Figure 2 33 p50 Peltier T hermopile heat pump OF Instrument Control Panel Showing Peltier Control Options Figure 2 34 Humidity Co
149. inimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type using the double wall Couette use the following equation Ks lc 4 1 ae e where K Stress Constant K Strain Constant and C is computed from the following C for G MAXIMUM C for G MINIMUM see note below Transducer 2K FRTN1 2K FRIN1E see note below 1K FRTN1 Ce 0 2K STD These Ge are not recommended 10K STD for use with the Double Wall Couette 100 FRT for 100 J 2 60e 05 200 FRT ae 100 FRTN1 for 0 10 J 2 60e 06 200 FRTN1 mm see note below NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination ARES User Manual To determine the maximum or minimum complex viscosity N that can be measured at a given frequency use the following formula nea 4 2 q where n Complex viscosity Poise G Complex Modulus dynes cm Frequency rad sec Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 2 Substitu
150. inning or pseudoplasticity In the opposite effect shear thickening or dilatancy the viscosity increases with increasing shear rate This is seen in some concentrated aqueous dispersions of clays and sands Steady Shear Testing Steady Shear Testing uses continuous rotation to apply strain When a steady shear rate is reached the shear stress T is measured as a function of the shear rate dy dt The stress to shear rate ratio yields the steady shear viscosity N Measurements are typically made over a wide range of shear rates to study the shear rate dependence of the sample Dynamic Mechanical Testing Definition of Variables Dynamic mechanical testing involves the application of an oscillatory strain to a sample The resulting sinusoidal stress is measured and correlated against the input strain and the viscous and elastic properties of the sample are simultaneously measured If the sample behaves as an ideal elastic solid then the resulting stress is proportional to the strain amplitude Hooke s Law and the stress and strain signals are in phase If the sample behaves as an ideal fluid then the stress is proportional to the strain rate or the first derivative of the strain Newton s Law In this case the stress signal is out of phase with the strain leading it by 90 For viscoelastic materials the phase angle shift 6 between stress and strain occurs somewhere between the elastic and viscous extremes The stress signal gener
151. irculator pump outlet to the fluid bath inlet This clamp is critical to adjust the flow to the bath If the clamp is not installed or the flow not adjusted properly it is possible to overflow the Fluid Bath and cause significant damage to the test station motor The clamp should be set by placing it on the inlet hose circulator off and completely closing the clamp as tight as it will go finger tight Make an index mark on the clamp knob and then using the index for reference open the clamp two to four complete turns The number of turns the clamp is opened will depend upon the make and model of circulator used We have found that when using the Julabo FS 18 supplied with new systems the clamp should be opened four turns For older NesLab chillers two turns was effective However these values should be taken as guidelines only and you should monitor the flow and bath to ensure that the flow rate to the bath is correct for their specific system When the clamp is set correctly you can feel by holding the outlet hose strong fluid flow through the bath outlet hose it will pulsate somewhat and the bath will stabilize at the desired temperature in about 30 minutes If the clamp is closed too much the flow through the bath outlet hose will feel weak or nonexistent and the temperature will continuously oscillate without stabilizing If the clamp is opened too much the bath will eventually overflow The bath should be monitored and if any flui
152. ish playing and the motor will stop Data will be collected for an additional 5 seconds in Zone 2 after which the test will end Equation Syntax Equations for Waveshape are entered as a function of time using the variable t Standard arithmetic operators an be used as well as a variety of mathematical functions such as sin cos exp etc Standard rules for operator precedence are used and parenthesis may be used to change the order of evaluation Table 3 5 contains a list of available functions Test Options e Delay Before Test e Analog Data input ARES User Manual Table 3 5 Available functions for the Arbitrary Waveshape Test Note The arguments to trigonometric functions are in radians Operation Exponentiation Highest Multiptication 1 7 Division fT Addition fT Subtraction Lowest Functions cosht asin Arccosine atan sat abs ARES User Manual Thixotropic Loop Rate Ramp Description In each of up to four zones Thixotropic Loop commands a steady shear rate that linearly accelerates or decelerates to a final shear rate The time allotted to achieve the final shear rate is selectable in each zone offering control of actuator acceleration Figure 3 18 In each zone the following parameters are set Final Shear Rate Shear rate to which the initial rate is accelerated or decelerated In the first zone the initial rate is zero In subsequent zones the i
153. l ARES User Manual Dynamic Temperature Step Test Figure 3 26 AutoTension Adjustment Set Up Screen Analog Data Input Analog Data Input allows you to apply an external 10 VDC analog input signal to the Analog Input BNC ANALOG 1 IN receptacle on the Test Station Rear Panel and measure and record with the rest of the data the input signal during any test Data are sampled at 1 Hz and only one measurement is recorded for each data point Apply an external 10 VDC input signal then check the Analog Data Collection checkbox Figure 3 27 During the test Orchestrator reports the analog input as Analog Input Data which can be displayed in the spreadsheet plot or as an on line parameter The reported values are normalized by dividing input voltage by 10 Thus an input voltage of 10 volts is recorded in the data as 1 00 Figure 3 27 Analog Data Input Set Up Screen 144 ARES User Manual AutoStrain AutoStrain is used to prevent the dynamic force signal from going above or below the specified force limits of the transducer When using AutoStrain control the actual sample strain may differ from that commanded Following is a description of AutoStrain parameters that must be set Figure 3 28 Maximum Applied Strain This value represents the maximum allowed strain to be used in the AutoStrain adjustment The strain amplitude will never exceed this value irrespective of the measured force Maximum Allowed Force Whe
154. l Each PRT is designed to contact the lower tool and provides the temperature of that tool Note that the PRT used with the different Couettes is shorter than the PRT used with the Parallel Plate tool Because of its length the Couette PRT can be difficult to remove by hand An extraction tool is provided to aid in the removal of this PRT When removing the short PRI slip the tool over the PRT end and engage the slot in the tool over the pin on the PRT as shown the detail of Figure 2 24 Pull the PRT straight up and out of the bath DO NOT rotate the PRT in its mount since damage to the connector can result Install the lower tool PRT as follows 1 Ensure that the proper PRT is selected from the lower tool PRTs available for use with the ARES Fluid Bath 2 2 Using very little force place the PRT plug keyed end through the hole in the bath and onto the receptacle that is installed in the motor 3 Gently push down on the PRT and rotate it until the PRT slips into the receptacle the keyed end of the PRT then slips into the key slot machined into the receptacle Seat the PRT completely into the receptacle When properly installed the displayed temperature parameter should indicate ambient temperature BATH HOUSING S COLLAR CROSS SECTION SHOWN FOR VISIBILITY Figure 2 23 Fluid Bath Alignment Pin ARES User Manual COUETTE PRT EXTRACTION TOOL BATH 2 PARALLEL PLATE lower fixture COUETTE PRT PN 700 03484
155. l Computer e Motor and Transducer e Environmental Control Control Computer The control computer synchronizes generates and directs test instructions to and processes raw data from all subsystems The control computer central processing unit CPU commands and monitors the control computer maintaining communications via the bi directional BUS The input output controller 1 0 controls all hardware switching within the instrument The analog to digital converter A D acquires analog signals from the motor and transducer scales the signals for optimum gain and converts them to digital form for processing by the CPU The temperature controller TEMP CONTROLLER sends electronic commands to operate the environmental control subsystem TEMP CMD AND MEASURE based upon your input It also acquires and processes temperature data TEMP CONTROL AND FEEDBACK for environmental control and display The CPU and random access memory RAM contain memory devices programmed to execute test sequences The RAM circuitry stores data received from all subsystems for further processing by the HOST COMPUTER IBM or 100 IBM compatible PC that communicates with the control computer through the RS 232C data communications link Motor In dynamic mode the Motor is configured as a position servo In steady mode it is configured as a rate servo Following the start of a test the FUNCTION GENERATOR determines the waveform to be applied COMMAND The MOTOR CONT
156. lation Delay 146 Couette test tool constants 190 tool installation 192 general information 190 operating range 190 sample loading 192 vane tool 193 Creep 126 D Delay Before Test 141 Dewar Flask 61 Diagnostic LEDs 230 Dilatancy 94 ARES User Manual Double Wall Couette test tool constants 195 tool installation 197 201 general information 195 operating range 196 sample loading 198 201 Dynamic Measurement Formulas 204 Dynamic Single Point Measurment 101 Dynamic Strain Sweep 100 107 Dynamic Temperature Ramp 109 110 Dynamic Temperature Step 105 Dynamic Time Sweep 100 102 E E See Elastic Modulus E See Viscous Modulus E See Complex Modulus Elastic Modulus E 94 Elastic Stress t 94 Elasticity 93 Elastomers 149 Emulsions 149 Environmental Control System configuring 64 description 57 principles of operation 27 specifications 30 Errors discrepancies in sample geometry 152 temperature variations 153 testing outsidde linear region 152 ARES User Manual F Fluid Bath circulator connections 87 description 85 inet line clamp 88 installation 85 lower tool 87 operating specifications 30 operation 92 Fluid Bath 2 circulator connections 70 description 67 installation 67 lower tools 71 operation 74 PRT installation 70 Force Gap test 134 Force Gap Test 134 Frequency Sweep 100 103 104 Frequency Temperature Sweep 100
157. le point measurement see section on Testing Options for further details e Steady PreShear e Delay Before Test e Analog Data Input e Correlation Measurement Options ARES User Manual 101 Dynamic Time Sweep Functional Description The Time Sweep test takes successive measurements at constant temperature frequency and strain at a selected interval The time required to make a measurement is frequency dependent At frequencies less than 2 0 rad sec 0 3 Hz it is equal to the time required to complete approximately 1 5 cycles of oscillation At high frequencies the limit is approximately 2 second per measurement Adjusting the Correlation Delay see Measurement Options can also have an effect on the time required to make a measurement If a Time Per Measure is entered that is less than the amount of time required to complete the measurement Figure 3 3 the control computer will take data points at its maximum speed in accordance with frequency If many points are to be taken over a short time period a short time measurement such as 2 0 sec could be used This sets the instrument to take measurements as fast as possible Dynamic Time Sweep Test ki El Frequency fl 0 0 rads Max 500 0 Min 1 00e 05 Ml 7 0 Max 372 5000 Min 0 0031 25 Temperature 25 0 CE Max 600 0 C Min 150 0 C Total Time fi 010 s or hems Time Per Measurement f s or Airs Options PreShear Ot Delay Off SutoTens Of
158. lease call the Thermal Analysis Help Desk at 1 302 427 4070 SERVICE U S A For instrument service and repairs please call 1 302 427 4050 BELGIUM LUXEMBOURG TA Instruments a Division of Waters N V S A Raketstraat 60 Rue de la Fus e 1130 Brussel Bruxelles Belgium Phone 32 2 706 00 80 Fax 32 2 706 00 81 EUROPE TA Instruments Ltd Cleeve Road Leatherhead Surrey KT22 7UQ United Kingdom Phone 44 1372 360363 Fax 44 1372 360135 FRANCE TA Instruments Division de Waters SA 1 3 Rue Jacques Monod 78280 Guyancourt France Phone 33 1 30 48 94 60 Fax 33 1 30 48 94 51 GERMANY TA Instruments Germany Max Planck Strasse 11 63755 ALZENAU Germany Phone 49 6023 96470 Fax 49 6023 964777 ARES User Manual ITALY Waters S p A Via Achille Grandi 27 20090 Vimodrone Milano Italy Phone 39 02 27421 283 Fax 39 02 250 1827 JAPAN TA Instruments Japan No 5 Koike Bldg 1 3 12 Kitashinagawa Shinagawa Ku Tokyo 140 Japan Phone 813 5479 8418 Sales amp Application Fax 813 5479 7488 Sales amp Application Phone 813 3450 0981 For Service amp Accounting Fax 813 3450 1322 For Service amp Accounting THE NETHERLANDS TA Instruments A Division of Waters Chromatography bv Postbus 379 Florijnstraat 19 4870 AJ Etten Leur The Netherlands Phone 31 76 508 72 70 Fax 31 76 508 72 80 SPAIN Waters Cromatografia S A Entenza 24 Planta Baja 08015 Barcelona Spain Phone
159. lowing the guidelines discussed in the section on the liquid seal ARES User Manual 171 172 Enter the sample dimension in the Orchestrator Test Geometry screen Note that if the tools were correctly zeroed the actual sample gap can either be read from the Gap real time parameter or measured automatically at the start of the test by selecting the Read Test Fixture Gap check box in the Geometry screen FILL PORT for sealing fluid eee ees UPPER a OL Ae SAMPLE GLASS CHAMBER LOWER TOOL Figure 4 8 Hastelloy Tool with Sample Loaded ARES User Manual Cone and Plate Strain Constant Stress Constant 3000 G A ta 2TR Normal Stress Constant First Normal Stress Difference _ 200 P K Z aR Go N K F Variables Gc Gravitational constant 980 7 cgs or 98 07 Sl R Radius of plate mm B Cone angle rad F Normal force g Options 25 50 mm Diameter 0 02 0 04 0 1 rad Cone Angle Disposable cones and plates Invar cones and plates Environmental Systems Ambient Oven Fluid Bath Fluid Bath 2 Peltier Cone and Plate Tool see Chapter 2 for more details regarding lower tool General Information The Cone and Plate tool is used in the testing of polymer melts as well as suspensions and emulsions By design there is no velocity gradient across its diameter during steady shear testing It is also used when shear normal stress measurements
160. lt in extensive damage to this instrument WARNING If this instrument is used in a manner not intended or specified in this manual the protection provided by the instrument may be impaired WARNING This is a high torque motor Turning on the motor while in dynamic mode causes the motor to snap to dynamic zero position at a high velocity This can cause severe damage to the transducer and or personal injury To avoid damaging yourself and the transducer Never turn on the motor while a sample is loaded Keep hands clear of the motor ARES User Manual ARES User Manual Q CAUTION Force Rebalance Transducers contain a precision air bearing that is equipped with a bearing lock which prevents movement of the air bearing when no air is applied To avoid damaging your transducer familiarize yourself with the operation of the bearing lock see the next topic and observe the following cautions Do not apply power to the instrument when the bearing is locked Do not unlock the bearing unless air is applied to the transducer If the air supply must be intentionally interrupted turn off instrument power and lock the bearing prior to removing air If the air supply is interrupted while the bearing is unlocked do not touch the anvil until air is restored Maintain air flow to the transducer at all times to prevent contamination of the air bearing Failure to observe these cautions will result in damage to the trans
161. ly collected Manual Mode Following the start of the test Manual Mode data collection takes a single measurement when commanded to do so Manual Mode operation is as follows e Start the test e When desired start the measurement by clicking either the Toggle Steady Measure button Figure 3 11 on the toolbar or the Toggle Steady Measure function accessed from the Control pull down menu e When desired stop the measurement by clicking either the Toggle Steady Measure button on the toolbar or the Toggle Steady Measure function Manual mode is designed to allow you to acquire data in the steady state region by manually monitoring the torque signal e 2 by using an external strip chart recorder which is proportional to the sample stress For accurate steady state data measurements should be made at a point where all of the transients in the torque signal have disappeared and the torque value is relatively constant aa Figure 3 11 Toggle Steady Measure Button Direction For positive Rate values Direction specifies the rotational direction of the actuator at the first commanded shear rate Selecting Directions per Measurements of One results in data collection while the actuator rotates in the specified Direction Selecting Directions Per Measurement of Two results in the following sequence of events 1 Data are collected while the actuator rotates in the specified Direction 2 Data are collected while the actuator rotat
162. made in the following sections you should refer to the Orchestrator online help and other software references for a complete description of how to use the software Test Station The Test Station is the main instrument component that houses the motor and transducer between which the sample to be tested is placed It also houses the environmental controller as well as the other electronic subsystems used in powering and controlling the Test Station Figure 2 2 and Figure 2 11 show Test Station assemblies that are described in more detail within this chapter Test Station Front Assemblies and Controls The front of the test station Figure 2 2 is where the motor transducer and oven are located In addition the basic controls necessary to operate the test station are located on the front panel All basic mechanical operations associated with the ARES are performed from the front of the test station The following sections describe front panel systems in more detail Motor The Motor Figure 2 2 also referred to as the actuator deforms the sample by applying a shear strain to the sample The Motor can be operated in either dynamic sinusoidal mode or steady constant rotational rate mode You can control the amplitude and frequency of the Motor movement dynamic mode causes the motor to snap to dynamic zero position at a high velocity This can cause severe damage to the transducer and or personal injury To avoid damaging yourself and the
163. mately 80 C exists between the fluid temperature and the upper limit of the thermal operating range To determine thermal operating range for a given fluid temperature add these differentials to the fluid temperature For example at a fluid temperature of 20 C the thermal operating range of the Peltier system is approximately 20 C to 100 C calculated as follows Lower Limit Upper Limit AT Fluid Temp ATy Fluid Temp 40 C 20 C 80 C 20 C 20 C 100 C At a fluid temperature of 40 C the thermal operating range of the Peltier system is approximately 0 C to 120 C calculated as follows Lower Limit Upper Limit AT Fluid Temp ATy Fluid Temp 40 C 40 C 80 C 40 C 0C 120 C ARES User Manual Installation of Peltier Three screws fasten the rotating Shaft of the Peltier Assembly Figure 2 29 to the Test Station Motor Anvil A threaded collar secures the Peltier Assembly Body to the Test Station Motor Housing Electrical contact to the Test Station is established by the PRT Plug a seven pin male Lemo plug that is attached to the rotating Shaft of the Peltier Assembly During mounting of the Peltier Assembly the PRT Plug is automatically pushed downward into the PRT Receptacle at the center of the Motor Anvil Two hoses supply fluid between the Peltier Assembly and the fluid source which is typically a temperature controlled circulator Prior to mo
164. ment if the final strain is less than the initial value Dynamic Strain Sweep Test Ei Es Frequency al 0 0 rad s Max 500 0 Min 1 00e 05 Temperature 25 0 PC Ma 500 0 Min 150 0 Sweep Mode Log C Linear Initial Strain 0 1 Max s12 5000 Min 0 0031 25 Final Strain i 00 0 Points Per Decade 5 Mas 500 Options PreShear Off DelawOth MeasUps Off Options End of Test Save As Help Cancel Figure 3 6 Dynamic Strain Sweep Test Set up Screen ARES User Manual 107 Suggested Uses Suggested uses of the strain sweep are as follows e Determination of the limits of linear viscoelasticity and torque levels e Characterization of samples that exhibit extreme nonlinear behavior such as filled thermoplastics thermoplastic blends etc Test Options The following test options can be selected for use with the strain sweep e Steady PreShear e Delay Before Test e Analog Data Input e AutoStrain e Measurements Options o Delay Settings o Strain Amplitude Control ARES User Manual Dynamic Temperature Ramp Test Functional Description Temperature Ramp testing takes measurements at selectable temperature ramp rates while holding a constant frequency and strain Temperature is automatically incremented or decremented from selectable lower and upper temperature limits at selected rates A unique set of test conditions can be entered in up to eight temperature ranges o
165. moved from the lock is one of 4 screws used to secure the cover ARES User Manual MACHINE SCREWS 3 MOTOR LOCK MOTOR COVER REMOVED PHILLIPS HEAD SCREW Figure 2 10 LS Motor Bearing Lock ARES User Manual Test Station Rear Input Panel The rear of the test station is where all electrical pneumatic and signal connections are made Figure 2 11 The main power switch is also located at the rear of the test station PNEUMATICS PANEL OO SIGNAL PANEL y gt P a e e MAIN POWER SWITCH Figure 2 11 Test Station Rear View Signal Panel The Signal Panel is the input output interface for electrical signals entering and leaving the Test Station Figure 2 12 and Table 2 1 identify and describe Signal Panel connectors including the basic connections for Test Station use Signal Connections There are two basic signal connections required for test station operation They are a connection to the host computer and a connection to the oven or bath circulator depending upon the environmental control system used Connect the test station to the host computer through the HOST port on the signal panel and the appropriate COM port on the host computer By default COM1 is selected by the software when it is run for ARES User Manual the first time If you are using a different COM port change the software configuration using the Instrument Set Up function in the Ut
166. mperature Ramp Functional Description The MultiWave test is a dynamic test method that superimposes up to 7 harmonic frequencies on a selected fundamental frequency This allows you to acquire data at several frequencies simultaneously in a fraction of the time required to run a conventional frequency sweep MultiWave is based upon the Boltzmann Superposition Principle which states that two or more simultaneous strain deformations are linearly independent of each other Because each wave acts independently the displacement strain of a point in the material is the sum of the strains caused by each wave providing the total strain is within the linear viscoelastic region of the material Data correlation takes place at each of the applied frequencies using the same set of raw data and the algorithm mathematically extracts the torque and displacement signals at the desired frequency from the total combination of signals In order to program this test you must provide information on the fundamental frequency Frequency The frequency of the fundamental lowest value used This value must be below 2 0 rad sec because of the way that the data correlation algorithm works Strain This is defined as the strain amplitude of the fundamental frequency Temperature This is the test temperature that will be used in your experiments Harmonic information is given in the next section of the test setup screen Harmonic This is an integer value by
167. mperature before starting the test to allow the bath and sample to stabilize 4 For normal applications set the Temperature Calibration Table to Default For critical temperature work the adjustable option can be used to enter calibration offsets for specific temperature setpoints Refer to the Orchestrator online help for details on how to set up this feature PID Loop Setup When using Tool Temperature control errors between commanded and actual temperature are driven to zero by a PID Proportional Integral Derivative loop control system The PID loop settings Figure 2 26 affect how the bath settles at a set point temperature The values are affected by circulator fluid used as well as the circulator specifications As the bath reaches a setpoint there will typically be a few degrees of overshoot after which the temperature will oscillate a few times and then stabilize Typical stabilization times are 15 minutes to reach 0 1 C and 35 minutes to reach 0 01 C By modifying the Proportional Band P coefficient less overshoot can be achieved but there will typically be more oscillations before the bath stabilizes so the overall stabilization time will be longer ARES User Manual PID Setup Form Ei E3 PID Temperature Control Setup Choose PID Bath Tool Temp Proportional Band 0 75 Cancel Figure 2 26 PID Setup Form The values listed in Table 2 7 should be used as guidelines and will work f
168. mple dimensions e Width e Thickness e Length STD transducers only length will be determined from gap setting for 2K FRT transducers 2 Select an insert and place the sample between the inserts 3 Place the sample with inserts into the lower tool then place both collars one above the other over the sample Ensure that the lower collar rests flush against the four stop pins in the lower tool 4 Lower the stage until the upper tool is about 1 4 inch from the sample 5 Open the Set Gap Instrument Control function Use the Motor Position Offset button to radially align the sample with the upper tool if necessary ARES User Manual 187 11 12 13 CAUTION In the next step do not generate a Torque or Normal Force greater than 50 of full scale Failure to observe this caution may result in damage to the transducer While confirming the upper insert and sample fits into the upper tool lower the stage until a compressive downward Normal Force of about 10 of full scale is generated If the sample is not aligned properly re raise the stage and realign the sample and tool using the Motor Position Offset button Ensure visually that the insert is resting on the four small pins that are located directly below the lower and above the upper insert Slide the upper collar up onto the upper tool ensuring that the collar rests flush against the four stop pins in the tool Tighten the collar just enough to hold it in plac
169. mpressed in a manual loading procedure with insufficient time for sample relaxation In either case the initial gap should be about 0 05 mm higher than the final desired gap ARES User Manual 163 164 Trim the sample flush with the edges of the plates Lower the stage to the final gap setting Again this can be done manually or using the Set Gap Instrument Control function changing the entered gap to the desired final value The sample should bulge slightly as shown in Figure 4 4 Allow samples to relax before beginning dynamic testing by monitoring the force and waiting for it to decay to close to zero Enter the sample dimension in the Orchestrator Test Geometry screen Note that if the tools were correctly zeroed the actual sample gap can either be read from the Gap real time parameter or measured automatically at the start of the test by selecting the Read Test Fixture Gap check box in the Geometry screen UPPER FIXTURE SAMPLE LOWER FIXTURE Figure 4 4 Parallel Plates with Sample Loaded ARES User Manual Hastelloy Tool Parallel Plates Strain Constant Stress Constant 2000 G es g 2006 H TR Variables G Gravitational Constant 980 7 cgs or 98 07 SI R Radius of plates mm H Gap between plates mm Options 40 mm size Environmental Systems Ambient Oven Hastelloy Tool General Information The Hastelloy Tool is a specialized set of 40 mm Parallel Plates This tool is used to test h
170. n 149 iii e E nc I E E A E A N E E oe errr 149 Fluids Suspensions and EMUlSIONS nar Rd 149 Solid Samples Including Thermosets Thermoplastics and Elastomers oooocnnccncnncnnnnoninnnnncnnanncnnannnnnos 149 POT EME E O O ias 150 Inermos ttine Resins and other Curing SUIS ss narnia mene 150 Testing Limits and Completa 150 Derr O nl SOL aC SAIC GM so resina n inean acre asp 150 Determination ot Operational Rad dia 151 Possible SOU ees and Causes OLEO ap 152 Discrepancies im Sample Geometry sansirnir eai arn oma RTN 152 Tests Ouis ide the near RE ION easing E E E E pcled 152 Ler E Y O a E E A EE N OE I E N 153 OET E ClO PP T AS 153 Eo o o Mi ea a a E E EE E A E EE E E ra 154 Upper Too In lonas 154 Lower Tool Installation Motor Mount Oven or Ambient cccooocccnnnoccccnonononnnnnonnnnnnnnanononononnnnnnnnnnnnnonnnnnos 154 Lower Tool Installation Fluid Bath MoUDE ooooonccncciccnoconinannnononacnnaninonnnnnanonanncnnoncnnnnonnannancnnn non cnn canncna cnn noncannos 154 lt a bateas A n a On E wari bausdonaads hess desdldauneameomuacsanertenntte 157 MATA AO e aaa 157 Automate Zeroing and Gap SOLANO erario tilde 158 FTO 19 Len sy o PAPA o E A O 158 rs DEN TM E o DOOR O OU o o O yay wee E E E E crus 158 Comments Concenime the Gap Control Pane rss icicii 158 Enable the Gap Control Ponent pio 158 Read Test POOH Cap GCC DO aye E OE E E E S E 159 DONS play Me the Atunes 159 Max Allowed Force While Seitine ii 159 Test Tool Installation and S
171. n of the oven including use of either the LN2 controller or Chiller LN2 Controller Operation Open the valve on the liquid nitrogen source All remaining operation of the LN2 controller is performed through Orchestrator In order to fill the Dewar the LN2 Controller Dewar must be turned ON using the Orchestrator Instrument Control Panel While the Dewar is filling the software system status will indicate LN2 filling and temperature control is not active Once the Dewar is filled the software status will indicate LN2 READY at which point temperature control will be active ARES User Manual Maintenance There are no user serviceable parts inside the LN2 controller Periodic servicing is performed in conjunction with Test Station maintenance visits by Technical Services LN2 Transfer Line Maintenance This transfer line utilizes an insulating vacuum jacket The stainless steel used to manufacturer this transfer line outgases under vacuum conditions This outgasing degrades the transfer line s vacuum jacket and therefore its insulating properties Absorbents or getters are added in the vacuum space to absorb the gases and prevent the metal s outgasing from destroying the transfer line s insulating vacuum The getters must be renewed periodically to maintain their absorbent qualities This is simply done by using the transfer line to transport nitrogen gas from the dewar to the oven The low temperature of the N2 gas
172. n the dynamic force rises above this value strain is decreased This should be set this to the maximum dynamic force that you wish to maintain during a measurement Minimum Allowed Force When the dynamic force drops below this value strain is increased This should be set to the minimum dynamic force that you wish to maintain during a measurement Strain Adjustment This is the percentile by which strain is increased or decreased when the measured dynamic force is below the entered Minimum Allowed Force or above the entered Maximum Allowed Force The percentage of commanded strain entered depends upon how fast the dynamic force is decreasing between measurements Dynamic Temperature Ramp Test EAE Options Steady PreShear f Delay Before Test f AutoTension Adjustment f Analog Data Input f AutoStrain Adjustment f Measurement Options W AutoStrain Strain Limits Max 312 5000 Min 0 003125 Max Applied Strain i D Max Allowed Torque i 800 0 g em Min Allowed Torque 5 0 g em Strain Adjustment 50 0 of Current Strain Figure 3 28 AutoStrain Set Up Screen ARES User Manual 145 Measurement Options The Measurement Options in a test can control the delay settings The Default Delay setting gives 0 5 cycles and 3 seconds whichever is longer delay before data collection For some samples this may need to be increased to allow the material to reach a steady state
173. n to sample stress This is known as a compliance and is represented by a J in shear testing and a D in linear testing As in case of modulus values it is possible to define both elastic J or D and viscous J or D components to the complex compliance J or D The ratio of the viscous modulus to the elastic modulus is the tangent of the phase angle shift between stress and strain or tan Tan 6 is a measure of the damping property of the material Table 3 1 and Table 3 2 summarize the variables frequently used in dynamic mechanical testing for both linear and shear testing geometries Table 3 1 Dynamic Mechanical Variables Shear Geometries Complex Stress Amplitude a Complex Strain Amplitude G Complex Modulus Complex Modulus Elastic Modulus G a Storage Modulus Viscous Modulus G sin 0 a Modulus ue Complex Compliance ye Elastic Compliance J cos A Storage Compliance Viscous Compliance J sin A a Glo nt Complex Viscosity Viscosity a In phase Viscosity n sin Out of phase Viscosity n cos d ARES User Manual 95 Table 3 2 Dynamic Mechanical Variables Linear Geometries or complex Suess Ampiudo fe Complex ran Ampiudo o ees oo C Lone Elastic Modulus E cos d Storage Modulus Viscous Modulus E sin d Fo Fon Modulus DY Complex Compliance Compliance Elastic Compliance D a Storage Compliance Viscous Compliance D sin z Co E Bo pe Comple
174. ng Figure 2 23 aligned with the corresponding notch which should be located toward the rear of the instrument machined into the motor housing 6 Mount the bath onto the motor by placing the threaded collar onto the threads machined into the motor and seating the alignment pin into the notch machined into the motor housing It may be necessary to rotate the bath back and forth until the pin falls into the notch 7 Tighten the threaded collar then tighten the knob on the motor anvil hand tighten only do not over torque 8 Install the lower tool PRT as follows a Ensure that the proper PRT is selected from the three lower tool PRTs available for use with the ARES Bath Lower Plate Parallel Plate or Cone and Plate Geometries 700 02647 EA eS S Lower Cup Standard Couette Geometry 700 02647 1 17mm Lower Cup Shallow Couette Geometry 700 02647 2 b Using very little force place the PRT plug keyed end through the hole in the bath and onto the receptacle that is installed in the motor ARES User Manual 85 c Gently push down on the PRT and rotate it until the PRT slips into the receptacle the keyed end of the PRT then slips into the key slot machined into the receptacle When properly installed Orchestrator should indicate ambient temperature CAUTION BATH PRT CHECK FOR FLUID LEAKS AT THIS SEAM A BATH WELL ACCESS PORT THREADED COLLAR MOTOR COVER Figure 2 35 Fluid Bath Installation 86 ARES
175. ng the Zero button Wait about 30 seconds during which time the instrument takes several readings to establish a zero torque reference When zeroing is completed the Transducer Calibration form is displayed Figure 5 4 If after selecting the Zero button the NORMAL FORCE value displayed is either very high such as 1E 5 or exactly zero refer to the Troubleshooting Guide The normal force should be less than 0 1 of the full scale normal force NOTE Do not hang any weights until after at least one 1 zero reading has been taken 8 Hang the weight specified in Table 5 4 depending on the transducer in use from the hook on the bottom of the calibration tool Figure 5 6 Ensure that the weight is free to hang without obstruction and that the weight is steady not swinging from side to side 9 Select the Normal Cal button The Normal Calibration form is displayed 10 Enter the APPLIED NORMAL FORCE specified in Table 5 4 depending on the transducer in use ARES User Manual 215 Figure 5 6 Applying Normal Force Using the Calibration Weight 11 Select the Calibrate Now button When calibration is complete the Transducer Calibration form is displayed again 12 Verify that the Normal value displayed on the Transducer Calibration Form Figure 5 4 is within the limits for the NORMAL FORCE VALUE shown in Table 5 4 depending on the transducer in use Verify that the Current Normal Cal value displayed in the Transducer
176. ng the gap Manual Zero and Auto Zero For most applications the Auto Zero method is recommended The Set Gap Instrument Control function in Orchestrator is used to control the stage movement when zeroing and setting the gap If testing is to be done at temperatures other than ambient install the tool and then adjust the temperature to the desired initial value Allow the tools to reach thermal equilibrium before zeroing and setting the gap Manual Zero To manually zero and set the gap between upper and lower tools perform the following steps 1 Ensure that the upper and lower tools are clean and install them 2 Select the Set Gap Instrument Control function The Gap Instrument Control Panel is displayed 3 Zero the Torque and Normal Force by pressing the Offset Torque To Zero and Offset Force To Zero buttons 4 Using the slew rapid mode of the Manual Stage Control lower the stage until the distance between upper and lower tools is about 0 5 mm 5 Using the step slow mode of the Stage Control lower the stage until the Normal Force indicated on the Set Gap Instrument Control Panel just begins to deflect from zero indicating that the tools are in contact Zero the Gap value by pressing the Zero Indicator button under the displayed Gap 7 Raise the stage to a height that allows the sample to be loaded Sh The sample can now be loaded When the stage is lowered the Set Gap Instrument Control Panel displays the cor
177. nimum dynes cm 2 05E 02 High range eee 2 05E 00 Low range 1 02E 02 High range 2 22E 06 1 02E 00 Low range 5 11E 01 High range ESOO 5 11E 01 Low range 1 28E 01 High range 2 78E 05 1 28E 01 Low range 6 39E 00 High range 1 39E 05 6 39E 02 Low range 3 20E 00 High range 6 95E 04 3 20E 02 Low range Appendix Table A1 2 Complex Modulus Limits for Parallel Plate STD Transducer PLATE DIAMETER mm Gx Minima dwnaclem 1 02E 03 10K STD eee 5 10E 2 10K STD 2 56E 02 10K STD 6 40E 01 10K STD 4 09E 01 10K STD 8 1 60E 01 10K STD ARES User Manual 249 Appendix Table A1 3 Complex Modulus Limits for Parallel Plate 100 and 200 FRTN1 Transducers PLATE G Maximum dynes cm Gap mm y G MINIMUM dynes cm DIAMETER mm SAP mm at Frequency rad sec dy 9 84E 04 100 2 05E 00 High range 100 FRTN1 q EOS 010 4 10E 00 High range 200 FRTN1 10 2 05E 01 Low range 100 FRTN1 25 5 11E 0 0 lt 4 10E 01 Low range 200 FRTN1 4 92E 04 w 100 1 02E 00 High range 100 FRTN1 0 5 E 2 04E 00 High range 200 FRTN1 canis Aaa 1 02E 01 Low range 100 FRTN1 2 56E 07 lt 10 2 04E 01 Low range 200 FRTN1 6 15E 03 1 28E 01 High range 100 FRTN1 eae vod 2 66E 01 High range 200 FRTN1 1 28E 02 Low range 100 FRTN1 3 20E 06 2 66E 02 Low range 200 FRTN1 3 07E 03 w 100 6 39E 02 High range 100 FRTN1 05 edo 1 28E 01 High range 200 FRTN1 q 6 39E 03 L
178. nitial rate is the Final Shear Rate from the previous zone Zone Time Total time allotted to achieve the Final Shear Rate Direction Direction specifies the rotational direction of the actuator for positive Final Shear Rate values Thixotropic Loop Test Ei x Sampling Mode log Linear Paints Per one 200 Max 350 Min 20 Shear Rate Limits 17s Max 200 0000 Min 0 007 000 one Number 1 2 3 4 Final Shear Rate Meloo foo foo foo Zone Time s or hwag ooo oo mo IN Direction o f Clockwise Counterclockwise Options Delay Off Options End of Test Save As Help Cancel Figure 3 18 Thixotropic Loop Test Set Up Form Suggested Uses e Thixotropic Loop is used to determine material thixotropy or hysteresis This refers to the dependence of the material s response as measured by shear stress or viscosity to the previous strain rate history This in turn can be related to the build up or breakdown of structure in complex fluids ARES User Manual Options The following test option is available for use with Thixotropic Loop e Delay Before Test ARES User Manual Torque Normal Relaxation Functional Description Torque Normal Relaxation applies and maintains a single transient deformation step strain Data is then collected during each of four zones the duration of each can be selected Figure 3 19 Torque and normal force are monitored and reported during the test This is in contras
179. nsducers occcccccnnnnnnnn 218 Procedure for 100 FRTN1 200 FRTN1 100 FRT 200 FRT and 1K FRIN1 wee eeeeeseeeeeeeees 219 Sua Colorao ICC ooo EE E noises E Oa 220 Pole UN y IPP no o OOO N EE T 220 yate Che Us MIS a a 222 o geese once ac vsc tae see vec psec yee co E otecaeecceseae eerie 222 Tempera nie NON estan pacers a e E E 224 Temperature Calibration usin es Orchestrator asii a Na 224 khair GO Dane msn dida 227 Sos Mio e A A A PP E E A T 221 Route IV a NVC odo escent ects patente eee owe te cocacola ooi cesta 227 Cableand Hose Tns pecuarias 227 roo AP o A O A EN II E E 227 AIE FO SS ease sai POT E E EE E EE AE E E E E A 227 A LU T EEC E E E E E E E E eee 228 Caa N r trio 228 Line anda earra LV SES I Le inepto ae Ee SEARE SAE EA E E 229 EON tee os acta T E AER T T O O E E EE meee essen 229 Specii Mane Ba eea cara o e o E E E Seo cores 230 cervice and Repair ile deco AAA e o E E E 230 asnos LS iento bip rrr Tr cre 230 liga elol oiqta lo dieing 5 110 l APA REO o o ae eee ec en E 232 GEN 0 A ON o A ee eee ee E E A 232 Apera MO q Ao carseat der ets ceaaese ts stages E A 233 Daca bate treks ak E TO 239 Appen A Complex Modulas Tis anna sia 249 ARES User Manual Chapter I Introduction Overview This manual describes the following instrument specific features of the Advanced Rheometric Expansion System ARES The figure to the right shows the test station equipped with the Forced Convection Oven For information
180. nside the instrument while power is applied to the instrument ARES User Manual 207 Procedures Calibration Intervals Table 5 1 lists required calibration tasks and the recommended calibration interval for each task The table also shows when certain calibrations must be performed following repairs Table 5 1 Calibration Tasks and Recommended Intervals Torque Calibration Suggested Monthly Mandatory Following transducer replacement Normal Force Calibration Suggested Monthly Mandatory Following transducer replacement Phase Angle Check Suggested Monthly Mandatory Following transducer replacement When attempting to diagnose system problem Suggested Monthly Mandatory When attempting to diagnose suspected motor control system problems Strain Calibration Check ARES User Manual NEW STYLE CALIBRATION FIXTURE HUB ONE EITHER SIDE CALIBRATION FIXTURE new style PULLEY SHAFT new style Pully Wheel mounts here for 100 200 FRT 100 200 FRTN1 2K STD and 10K STD transducers On Pully Wheel mounts here for 1K FRTN1 NOTE this hole is not present on all Pully Shafts Pully Wheel mounts here for 2K FRT and 2K FRTN1 transducers OLD STYLE CALIBRATION FIXTURE Mount Hub here for 100 200 FRT 100 200 FRTN1 2K 10K STD Transducers PULLEY Mount Hub here for HUB KFRT 2K FRTN1 f Transducers CALIBRATION FIXTURE old style Figure 5 1 ARES Calibration Tools
181. nt When the commanded temperature has been achieved wait 20 to 30 minutes at the commanded temperature before starting the test to allow the bath and sample to stabilize 4 For normal applications set the Temperature Calibration Table to Default For critical temperature work the adjustable option can be used to enter calibration offsets for specific temperature setpoints Refer to the Orchestrator online Help for details on how to set up this feature PID Loop Setup When using environmental control systems errors between commanded and actual temperature are driven to zero by a PID Proportional Integral Derivative loop control system The PID loop settings Figure 2 39 affect how the bath settles at a set point temperature The values are affected by circulator fluid used as well as the circulator specifications As the bath reaches a setpoint there will typically be a few degrees of overshoot after which the temperature will oscillate a few times and then stabilize Typical stabilization times are 15 minutes to reach 0 1 C and 35 minutes to reach a temperature stable at 0 01 C By modifying the Proportional Band P coefficient less overshoot can be achieved but there will typically be more oscillations before the bath stabilizes so the overall stabilization time will be longer PID Setup Form Fla PID Temperature Control Setup Choose PID le ath Tool Temp Froportional Bard 0 75 A oo eee 0 5
182. nt Waveforms X REFERENCE Y REFERENCE 90 S STRAIN VECTOR F FORCE VECTOR Bs STRAIN PHASE SHIFT FROM REFERENCE FORCE PHASE SHIFT FROM REFERENCE B Phaser Diagram F FORCE VECTOR S STRAIN VECTOR O FORCE PHASE SHIFT Xp COMPONENT OF FROCE IN PHASE WITH STRAIN Ye COMPONENT OF FORCE 90 OUT OF PHASE WITH STRAIN X STRAIN AXIS REFERENCE Y STRAIN AXIS 90 xY C Phaser Diagram Referenced to Strain Figure 3 1 Dynamic Waveforms and Vectors ARES User Manual Documents Describing Instrument Software Operation The interface between you and the instrument is the TA Orchestrator software the latest generation of instrument operating software Operational procedures shown this manual are given using Orchestrator version 6 5 6 which is the software released with the instrument at the time of this manual publication However menu and function names may change without notice during subsequent software releases Please refer to the Orchestrator Online Help system for specific details regarding the software version you are currently running Comprehensive procedures concerning Orchestrator operation are provided in the two TA Instruments documents e Orchestrator Getting Started Guide TA Instruments document number 902 30010G This document included in the Orchestrator Setup Kit contains information on the operation of the system software e Orchestrator Online Help system
183. nta pipa apenas 33 ale Bou PM ccna sce o S 35 lion AA e o E E AA E E N OE A A T 35 ARES User Manual MIO poo 35 DEO Ch SCO urna pta 36 Motor OV e Patio E E Tne rena ee en ert eer 36 RS 37 no y ea E o cae E can cap E E E A T T A E EE ease 37 e aiie erara ao ie 37 sea ON ON E E E E A E E E A E 38 oae Rae AU EN N eea S T EE SR 39 Re nE ME AAB e A E E E E esa E N E eer 40 Ae aor bese EO EE aa E S A NE 41 Standard Transducers 2K STD and 10K STD ccccccccssseceeessneceesssecesseeseeeceseaaeeeseseaseeceseseeecsseeeesenseaaeees 41 FRT without Normal Force 100 FRT and 200 FRT ooooooocccnnonoccnonononnnonononnnonononnnnnnnnonnnononnnnnnnnnnnnnnnnnnonnnnnnnnnnnos 41 Procedure for Locking and Unlocking Air Bearings 100 FRT and 200 FRT oooncnncccccicanicinnnnninncananacinno 41 FRE vita Normal Force ERIN estriado 42 Procedure for Locking and Unlocking Air Bearings FRTN1 and FRIN1E oocnncnnccnccnccnnncnnonncnanacnnaninns 43 NOTE ORE TIN d Bearing Lock Olen ia WON esmero nc 43 High Resolution HR and High Torque HT Motor ocoococnnccconanoninnanononninnonancnnonanonnananonnn corona nean aS 45 Low henr ES Mora picas 45 Procedure for Locking and Unlocking Air Bearings LS MotOT conccnocnoconnnnnaninnnnnnnonanananccnncnnnonacnanccnnannaso 45 Test Staton Rear Input Late asin tado 47 al A e E ER E E O o open eee cea ingaeensose hance goes 47 gt A a AA o EE ooo E eee Meese ieeness 47 Nacio APP o o o E A A 50 Power OnneC ONS estancias
184. nterclockwice Directions Per Measurement O Onei Two Options Delay Ot Analoglr Off Options End of Test Save Az Help Cancel Figure 3 13 Steady Rate Sweep Test set Up Screen Suggested Uses This test is used to generate flow curves for samples by measuring the stress and viscosity as a function of shear rate This can be used to characterize the non Newtonian behavior of materials ARES User Manual 119 Options The following test options are available when using Steady Rate Sweep e Delay Before Test e Analog Data Input ARES User Manual Strain Controlled Transient Test Methods Step Shear Rate Functional Description Step Shear Rate is a steady transient test that applies a constant commanded shear rate for a selected time period Up to four separate zones can be programmed each with its own set of parameters Figure 3 14 A maximum of 350 data points can be sampled in each zone The interval between data points can be incremented either logarithmically or linearly Within each zone the following are then set Shear Rate Commanded shear rate in reciprocal seconds Entering a Shear Rate of zero prevents actuator movement during data collection allowing study of relaxation after steady shear Zone Time Total time during which Shear Rate is commanded Direction Direction specifies the rotational direction of the actuator for positive Shear Rate values Step Rate Test El x Sampling Mode Log
185. ntering the appropriate parameters as necessary If the specimen is a regularly shaped non flowing material you can also manually set the gap by continuing to lower the upper plate until only a slight force is generated The initial gap should be set approximately 0 05 mm above the final desired gap to facilitate sample trimming If the specimen is a gel or flowing material lowering the upper plate onto the sample will result in the specimen being distributed across the lower plate into a regular cylindrical geometry For this type of sample using the normal force limits helps to avoid damaging the sample as the sample may be rapidly compressed in a manual loading procedure with insufficient time for sample relaxation In either case the initial gap should be about 0 05 mm higher than the final desired gap Trim the sample flush with the edges of the plates NOTE Given the nature of materials used with this tool sample trimming may not be practical or possible In this case lower the tool to the final gap For liquid samples there is a catch well that will hold excess sample Lower the stage to the final gap setting Again this can be done manually or using the Set GaplInstrument Control function changing the entered gap to the desired final value The sample should bulge slightly Remove the cover clip and slide the cover down onto the glass chamber Fill the liquid seal well with an appropriate fluid for the sample material fol
186. nu and set up the instrument using the guidelines shown in Figure 2 19 Setup Instrument Options Temperature Control y Oven Air Chiller or LN Dewar 7 500 0 Figure 2 19 Setup Instrument Options Form Used to input the environmental system configuration NOTES 1 Make sure the following are selected e Instrument Setup TEMPERATURE CONTROL e Temperature Control OVEN AIR CHILLER OR LN2 DEWAR 2 Ensure that the maximum and minimum temperatures correspond to the desired allowable operating range Normally these are set to the instruments environmental system limits e Be sure to set cooling controller to LN2 if this optional feature is installed and used e Select the Temperature Loop Control option based upon Table 2 4 ARES User Manual Table 2 4 Oven Temperature Control Loop Options Temperature Temperature is Temperature Control Method is controlled reported by by 1 Oven Air Oven PRTs Tool PRT Gas entering the Oven is maintained at the commanded Temp both upper temperature Temperature is reported by the Lower Tool and lower PRT 2 Sample Tool PRT Tool PRT Oven temperature is maintained at the commanded Tool Temp temperature using the Lower Tool PRT Temperature is reported using the same PRT Tool PRT such as Torsional Rectangular test tools Tool PRT Lower Oven Oven temperature is maintained as in Mode 2 PRT Temperature is reported using the lower Oven PRT NOT NORMALLY USED WITH ARE
187. o plug on Main Fused 220VAC power input to the test Power Switch Station OVEN IN Connected to Oven 220VAC power input to the oven control circuitry N2 HEATER Connected to optional LN2 Power for the optional LN2 Controller Controller Main Power Switch The Main Power Switch Rear Panel switches power on and off to the main portion of Test Station Figure 2 14 The AC line fuse to the main portion of the test station is located below the power cord socket x WARNING The Main Power Switch does not remove power to the oven or LN2 Controller The main power cord 220V IN must be disconnected from the Power Panel to completely remove AC power from the system ARES User Manual 220V power connection from Power Panel Figure 2 14 Main Power Switch ARES User Manual Pneumatics Panel The Pneumatics Panel is where all gas connections are made adjusted and monitored This panel is located at the right rear corner of the Test Station This panel is unique in that it is a two sided panel and wraps around the Test Station from side to back Figure 2 15 shows both the side and back of the Pneumatics panel Gas Inputs Two gas inputs are available one for standard compressed air Air Supply MAIN and an optional port N2 GAS for other compressed gases The main air supply serves two very important functions It provides air to the transducer and motor air bearings Additionally it serves as a circulating medium for the gun
188. ocation of the gun heaters and two PRIs Table 2 4 contains a complete description of temperature control loop options ARES User Manual Chiller The Air Chiller extends the lower range of the oven to 60 C by use of mechanical refrigeration The Chiller is a single integrated package consisting of air filters air dryers and the refrigeration unit It is designed to connect directly to Test Stations equipped with a Forced Convection Oven The Chiller requires a separate air input line at 85 psi and 4 scfm Air is sent through the filter and air dryer and then is input to the refrigeration unit where it is chilled to 70 C The cold air is then sent on to the oven Connection The Chiller air output connects to the Forced Convection Oven Connect the signal cable from the Chiller to the LN2 port on the Signal Panel Figure 2 12 Plug the Chiller into the appropriate power source Installation should be performed by a qualified TA Instruments service technician software Configuration The Chiller operates using Orchestrator software The following sections discuss set up and operation of the oven including use of either the LN2 controller or Chiller Chiller Operation To operate the Chiller turn on the Polycold power switch located on the opposite side of the refrigeration unit as the air dryer J box and air filter and J box on off switch Figure 2 17 Verify that the pressure regulator gauge indicates 60 psi Adjust the pressur
189. odulus G that can be measured by each transducer type using the parallel plate geometry The following geometry specific factors affect the operating range of parallel plate geometry e Plate diameter strain constant K and stress constant Kx e Gap between plates strain constant K ARES User Manual 161 Additionally the following instrument specific factors affect the operating range of all geometries e Minimum torque that can be measured by the transducer e Transducer compliance e Maximum strain that can be generated by the motor To calculate the minimum and maximum G that can be measured by each transducer type using the parallel plate geometry use the following equation a Ks lc 4 1 o K Y where A Stress Constant K Strain Constant and C is computed from the following C for G MAXIMUM C for G MINIMUM 2K FRTN1 2K FRTN1E J 1 15e 06 rad gecm a an see note below 1K FRTN1 l J 4 9 e 06 see note below 2K STD 10K STD N J 2 60e 06 see note below 100 FRT for 100 J 2 60e 05 200 FRT a 100 FRTN1 for 0 10 J 2 60e 06 200 FRTN1 Za see note below for w lt 10 see note below NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination To determine the maximum or minimum complex viscosity n that can be measured at a given frequency
190. onger soak times to equilibrate Typical soak times are from 1 to 5 minutes The minimum soak time is zero seconds maximum 65000 seconds Dynamic Temperature Step Test El E Frequency f 0 0 rads Max 500 0 Min 1 00e 05 Initial Temp 25 0 PC Max B00 0 C Min 1 50 0 strain Limits 2 Max 31 25000 Min 0 003125 one Number 1 2 3 4 Final Temp E 50 0 200 0 0 0 0 0 Temp Increment C1 5 0 10 0 0 0 0 0 Soak Time sorhms ffag Bon fo fo e ipo feo foo foo Options PreShearcOff Delay Of AutoTens OF AutoStrn On MeasOpe Off Dk End of Test Save Ag Help Cancel Figure 3 5 Temperature Step Test Set Up Menu ARES User Manual 105 Suggested Use Temperature step tests are generally used to analyze the behavior of a sample as a function of temperature Temperature steps are preferred over the temperature ramp method if accurate isothermal data are needed This is because any sample thermal conductivity effects cause internal temperature gradients until the sample has had sufficient time to equilibrate at a given temperature Test Options The following test options can be selected for use with the temperature sweep e Steady PreShear e Delay Before Test e Analog Data Input e AutoTension e AutoStrain e Measurement Options o Delay Settings o Strain Amplitude Control ARES User Manual Dynamic Strain Sweep Functional Description Strain Sweep takes successive measurements at selected
191. or begins all tests at the motor zero position and drives symmetrically about motor zero at the chosen frequency to the commanded displacement strain The maximum angular deflection of the motor is 0 5 radians from either side of motor zero When in dynamic mode the instrument measures strain and torque In Steady Mode the motor can begin a test from any position rotating either clockwise or counterclockwise as specified at a specific rotational shear rate When in steady mode the instrument measures rotational rate sample torque and if equipped with the appropriate transducer normal force Transducers There are two types of transducers available for ARES The Force Rebalance Transducer FRT is an active type transducer and provides excellent resolution and temperature stability The Standard Transducer is a passive spring type transducer that provides high frequency response with the ruggedness desired by QC labs Several different ranges are available for each transducer type Force Rebalance Transducer with Normal Force FRTN7 The Force Rebalance Transducer with normal force FRTN1 consists of independent rotational torque and axial normal force servo control systems each utilizing position feedback to maintain the FRT shaft mass in contact with the sample in a null position when no force is applied When force is applied to the FRT shaft the servo control systems drive the shaft back to null position The electrical
192. or most applications However you may need to experiment somewhat to determine their baths best PID settings for their system or specific applications The Orchestrator ON Line Help has a complete description of how to determine and tune the PID coefficients Table 2 7 PID Values for the Julabo Circulator and Selected Fluids Julabo Circulator ES 18 50 Water PAPUG 50 Ethylene Glycol Proportional Band 0 75 Fluid Bath 2 Operating Requirements The Fluid Bath can operate only if the following conditions are met e The Fluid Bath is selected as the current environmental system e The circulator must be filled on and circulating fluid through the bath e The circulator must be connected to the test station via the correct RS 232 cable Fluid Bath 2 Operation The Fluid Bath is operated using the Instrument Control Panel Figure 2 27 The desired temperature is set in the Temperature input field For most applications especially isothermal testing or when the actual tool temperature is required Tool Temperature control is used For temperature ramp tests where a steady ramp rate is most important the circulator control gives better results If using manual temperature control for isothermal testing you may have to adjust the circulator fluid temperature somewhat to give the desired temperature at the tool ARES User Manual Instrument Control Panel Figure 2 27 ARES User Manual p50 Bath Instrument Controlle
193. ormal force and torque on the motor using the Offset Normal Force to Zero and Offset Torque to Zero buttons 4 Zero the gap using the Zero Indicator button in the Set Gap Instrument Control function Using a Maximum Allowed Force of 100 gm works well Using the Set Gap Instrument Control function set the Gap to 1 mm 6 Raise the stage to provide sufficient room for sample loading m Sample Loading Fluid Bath 2 The nominal sample volume is between 8 to 9 ml For lower viscosity fluids a volume closer to 9 ml is optimal For higher viscosity fluids using a volume closer to 8 ml gives good results In all cases the fluid level must be at least up to the sample fill level lip To avoid edge and boundary layer errors filling slightly past the lip is desirable as shown in Figure 4 18 Overfilling the sample however especially in the case of higher viscosity fluids may result in errors due to an actual wetted bob length longer than the entered effective length Carefully pour the sample into the cup making sure not to spill sample into the recess that holds the inner cup mounting screw A small graduated cylinder can be used to transfer material into the Couette as well as a syringe or pipette In any case a consistent sample volume from sample to sample is desirable for each material tested After filling the cup return the bob back to the 1 mm gap This will ensure that the nominal bob length is the correct 32 mm ARES
194. ote below 100 FRT e au These transducers are not recommended 200 FRTN1 for use with the torsion rectangular tool NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 for a sample of fixed length and width and the minimum and maximum thicknesses the tool can accommodate 2 Generate an X Y scatter plot of sample thickness Y axis versus complex modulus G X axis The region between the upper and lower limits of operation is the range of complex modulus that can be tested Coefficient of Thermal Expansion a When testing at other than ambient temperatures the coefficient of thermal expansion for Torsion Rectangular geometry is defined as AL 1 At Ly where Coefficient of Thermal Expansion aa At Change in temperature C Lo Original length of sample mm AL Change in length of sample mm Positive AL indicates increasing sample length ARES User Manual Tool Installation 1 Select the Set Gap Instrument Control function under the Control menu in Orchestrator Use the Send to Top button to rai
195. ote below max a i au for 100 J 2 60e 05 7 form 10 J 2 608 06 100 FRTN1 200 FRIN1 NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination To determine the maximum or minimum complex viscosity N that can be measured at a given frequency use the following formula n 42 a ARES User Manual 191 where n Complex viscosity Poise G Complex Modulus dynes cm Frequency rad sec Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 2 Substitute the G MAXIMUM value into equation 4 2 then determine the upper limit of operation by calculating N at each O O values chosen to be from the lowest to highest frequencies within the transducer operating range 3 Substitute the G MINIMUM value into equation 4 2 then determine the lower limit of operation by calculating 1 at each 4 Generate an X Y scatter plot of complex viscosity N Y axis versus frequency X axis The region between the upper and lower limits of operation is the range of complex viscosity that can be tested Appendix 1 contains tables of G values for some combinations of bobs
196. ote that this tension level is a general recommendation only and you should set the tension level according to the sample characteristics with thinner and or lower modulus materials requiring less axial force When using the AutoTension feature adjust the stage so that the normal force is zero a ARES User Manual 181 10 Using the Motor Position Offset slider in the Set Gap Instrument Control function in Orchestrator adjust the motor position until the displayed torque is zero DO NOT use the Offset torque to Zero button 11 Read the gap and record this distance as the sample length 2K FRT transducers only 12 Use the Hold function under the Control pull down menu when changing temperature Setting Anvil Sliding Clamp Centering Lines Nominal Clamping Thickness Shown on This Face Adjusting Screw Figure 4 10 New Torsion Rectangular Tool Details 182 ARES User Manual SIDE VIEW NOTE Each Setting Anvil is designed to clamp two different thickness ranges The Anvil should be mounted as shown below with the desired nominal thickness on the outside face The number on the face that actually touches the sample is NOT the clamp thickness in use SETTING ANVIL CENTERING LINES Seed iididiil J aa i TOP VIEW LOWER FIXTURE The number shown on this face of the Setting Anvil is the Nominal thickness the fixture will properly clamp on UPPER FIXTURE
197. ow 1K FRTN1 0 J 4 9 e 06 see note below 2K STD 10K STD i J 2 60e 06 see note below 100 FRT for 100 J 2 60e 05 200 FRT ON 100 ERTN1 for 0 10 J 2 60e 06 200 FRTN1 2 see note below for w lt 10 see note below NOTE The values for M gecm and 6 rad are found in the specification tables in Chapter 1 Table 1 6 through Table 1 13 Pick the correct values for your specific transducer and motor combination 174 ARES User Manual To determine the maximum or minimum complex viscosity N that can be measured at a given frequency use the following formula nea 4 2 q where n Complex viscosity Poise G Complex Modulus dynes cm Frequency rad sec Using a spreadsheet application such as Microsoft Excel you can use the equations above to plot the range of complex viscosity that can be tested for a given geometry transducer combination as follows 1 Calculate G MAXIMUM and G MINIMUM using equation 4 1 2 Substitute the G MAXIMUM value into equation 4 2 then determine the upper limit of operation by calculating N at each O O values chosen to be from the lowest to highest frequencies within the transducer operating range 3 Substitute the G MINIMUM value into equation 4 2 then determine the lower limit of operation by calculating N at each 4 Generate an X Y scatter plot of complex viscosity N Y axis versus frequency X axis The region between the upper and low
198. ow range 100 FRTN1 1 60E 06 w lt 10 1 28E 02 Low range 200 FRTN1 Appendix Table A1 4 Complex Modulus Limits for Parallel Plate 100 and 200 FRT Transducers PLATE G Maximum dynes cm GAP mm y G Minimum dynes cm DIAMETER mm Gae mm at Frequency rad sec al 9 84E 04 w 100 1 02E 00 High range 100 FRT 1 84E 4 2 04E 00 High range 200 FRT tii po 1 02E 01 Low range 100 FRT 25 9 11E 07 0 lt 2 04E 01 Low range 200 FRT 4 92E 04 w 100 5 11E 01 High range 100 FRT 1 02E 00 High range 200 FRT 4 92E 1 eo E 5 11E 02 Low range 100 FRT 2 56E 07 w lt 10 1 02E 01 Low range 200 FRT 6 15E 03 6 39E 02 High range 100 FRT 6 15E 04 1 28E 01 High range 200 FRT 6 39E 03 Low range 100 FRT 3 20E 06 1 28E 02 Low range 200 FRT 3 07E 03 3 20E 02 High range 100 FRT 3 07E 04 6 40E 02 High range 200 FRT 3 20E 03 Low range 100 FRT 1 60E 06 6 40E 03 Low range 200 FRT ARES User Manual Appendix Table A1 5 Complex Modulus Limits for Cone and Plate 2K FRTN1 and 2K FRTN1E Transducers PLATE DIAMETER CONE ANGLE G MAXIMUM G MINIMUM mm e dynes cm dynes cm 9 59E 01 high range 2 08E 06 9 59E 01 low range 1 92E 01 high range 4 17E 05 4 996 01 low range 3 84E 01 high range eile 3 84E 01 low range 2 40E 00 high range lt a 5 21E 04 5 40E 02 low range 4 79E 00 high range 1 04E 05 4 79 02 low range Appendix Table A1 6 Complex Mo
199. perature step test Figure 3 5 you can enter a test frequency and an initial or starting temperature Next you can enter each individual zone final temperature step size soak time and strain Testing limits are displayed for each of these fields When setting strain values in this test be aware that the sample modulus can change significantly with temperature and the torque signal generated at a given strain may vary dramatically A strain that provides good torque and is within the linear viscoelastic region at room temperature may overload the transducer at lower temperatures Single point tests at the temperature extremes are a good way to find the appropriate strains to set for each zone The AutoStrain adjustment is also a good option for optimizing the torque generated in this test Note that when AutoStrain is used it is possible to have the current strain propagate into a new zone by entering a value of zero for the strain Inherit feature The final temperature can be any temperature within the range of the instrument and there is no limitation on step size Data Measurement Method Each measurement is equivalent to a data point For example changing temperature from 10 to 100 in 10 steps produces 10 data points Making the same temperature change in 5 steps results in 19 data points Soak time should be chosen with consideration given to sample volume and temperature increment Larger samples and larger step sizes require l
200. r In particular any and all warranties of merchantability fitness for a particular purpose or non infringement of third parties rights are expressly excluded Further TA Instruments makes no representations or warranties that this software and documentation provided are free of errors or viruses or that this software and documentation are suitable for your intended use LIMITATION OF LIABILITY In no event shall TA Instruments or its suppliers be liable to you or any other party for any incidental special or consequential damages loss of data or data being rendered inaccurate loss of profits or revenue or interruption of business in any way arising out of or related to the use or inability to use the software described above and or documentation regardless of the form of action whether in contract tort including negligence strict product liability or otherwise even if any representative of TA Instruments or its suppliers has been advised of the possibility of such damages This LICENSE represents the entire agreement concerning the software described above between you and TA Instruments It supersedes any prior proposal representation or understanding between the parties The Oracle software used in conjunction with the Advantage Integrity software is not included as part of the TA Instruments Advantage Integrity license agreement Users of Oracle database software must abide by the terms and conditions as specified by the Oracle Co
201. r zones A programmable thermal soak time at the end of each zone ensures temperature stability prior to beginning the next ramp When setting up a temperature ramp test you enter a test frequency and an initial or starting temperature Next you enter each individual zone final temperature ramp rate i e 2 C min 5 C min etc soak time and strain When setting strain values in this test be aware that the sample modulus can change significantly with temperature such that the force generated at a given strain may vary dramatically at different temperatures A strain that provides good force and is within the linear viscoelastic region at room temperature may overload the transducer at lower temperatures Single point tests at the temperature extremes are a good way to find the appropriate strains to set for each zone The AutoStrain adjustment is also a good option for optimizing the force generated in this test Note that when AutoStrain is used it is possible to have the current strain propagate into a new zone by entering a value of zero for the strain Inherit feature Frequency and initial temperature are entered first Figure 3 7 and then the following parameters are entered for each zone Final Temperature Final temperature is the temperature at which the instrument stops ramping temperature while in the respective zone The final temperature is independent of time Ramp Rate Ramp rate is the rate of change positiv
202. r Displacement is incorrect Ensure that correct geometry is entered Ensure that the desired strain is entered Verify that the diagnostic LEDs are lit Call Technical Service Motor oscillates with an accompanying high Ensure sample is not too stiff pitched audible noise when running a test Call Technical Service OVEN AND LN2 CONTROLLER Can not turn on the oven If air is being used as an input to the heaters ensure that the Orchestrator AIR LOW indicator is not on If itis the air supply to the oven has been interrupted Restore air flow If using the LN2 Controller ensure that The LN2 supply is adequate and the valve is open The LN2 READY indicator is on The LN2 FAULT indicator is off if on go to 7 Ensure that the oven door is closed and the OVEN OPEN indicator is not on Ensure that the reported temperature is not constantly above 650 C If itis there is an open in the PRT electrical circuit Go to 8 Ensure that the SET USER TEMPERATURE LIMIT is set to a reasonable value Ensure that the instrument MAXIMUM TEMPERATURE is set to a reasonable value An oven or heater fuse may be open Check and replace Call Technical Service ARES User Manual 233 Table 6 2 Instrument Operation Troubleshooting Guide Continued PROBLEM CORRECTIVE ACTIONS Oven can be turned on but does not heat Oven can be turned on but is not correctly heating No LN2 READY indication Orchestrator 1 2
203. r a single decade of rate from 10 to 100 reciprocal seconds 1 s Selecting five data points to be measured per decade divides the difference of the endpoint logarithms into five equally spaced fractional exponents Six discrete rates are generated in succession by taking the antilogarithm of each exponent e Initial Rate 10 1 sec e Decade Rates 15 9 25 1 39 8 63 1 1 sec e Final Rate 100 1 sec One data point is measured at each of the rates Discrete The discrete rate sweep generates up to five shear rates in succession Each shear rate is entered into a Zone Data Collection Mode Data can be collected in either time based mode one measurement is taken at each rate or manual mode one measurement is taken at selected rate Time Based Following the start of the test Time Based data collection takes one measurement at each rate Setting the Sweep Mode to Log commands logarithmically incremented shear rates A Discrete Sweep Mode commands up to five unique shear rates in succession At each shear rate Measurement Time is the period during which data are collected At each shear rate Delay Before Measure is the time period between command of the current rate and the beginning of data collection ARES User Manual Manual Mode Following the start of the test Manual Mode data collection takes a single measurement when commanded to do so Manual Mode operation is as follows e Start the test e When desired start t
204. raphically and provide the option to download directly into the instruments waveform memory Any subsequent change to the equations or Wave Time fields requires recalculating and re sending the waveform The software keeps track of any new changes and when the test is started reminds you to resend the waveform if necessary The Zone 1 through Zone 4 times as displayed on the host computer refer to data collection time and are independent of the wave playback times That is the waveforms will be played back one immediately after the other based on their entered Wave Times and not on the data collection Zone times It is possible to playback more than one waveform in a Zone or play an equation across Zones Once all the waveforms have been played the motor will stop movement but the software will continue to acquire data until the end of the last entered data collection Zone time Consider the following example Equation One Wave Time 10 seconds Equation Two Wave Time 15 seconds Zone 1 acquisition time 20 seconds Zone 2 acquisition time 10 seconds Data will be collected in Zone 1 for the entire Equation One playback duration Wave Time of 10 seconds As soon as Equation One finishes Equation Two will start playing with data still being collected in Zone 1 Ten seconds later Equation Two still playing data collection will end in Zone 1 and will data collection will start in Zone 2 After five more seconds Equation Two will fin
205. re or the temperature at which the sample was loaded the clamps on some tools may loosen as they cool This is due to difference in the thermal expansion coefficients of the sample and that of the tools Immediately prior to initiating testing at the lowest test temperature you may wish to open the oven door and verify that the screws securing the clamps are tight taking care not to touch any surface of the oven or tools which may be at dangerous cryogenic temperatures ARES User Manual Parallel Plates Strain Constant Stress Constant 2000 G K 2 al Y H i TR Variables G Gravitational Constant 980 7 cgs or 98 07 SI R Radius of plates mm H Gap between plates mm Options 8 25 40 50 mm sizes Serated plates Disposable plates Invar Plates Environmental Systems Ambient Oven Fluid Bath Fluid Bath 2 Peltier Parallel Plate Tool see Chapter 2 for more details regarding lower tool General Information Parallel Plates are used to test polymer melts soft solids and higher viscosity fluids Using disposable plates they are used for testing thermosetting resins and epoxy curing The wide range of sizes use over a wide range of viscosities variable gap and ease of loading make them a very versatile tool Additionally high shear rates are accessible using a small gap setting Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex m
206. rect distance between tools ARES User Manual 157 Automatic Zeroing and Gap Setting The Set Gap Instrument Control Panel function allows you to automatically zero and set the gap between upper and lower tools Zeroing the Gap Establish a zero reference gap between Upper and Lower tools as follows 1 Ensure that a sample is not loaded and the upper and lower tools are clean 2 Using the Manual Stage Control lower the stage to achieve a Gap of about 1 mm as judged visually 3 Select the Set Gap Instrument Control Panel function The Set Gap Instrument Control Panel dialog box is displayed 4 Zero the Torque and Normal Force by pressing the Offset Torque To Zero and Offset Force To Zero buttons 5 Click Zero Tool An information form is displayed showing the duration Elapsed Time of the zeroing operation The present gap is displayed in the Current Gap field which updates at one second intervals The following events occur during the zeroing operation a The stage lowers to achieve contact between tools b Following contact the Gap display is zeroed 6 In preparation for loading the sample raise the stage to maximum height by clicking Send to Top Remain in the Gap Control Panel and proceed to the next topic Setting the Gap Setting the Gap After zeroing the Gap set it as follows 1 Place the sample onto the lower tool 2 Enter the following information a Commanded Gap Position Enter the desired
207. response Manual settings can be adjusted as shown in Figure 3 29 Correlation Delay Correlation delay is the time period between the start of sample deformation and the first measurement in a dynamic test During this period the instrument does not collect data Note that data collection is delayed not motor movement Correlation delay allows the sample to achieve equilibrium with the test conditions before the measurement is taken and allows development of the phase angle from the start of stress and strain sine waves Internally the instrument computes the correlation delay in seconds with a minimum increment of 0 1 second and a minimum time period of 0 2 second The number of cycles to which this corresponds varies depending upon the frequency The maximum allowable time period is 65 000 seconds One Cycle Correlation The One Cycle Correlation option speeds the test by commanding the control computer to use data measured over one cycle regardless of test frequency Normally at frequencies above 2 rad sec data are collected over multiple cycles and averaged One Cycle Correlation forces measurements to be made with only on cycle worth of data saving the time that would be required for the subsequent cycles One Cycle Correlation is useful for applications requiring fast measurements such as sample curing at high frequencies The disadvantage is that due to the absence of data averaging resulting data points may contain more noise than
208. rmulas All formulas and geometry constants are also listed in Orchestrator Online Help see Reference Guide under the Contents tab Dynamic Measurement Formulas Table 4 1 Dynamic Measurement Formulas VARIABLE AND FORMULA DEFINITION OF VARIABLES 204 STRESS Kz M STRAIN Ky 8 ELASTIC STORAGE MODULUS cos 0 a Yy VISCOUS LOSS MODULUS sin E Y COMPLEX MODULUS BP 6 LOSS TANGENT REAL PART OF DYNAMIC COMPLEX VISCOSITY G 0 IMAGINARY PART OF DYNAMIC COMPLEX VISCOSITY G 0 Stress Constant Torque g cm Strain Constant Shearing angle of motor radians Phase angle phase shift between stress and strain vectors Frequency angular in rad sec ARES User Manual Table 4 1 Dynamic Measurement Formulas Continued VARIABLE AND FORMULA DEFINITION OF VARIABLES n DYNAMIC COMPLEX VISCOSITY Steady and Transient Measurement Formulas Table 4 2 Steady and Transient Measurement Formulas STRESS K Stress Constant Kz M Torque g cm STRAIN Strain Constant K 0 Shearing angle of motor radians y STRAIN RATE SHEAR RATE Strain Constant Angular velocity of motor radians sec n VISCOSITY N NORMAL STRESS Kz Normal stress constant Ger F Normal force g ARES User Manual 205 Table 4 3 Strain and Stress Constants Strain Constant K Stress Constant K Parallel Plates Cone and Plate Feroe canghlar TOR IATIW LW L
209. rporation ARES User Manual Trademarks and Patents The following references apply to the information presented in this document TA Instruments Trademarks O Series is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Advantage Integrity is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Modulated DSC and MDSC are registered trademarks of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Tzero is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 pTA is a registered trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Smart Swap is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Hi Res is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Mobius Drive is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 Orchestrator is a trademark of TA Instruments Waters LLC 109 Lukens Drive New Castle DE 19720 TA Instruments Patents Method and Apparatus for Modulated Differential Analysis MDSC describes proprietary technology patented by TA Instruments Waters LLC U S Patent Nos 5 224 775 5 248 199 5 346 306 Additional Patent Nos CA 2 089 225 JP 2 966 691 and BE DE EP GB IT NL 0559362 Heat Flux Differential Scanning Calorimeter Sensor Tzero de
210. rque on the motor using the Offset Normal Force to Zero and Offset Torque to Zero buttons Using the stepper control buttons lower the stage to a point where the tools are close but not touching Use the Zero Fixture button in the Set Gap Instrument Control function to determine the zero point for the test tools Raise the stage to provide sufficient room for sample loading Sample Loading The recommended gap setting for parallel plates is between 0 5 and 2 millimeters Figure 4 4 shows parallel plates with sample loaded 1 2 Place the sample on the lower plate Ensure that the sample is centered on the tool Using the stepper motor buttons on the right side of the test station adjust the sample gap until the upper plate is close to the specimen Set the gap using the Set Gap Instrument Control function entering the appropriate parameters If the specimen is a regularly shaped non flowing material you can also manually set the gap by continuing to lower the upper plate until only a slight force is generated The initial gap should be set approximately 0 05 mm above the final desired gap to facilitate sample trimming If the specimen is a gel or flowing material lowering the upper plate onto the sample will result in the specimen being distributed across the lower plate into a regular cylindrical geometry For this type of sample using the normal force limits helps to avoid damaging the sample as the sample may be rapidly co
211. rted as gap Instrument Gap Measurement versus time Force Gap Test E E Force Sample Gap tofo mrn Gap Adjustment Time i ad e or Fem s Temperature 25 0 PC Ma 500 0 Min 1 50 0 Save Test Data Save As Help EA Figure 3 20 Force Gap Test Set up Screen Suggested Uses This test is useful during test sequences as it can be inserted into the sequence to effect a controlled gap adjustment between tests This test is also good for sampling loading It allows for documentable consistent sample loading and will minimize damage to or axial force on a sample during loading Test Options There are no options available with this test ARES User Manual Steady Step Rate Temperature Ramp Description Steady Rate Temperature Ramp monitors material stress and viscosity as a function of time at a series of specified shear rates within up to eight independently programmable zones Within each zone you can ramp temperature at a selectable rate upward or downward from the initial temperature Figure 3 21 In each zone specifying Log sampling takes the specified number of data points at logarithmically incremented intervals Selecting Linear takes the specified number of data points at linearly incremented intervals A maximum of 350 data points can be taken in each zone In Each Zone the Final Temp is the Temperature at which the instrument stops ramping temperature while in the respe
212. rument Control Button Gap Instrument Control 3 Gap mm 117 47 Send to Top eno Indicator Gap Command Commanded Gap mm i 050 Max allowed Force gm li FOO Set Gap ero Fixture Torque gr cm Offset Force To Zero Status Ton Motor Wn Reset eid Remove ero Offset Motor Position Offset 4 F 5 k 0 00 Advanced Help Exit Figure 2 4 Set Gap Instrument Control function main input form ARES User Manual Stage Rate Adjustment Both the operator controlled step rate and slew rate of the stage can be adjusted through the Advanced Control form shown in Figure 2 5 Click the Advanced button in the Set Gap Instrument Control function main form to access the Advanced Control form Adjust the step speed and slew speed as desired Automatic stage movement rates initiated using the Send to Top and Set Gap buttons cannot be adjusted The Front Panel LCD contrast is also adjusted from this dialog box Advanced Control Figure 2 5 Advanced Control Form of the Gap Instrument Control Function ARES User Manual 39 Front Panel LCD Display The front Panel LCD Display Figure 2 6 is used to display certain instrument status information For the ARES temperature gap torque and normal force are displayed The LCD display can be turned on and off from the Advanced Control form of the Set Gap Instrument Control function Figure 2 5 ARES TEMP 22 4 C
213. s may undergo relatively large dimensional fluctuations as a result of temperature changes AutoTension or AutoStrain may be necessary to adjust for temperature related changes Other Factors Other factors that will cause errors include sample edge failure sample buckling and sample slippage or clamping problems Care should be taken to load the sample properly determine it s proper testing range and when needed apply AutoTension correctly ARES User Manual 153 General Test Tool Installation WARNING If this instrument is used in a manner not intended or specified in this manual the protection provided by the instrument may be impaired Upper Tool Installation To install an upper tool loosen the knob on the anvil Figure 4 1 and insert the tool into the anvil pulling apart the retainers if necessary Tighten the knob Hand tighten the knobs do not over torque them Lower Tool Installation Motor Mount Oven or Ambient To install a lower tool onto the motor refer to Figure 4 2 while performing the following steps 1 If the tool accepts a PRT install the tool PRT as follows a Place do not push the plug onto the electrical jack mounted in the motor anvil b While applying light downward force rotate the tool PRT until it slips into place indicating that the PRT has aligned with the keyway in the electrical jack When properly installed Orchestrator will indicate ambient temperature 2 Loosen the knob on the
214. sample thickness ranges which are listed on the next page ARES User Manual 177 Sample Dimensions To prepare samples that fit within the physical constraints of the tool use the following guidelines e Maximum Sample Width 12 7 millimeters e Typical Sample Length 45 millimeters e Sample Thickness depends on the size of the setting anvil used SETTING ANVIL NOMINAL THICKNESS ACTUAL SAMPLE THICKNESS STAMPED ON FACE CLAMPING RANGE 1 5 to 2 5mm Clamping Torque Always use the correct size setting anvil for the sample thickness If the sample does not fit properly in the tool erroneous data may result Adjusting the sliding clamps to the proper tightness is imperative A torque screwdriver is included with this tool For each material some experimentation may be required to find the best clamp torque value to obtain good results Under tightening or for softer materials over tightening the clamps will result in erratic data Once a good torque value is obtained for a specific sample material and thickness all subsequent samples should be tightened to the same value Also both clamps should always be tightened to the same torque value NOTE Loading soft samples or samples that do not properly fit the clamps can result in inaccurate data Operating Ranges Operating range is defined as the region bounded by the maximum and minimum complex modulus G that can be measured by each transducer type using the torsion rectangular
215. scribes proprietary technology patented by TA Instruments Waters LLC U S Patent No 6 431 747 Method and Apparatus of Modulated Temperature Thermogravimetry MTGA M5 describes proprietary technology patented by TA Instruments Waters LLC U S Patent Nos 6 336 741 and 6 113 261 Modulated Temperature Thermomechanical Analysis describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 6 007 240 Method and Apparatus for Parsed Dynamic Differential Analysis describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 5 474 385 and EP Patent No 0701122 Method and Apparatus for AC Differential Thermal Analysis describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 5 439 291 continued on next page ARES User Manual 5 TA Instruments Patents continued Method and Apparatus for High Resolution Analysis of the Composition of a Material describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 5 368 391 and 5 165 792 Additional Patent Nos CA 2 051 578 and DE EP FR GB IT 0494492 Method and Apparatus for Thermal Conductivity Measurements describes proprietary technology patented by TA Instruments Waters LLC U S Patent No 5 335 993 and EP Patent No 0634649 Dynamic and Thermal Mechanical Analyzer Having an Optical Encoder with Diffraction Grating and a Linear Permanent Magnet Motor describes
216. sducer is a STD transducer go to step 19 a Access the Set Transducer Characteristics form Figure 5 7 by selecting the Transducer option from the Service function of the Utilities pull down menu b Divide the displayed Torque Calibration Value for the high range transducer by 10 then enter this value into the form as the Torque Calibration Value for the low range transducer For the 1K FRTN1 transducer only divide the high range Torque Calibration Value by 50 and enter this value for the low range transducer setting 19 Click Ok Proceed to the Normal Force Calibration if desired If Normal Force Calibration is not to be performed remove the calibration tool weight and pulley and store them in the calibration kit This concludes the Torque Calibration Table 5 3 Torque Calibration Weights Applied Torques and Full Scale Values CALIBRATION TORQUE CALIBRATED FULL TRANSDUCER WEIGHT TORQUE VALUE SCALE VALUE applied displayed computed 2K FRIN1 200 grams 500 gecm 500 2 gecm 2100 5 2K aaa E p n 613 01221 498 to 502 1995 to 2205 2K STD 1K FRTN1 200 grams 500 gecm 500 1 gecm 1050 5 p n 613 01221 499 to 501 997 5 to 1102 5 100 FRTN1 20 grams 50 gecm 50 0 1 gecm 105 5 100 FRT p n 613 02775 49 9 to 50 1 99 75 to 110 25 200 FRTN1 20 grams 50 gecm 50 0 2 gecm 210 5 200 FRT p n 613 02775 49 8 to 50 2 199 5 to 220 5 10K STD Two 1000 gram 5000 gecm 5000 10 gecm 10 500 5 p n 6
217. se the stage to the loading position 2 Verify that the motor is on and in dynamic mode 3 Mount the upper and lower tools on the actuator shafts 4 Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset torque to Zero buttons 5 Using the stepper control buttons lower the stage to a point where the tools are close but not touching 6 Use the Motor Position Offset button in the Set Gap Instrument Control function to ensure that the upper and lower tool openings are aligned 7 For 2K FRT transducers only skip this for STD transducers use the Zero Fixture button in the Set Gap Instrument Control function to bring the tools together and determine the zero point for the test tools 8 Raise the stage to provide sufficient room for sample loading Sample Loading This procedure is for use with 2K FRT and STD transducers only Refer to Figure 4 12 during the following procedure 0 WARNING POSSIBLE PERSONAL INJURY POSSIBLE DAMAGE TO INSTRUMENT This is a high torque motor Turning on the motor while in dynamic mode causes the motor to snap to dynamic zero position at a high velocity This can cause severe damage to the transducer and or personal injury To avoid damaging yourself and the transducer Never turn on the motor while a sample is loaded Keep hands clear of the motor 1 Measure and record the following sa
218. seal degradation and corrosion 80 ARES User Manual Peltier Configuration in Orchestrator When you command a temperature Orchestrator software uses the Instrument Configuration to determine the environmental system currently in use and establish operating conditions Prior to operating the fluid bath access the Instrument Configuration function located under the Service function of the Utilities menu and set up the instrument using the guidelines shown in Figure 2 31 Setup Instrument Options Temperature Control na Peltier Thermopile heat pump E 150 0 30 0 ol Figure 2 31 Setup Instrument Options form used to input the Peltier system configuration NOTES 1 Make sure the following are selected e Instrument Setup TEMPERATURE CONTROL e Temperature Control PELTIER THERMOPILE HEAT PUMP 2 Ensure that the maximum and minimum temperatures are set as follows e Maximum Temp 150 C e Minimum Temp 30 C 3 For normal applications set the Temperature Calibration Table to Default 4 For critical temperature work the adjustable option can be used to enter calibration offsets for specific temperature setpoints Refer to the Orchestrator online help for details on how to set up this feature ARES User Manual PID Loop Setup When using environmental control systems errors between commanded and actual temperature are driven to zero by a PID Proportional Integral Derivative loop control system Th
219. sed to ensure consistent fluid volumes from sample to sample The well is filled through the hole in the center of the cover fill port in Figure 4 8 Even though a low viscosity fluid is used it can affect the test Basically the sealing fluid can act like a sample For the most demanding work it may be desirable to run preliminary tests on just the sealing fluid to ARES User Manual determine its characteristics Once the sealing fluid influences are known they can be removed for the sample data To determine the effect of the sealing fluid set up the tool exactly as if you were running a sample but without actually loading a sample For these tests air will be the sample Set the gap to the intended setting and fill the sealing well with the desired volume of the chosen sealing fluid Run the actual tests that you are going to use on your real samples The results are then used to correct the real sample data Use with the Oven When using the Hastelloy tool with the oven some minor modifications to the oven may be necessary to facilitate sliding the oven past the tool Referring to Figure 4 7 shave the edge of the oven foam to allow the oven to slide past the tool during opening and closing Only a small amount of material should need to be removed approximately 1mm While adjusting the clearance be careful that you do not force the oven or tool to the point that either is damaged Also pay attention to the position of the PR
220. st Set up Screen ARES User Manual 123 Suggested Uses Suggested uses of strain relaxation are as follows e Determination of time required for a sample material to relax after a deformation as in sample material loading e Analysis of time dependent behavior of a sample Test Options e Delay Before Test e Steady Preshear e Analog Data Input ARES User Manual Multiple Extension Mode Functional Description Multiple Extension mode offers four zones in which a variety of separate extensional test types can be performed The mode of extension can be based on linear rate Hencky strain rate related to the specimen geometry force imposed to create the extension or as a compressive Rim Shear mode also known as squeeze flow The set up screen for multiple extension mode Figure 3 16 requires you to select a zone time for each zone This is the time in seconds minutes hours over which the test type will occur in each zone The extensional value units are dependent upon the test mode selected Several different test options are available in this mode Any test type can be combined in any sequence during a multiple extension mode test A fifth test type selection that is available is End Test which halts the series of extensional mode testing Table 3 4 provides a summary of the different test types available and the uses of each of them Multiple Extension Mode Test kE x Temperature 25 0 PC Max 500 0 C Min 150
221. strator software HOST is connected to the Host Computer serial communications port COM1 Communications interface between the optional fluid bath environmental control CIRCULATOR circulator and the instrument RS 232 Accepts a communication link that uses RS 232 protocol used with OAM2 and DETA options OVEN Electrical interface between the oven switches and temperature sensors and the instrument Connected to the oven ARES User Manual HOST Power Panel For Test Stations equipped with an oven the Power Panel serves three functions 1 Electrical power interface for the Test Station 2 Electrical power interface to the oven 3 Electrical power interface to the optional LN2 Controller For Test Stations without an oven the power panel is not required Main power plugs directly into the Main Power Switch shown in the next section Figure 2 13 identifies the Power Panel connectors 220V IN 0 O oO OVEN N IN HEATER o o O o 000000000000000000000000 000000000000000000000000 00 000000000000 0000000000 000000000000000000000000 00000000 0000000000000000 O Figure 2 13 Power Panel ARES User Manual Power Connections Power connections for the system are made as outlined in Table 2 2 Input power requirements are 220 VAC 20A 50 60 Hz Table 2 2 Power Panel Connectors 220V IN 220 Volt input power supplied Main power to the system by customer 220V OUT Connected t
222. t into the linearity of the measurement After all frequency components are specified the implementation of single point measurement test and temperature ramp differ The MultiWave Temperature Ramp test requires additional input to specify up to eight zones of temperature control See the section on the Temperature Ramp Test for more information Once the strains and frequencies have been specified the resulting waveform must then be downloaded into the instrument The Wave button is used to compute the resulting waveform display the results graphically and provide the option to download directly into the instruments waveform memory Any subsequent change to the strain or frequency parameters requires recalculating and re sending the waveform The software keeps track of any additional changes and when the test is started reminds you to resend the waveform if necessary Hult ave Single Point Test H E Fundamental Frequency Frequency sof rad s Max 2 0 Min 1 00e 05 Strain 0 1 Max 31 2 5000 Min 0 003125 Temperature 25 0 PC Max 600 0 C Min 150 0 C Harmonics 1 2 3 4 Harmonic 3 5 o o strain 0 2 0 2 0 0 0 0 Options PreShear Off Dela OF Analogin OH MeasOps Otf Ok Options End of Test d Save As Help Cancel Figure 3 8 MultiWave Single Point Test Set up Screen ARES User Manual 113 Hult ave Temperature Ramp Test Figure 3 9 MultiWave Temperature Ramp Test Set up Scr
223. t to the Stress Relaxation experiment which uses the same type of deformation but monitors torque and strain instead of torque and normal force The direction selected is the rotational direction of the actuator for positive Strain values Data can be taken in either of two modes Log Logarithmic Logarithmic sampling takes data at logarithmically incremented intervals resulting in equally spaced data points when plotted as a function of logarithmically scaled time the number of points taken is inversely proportional to zone time As an example selecting 5 points per zone during a 100 second zone divides the difference of the endpoint times logarithms into five equally spaced fractional exponents Six data points are measured in succession at times determined by taking the antilogarithm of each exponent 10 15 9 25 1 39 8 63 1 and 100 seconds Linear Linear sampling takes data at linearly incremented intervals resulting in equally spaced data points when plotted as a function of linearly scaled time This technique is useful for relatively short zone times where linear time scaling is practical As an example selecting 5 points per zone during a 100 second zone results in five data points measured at linear increments 20 40 60 80 and 100 seconds Torque Normal Relaxation Test H ES SUTIN occ foa Mas 31 2 5000 Min 0 0031 25 Temperature 25 0 PC Max 600 0 C Min 150 0 sampling Mode Log Linear Points Per
224. tation 48 temperature control 58 Oven PRT 65 244 ARES User Manual P Parallel Plates test tool constants 161 165 tool installation 163 171 general information 161 165 operating range 161 165 sample loading 163 171 patents 5 Peltier description 76 humidity cover 83 installation 78 operating specifications 30 operation 83 PID loop setup 82 selecting operating range 77 Phase Angle description 94 shift 9 94 Platinum Resistance Thermometer See PRT Pneumatics Panel connections 54 description 53 location 47 Polymer Melts 150 Power Panel connections 51 description 50 location 47 PreTension See AutoTension PRI 27 58 65 224 233 Pseudoplasticity 94 R registered trademarks 5 Regulatory Compliance 14 ARES User Manual Rim Shear 125 S Sample PRT 65 Service and Repair 230 Shear Rate 93 Shear Stress 93 Shear Thickening See Dilatancy Shear Thinning See Pseudoplasticity Signal Panel connectors 49 description 47 general connections 47 location 47 software license 3 Squeeze Flow 125 Stage description 37 location 34 Stage Control manual 37 rate adjustment 39 software 38 Steady and Transient Measurement Formulas 205 Steady PreShear 140 Steady Rate Sweep 118 Steady Single Point 116 Steady Step Rate Temperature Ramp 135 Step Shear Rate 121 Stiffness 150 Storage Modulus See Elastic Modulus ARES User Manual Strain 93
225. te the G MAXIMUM value into equation 4 2 then determine the upper limit of operation by calculating N at each O values chosen to be from the lowest to highest frequencies within the transducer operating range 3 Substitute the G MINIMUM value into equation 4 2 then determine the lower limit of operation by calculating N at each 4 Generate an X Y scatter plot of complex viscosity N Y axis versus frequency X axis The region between the upper and lower limits of operation is the range of complex viscosity that can be tested Appendix 1 contains a table of G values for the double wall Couette for some transducers and a standard motor NOTE The cup installation and use procedures are different for the original fluid bath and the fluid bath 2 Please ensure that you identify which bath and Couette cup you have and follow the correct procedures for your specific bath cup arrangement Tool Installation Original Fluid Bath The Double Wall Couette lower tool cup mounts into the fluid bath or fluid bath 2 see next section to ensure precise thermal control Install the bath on the test station prior to mounting the tool in the bath _ CAUTION Never place any lower tool into the bath if the temperature 0 of the lower tool is cooler than that of the bath Placing a tool into a warmer bath will result in expansion of the tool during use After expansion the tool may not be removable without damaging your bath We
226. that may make testing in one geometry preferable to testing in another Additionally factors such as anisotropy and differences in strain dependence may yield inconsistent results for different geometries Recommendations for selection of a geometry based upon sample type are as follows Thin Films or Fibers Test thin films such as magnetic recording tape or fibers using the fiber film tool Enter the test geometry dimensions into the appropriate Tension geometry screen Fluids Suspensions and Emulsions Low viscosity fluids or suspensions of limited stability can be tested using either the Couette or Double Wall Couette geometry Higher viscosity fluids and thicker suspensions and emulsions can be tested using parallel plates or cone and plate geometries Solid Samples Including Thermosets Thermoplastics and Elastomers These materials can be tested using the Torsion Rectangular tool Several inserts are available to accommodate a variety of sample thicknesses ARES User Manual 149 Polymer Melts and Soft Solids Melts can be tested using the parallel plate or cone and plate geometries Thermosetting Resins and other Curing Studies These materials are best tested in a parallel plate tool Disposable plates are available for curing studies or other tool destructive materials Testing Limits and Compliance Definition of Compliance and Stiffness For this discussion compliance is defined as displacement in radians per
227. the Control pull down menu of Orchestrator Figure 2 18 ARES User Manual Set Test Conditions Form k E Change Test Parameters Temperature oo eeeeseseseees 5 0 PC Masw 500 0 Min 1 50 0 AutoTension Sensitivity 0 0 g Enable N2Gas Switch C No amp Yez Switch from Nz to Gas Above 45 0 FE Switch from Gas to We Below 30 0 FC Figure 2 18 Set Test Conditions Form Showing Gas Switching Enabled Note that N2 in the form refers to liquid nitrogen Oven Operating Requirements The oven can operate only if the following conditions are met e The oven is selected as the current environmental system e The environmental controller is turned ON in the Instrument Control Panel e The oven must be positioned all the way to the right and the oven must be closed e Either air or N must be supplied to the oven at a pressure greater than 35 psi e If using the LN2 Controller the liquid nitrogen LN2 level in the Dewar Flask must be between 50 and 75 of capacity When it is the Orchestrator Online Indicator LN2 Ready is displayed ARES User Manual Oven Configuration in Orchestrator When you command a temperature Orchestrator software uses the Instrument Configuration to determine the environmental system currently in use and establish operating conditions Prior to operating the oven access the Instrument Configuration function located under the Service function of the Utilities pull down me
228. the delicate high precision bearing surfaces of these components Damage to the bearing surfaces will result in faulty measurements and if significant enough the damage will require the replacement of the entire motor or transducer The relative humidity of the supplied air should be 35 to 70 with a dew point of 10 deg C We highly recommend installing the optional air dryer filter between the test station and the air supply If your air supply has excessive moisture levels which result in the immediate condensation into water an additional water trap will be required before the air dryer Excessive moisture in the air supply will damage the test station CAUTION Read the operating and maintenance instructions that were supplied with your air dryer Failure to properly operate and maintain your air dryer will result in extensive damage to this instrument Because of the critical nature of the air supplied to the instrument and the potential for expensive damage through mishandling we highly recommend that you inform your laboratory manager or compressor maintenance personnel of your instrument requirements in detail You should also ask to be informed before any air supply interruption or compressor maintenance so that you can properly shut down and protect the test station Typically after any compressor maintenance there will be some residual particulates and moisture present in the supply lines You should disconnect the air from the
229. the stage to the loading position Place the top cover onto the upper tool shaft and hold it in place using the clip The cover should be held near the top of the tool to allow access to the upper plate for mounting and sample loading Verify that the motor is on Mount the lower tool PRT as described in your main instrument manual if desired Mount the upper and lower tools on the actuator shafts Using the Set Gap Instrument Control function in Orchestrator zero the normal force and torque on the motor using the Offset Normal Force to Zero and Offset Torque to Zero buttons Using the stepper control buttons lower the stage to a point where the tools are close but not touching Use the Zero Fixture button in the Set Gap Instrument Control function to determine the zero point for the test tools Raise the stage to provide sufficient room for sample loading Sample Loading The recommended gap setting for parallel plates is between 0 5 and 2 millimeters For the Hastelloy tool the maximum sample gap is 2mm Beyond that the upper toll will rub on the cover Figure 4 8 shows the Hastelloy tool with a sample loaded and the cover installed 1 2 Place the sample on the lower plate Ensure that the sample is centered on the tool Using the stepper motor buttons on the right side of the test station adjust the sample gap until the upper plate is close to the specimen Set the gap using the Set Gap Instrument Control function e
230. tor S SS EN ARES User Manual Notes Cautions and Warnings Throughout this manual the following terms and symbols are used to draw attention to specific situations NOTE A NOTE highlights important information about equipment or procedures 0 CAUTION A CAUTION emphasizes a procedure that may damage equipment or cause loss of data if not followed correctly WARNING A WARNING indicates a procedure that may be hazardous to the operator or to the environment if not followed correctly ARES User Manual 9 Safety Do Not Attempt Service Do not attempt to service this instrument as it contains no user serviceable components Required Equipment While operating this instrument you must wear eye protection that either meets or exceeds ANSI Z87 1 standards Additionally wear protective clothing that has been approved for protection against the materials under test and the test temperatures Safety Notices The following notices are intended to draw your attention to situations that pose a risk to either your personal safety or the safety of the instrument Although these notices appear at relevant points throughout this manual they are repeated here for emphasis Additionally all safety notices that appear on the instrument are reproduced on page 13 01 CAUTION Read the operating and maintenance instructions that were supplied with your air dryer Failure to properly operate and maintain your air dryer will resu
231. tored by the ENVIRONMENTAL CONTROLLER that receives its commands from the temperature controller TEMP CONTROLLER located within the control computer When a test temperature is selected at the HOST COMPUTER the CPU configures the TEMP CONTROLLER to output a command TEMP CMD AND MEASURE to the ENVIRONMENTAL CONTROLLER This command combines with the heater power feedback signals to increase or decrease heater power as necessary to control oven temperature To monitor actual oven temperature Platinum Resistance Thermometers PRT are installed in the oven Two PRIs monitor the air temperature by each heater and a third PRT TOOL TEMPERATURE monitors the temperature of the lower sample tool in use The temperature controller electronics monitor PRT resistance to determine the actual internal oven temperature A difference between the actual temperature as sensed by the PRIs and the commanded temperature that is entered by you at the HOST COMPUTER results in the generation of an error signal by the ENVIRONMENTAL CONTROLLER electronics TEMP CONTROL AND FEEDBACK This error signal either raises or lowers the internal oven temperature until the PRT sensed temperature and the commanded temperature agree When using the Fluid Bath the circulator is under RS 232 control from the Test Station Either the fluid in the circulator using the circulator s internal PRT or the lower test tool itself using the lower tool PRT can be maintained at the desire
232. tropic loop test available on Shear Strain Controlled instruments Options The following test options are available for use with Stress Ramp e Delay Before Test ARES User Manual 139 Test Options This section describes the following test options that you can select while programming selected dynamic tests e Steady PreShear e Delay Before Test e Auto Tension Adjustment e Analog Data Input e Auto Strain Adjustment e Measurement Options Steady PreShear Steady PreShear allows you to subject the sample to a steady shear deformation prior to the start of a dynamic test If the Delay Before Test option is selected Steady PreShear occurs prior to the delay No data are taken while the pre shear is being applied The following parameters are set through the Steady PreShear Set Up Screen Figure 3 24 PreShear Rate Shear rate of the PreShear stress Positive PreShear Rates result in clockwise actuator rotation Negative PreShear Rates result in counterclockwise actuator rotation PreShear Time The length of time the PreShear is applied Dynamic Temperature Step Test Uptions Steady PreShear Delay Before Test AutoTension Adjustment AutoStrain Adjustment pa Mio Ha Measurement Options PreShear Rate fa T 1 3 Max 2500 000 Min 0 025000 Pres hear Time 45 e or hom Positive Rate Cf Negative Rate CEW Figure 3 24 Steady PreShear Set Up Screen AR
233. ts es eaaeeeaoe ona meanaeets 133 Fore a AA tE E err rr rere ere 134 PSS a o AAA E ct E Eo O T A S 134 PS o E E ness 134 USO TONG inte fisio 134 oleada tep kale Tempera i e Nai 135 Descrip Otesi onin oro E E E E T E E EEO 135 Saue o MOE A oo 5 E E corse pucainosonsaleases oe 136 a mo 191 A NE E E E E E ane ca eee taenaaeese 136 Sess ontrolled Transient Test Melodia 137 Sonae CSS CSU E E E E T E A E 137 Funcuonal D S WOM ea a E E R E E E E R EAA E opa 137 Saue Us nio noise 138 OPUS testi 138 MESS INN TEO ias 139 Descanso A E E E ai E E sahersbanate Rndaaansets 139 Sa D E E E A E A E E E A E E 139 Deon tcc o o 139 T EOD mapeo E E E E E E A E AE EEN E EE EEEE eipiro adoro moros 140 US My as 140 Delay STOR CS E E E ae eee eee 141 Mantel Dean ici 141 APP AO Ens icon 141 Automatically Start Test When On Temperature oooncnocnocnncnnononnnnnanncnnanonancnnnnanancnnnnnnnonncnnancanncnnnonnancancananins 141 AU Wiis Ol AU O aa 142 ae e E RE 144 PUT ue ON OP aps soem E EEA desea E E EO AE EA E AAEE EE A TA 145 Iie Ri mont Op 11019 a E E E EA 146 Sea EN EAE E E O 146 ARES User Manual ES Cy Cl Comi stereo 146 SO A ie o o AAA EU OO A A 146 Chapters Test Geometries and FOIS Sun d one 149 TRU cig creat cts ts apart c o e rn ht aatuntanen eagancnrtenees 149 General Test Tool Morna UON AAA o O aa AARTE NE a a O 149 General Recommendations for Geometry Selection ssessssessssessssessrsessssesesstsersrsesrtstsresrsrrnenesnrsesresenessese
234. ttons 5 Using the stepper control buttons lower the stage to a point where the tools are close but not touching 6 Use the Motor Position Offset button in the Set Gap Instrument Control function to ensure that the upper and lower tool openings are aligned 7 For 2K FRT transducers only skip this for STD transducers use the Zero Fixture button in the Set Gap Instrument Control function to bring the tools together and determine the zero point for the test tools 8 Raise the stage to provide sufficient room for sample loading ARES User Manual Sample Loading Refer to Figure 4 10 and Figure 4 11 during the following procedure WARNING This is a high torque motor Turning on the motor while in ES dynamic mode causes the motor to snap to dynamic zero position at a high velocity This can cause severe damage to the transducer and or personal injury To avoid damaging yourself and the transducer Never turn on the motor while a sample is loaded Keep hands clear of the motor 1 Measure and record the following sample dimensions e Width e Thickness e Length STD transducers only length will be determined from gap setting for 2K FRT transducers 2 Select a matching pair of setting anvils based upon sample thickness and secure them in the upper and lower tool Please note that each setting anvil is machined in such a way as to provide mounting for two different sample thickness ranges A nominal thickness roughl
235. umatic input to the Oven Pressure Sensor which is used to monitor oven gas pressure The gas pressure must be above 35 psi for the oven to function Pneumatic input to the Oven that accepts air which is circulated throughout the Oven in order to maintain positive pressure and minimize frost when using LNo ee ee Gas Supply to OVEN Selector Switch Position for AIR i SSeS SSeS SS SS ses SS SSS Fosition for i gt N2AGAS SS SSS SPS SRS SS SPSS SSS SSeS eS ee ee Panel Side ADUCER RSA 111 40 PSI XDUCER BENDIXFRT 35 PSI MOTOR 60 PSI MAIN 50 PSI SZ 5 5 BAR Panel Back Figure 2 15 Pneumatics Panel TRANSDUCER Air Pressure Adjust Knob MOTOR Air Pressure Adjust Knob OVEN Air Pressure Adjust Knob OVEN PRESSURE SENSOR N2 GAS 70 PSI YN This panel has 2 sides and wraps around the right rear corner of the Test Station ARES User Manual Environmental Control Systems There are three environmental control systems available for use with ARES Each system is used to precisely control sample temperature The three systems are a forced air convection oven Oven a re circulating fluid bath and a rotating oscillating Peltier The air convection oven has a dual element heater with counter rotating air flow for a wide temperature range ambient to 600 C and maximum temperature stability If temperatures below ambient are required then either th
236. unting the Peltier Assembly perform the following actions on the ARES instrument e Raise the Stage to maximum height e Remove all Upper and Lower Test Tools and loosen the Anvil Tightening Knob on the Motor Anvil e Thoroughly inspect the Test Tool mounting surfaces i e inspect the transducer anvil and the motor anvil and clean off any material that may interfere with the mounting of the Peltier This is essential to ensure proper mechanical mating between the Peltier Assembly and the instrument e Turn off the Motor Refer to Figure 2 29 during the following installation procedures 1 Remove the protective plastic base from the Peltier Assembly Collar by placing the two pins on the spanner wrench provided into two of the holes machined into the Collar and rotating the wrench counterclockwise 2 Gain access to the Peltier Assembly Shaft by sliding the cover of the Peltier Assembly fully upward 3 Hold the Peltier Assembly above the ARES Motor Anvil with the Bath Hoses facing toward the right of the instrument 4 Rotate the Peltier Assembly Shaft to align the flat portion of the Shaft with the flat portion of the ARES Motor Anvil both flats should be facing toward the right as you face the instrument At this time the red dot on the PRT Plug should be facing toward the front of the instrument CAUTION As you lower the Peltier Assembly in the next step the 01 Peltier Assembly PRT Plug will be inserted into the ARES PRT Re
237. ver ARES User Manual Fluid Bath Description The Fluid Bath offers precise control of sample temperature using an open fluid re circulant system The lower test tool is mounted within the Bath Well around which flows thermally controlled fluid supplied by a circulator The temperature of the lower tool is measured by the bath PRT which mounts through the Bath Well into the Motor You can choose to control the temperature of either the lower tool or circulator fluid The Circulator regulates the temperature of the bath fluid and pumps the fluid through the Fluid Bath The circulator as supplied by TA Instruments is connected to and is under the control of the test station and software The fluid circulated through the bath is maintained at the temperature selected in Orchestrator The circulator has its own fluid temperature regulation which can optionally be used as the temperature control loop for the Bath Installation of Fluid Bath The fluid bath is mounted onto the motor using a threaded collar Refer to Figure 2 35 while performing the following steps to install the bath Raise the stage to maximum height and remove the upper test tool Slide the Oven all the way to the left Turn off the Motor Position the motor anvil with the knob facing the front of the instrument Position the bath with the access port facing the front of the instrument and the alignment pin which is located on the inside diameter of the bath housi
238. vides the difference of the endpoint times logarithms into five equally spaced fractional exponents Six data points are measured in succession at times determined by taking the antilogarithm of each exponent 10 15 9 25 1 39 8 63 1 and 100 seconds Linear Linear sampling takes data at linearly incremented intervals As an example selecting 5 points per zone during a 100 second zone results in five data points measured at linear increments 20 40 60 80 and 100 seconds Select a strain and direction which is maintained throughout the entire test Figure 3 15 and then a sample time zone time for each of the four zones The times can be anywhere from 2 0 to 1 6x10 seconds in length Usually the first zones are set at very short time periods typically from 2 0 to 10 seconds as most of the relaxation happens very quickly with subsequent zones being set to longer times Please note that regardless of the field inputs the fastest the instrument will take data is 1 data point every 3 msec Stress Relaxation Test E ES SEAMOS sossoscoooscso0ss fico Max 31 2 5000 Min 0 003125 Temperature IET PC Max 600 0 C Min 150 0 C Sampling Mode Log Linear Points Per Zone f200 Max 350 Min 20 Zone Number 1 2 3 4 Zone Time s or e aa fc IS Directora f Clockwise O Counterclockwise Options FreShear Ot Delay Ot Analogln OFf Options End of Test Save As Help Cancel Figure 3 15 Stress Relaxation Te
239. when very stiff samples are tested and the transducer displacement becomes close to the motor displacement In this case because the difference between the two displacements is small the resulting relative error is large and of similar magnitude as the measurement If the measured strain value is significantly smaller than the commanded strain value the data are likely affected by transducer compliance As a practical guideline measured sample strain should be at least 30 the commanded strain Although measurements can be taken below these limits you are cautioned that accuracy may be affected Measurements that are affected by transducer compliance typically report modulus values that are lower than the true modulus One method of determining if transducer compliance is affecting the data is to switch to a different geometry and compare the results to the first tests If the data are unaffected by compliance the results from the two geometries should be nearly identical Sample compliance or stiffness is related to both the modulus and geometry of the sample Since the modulus is fixed the sample dimensions are normally adjusted to make the sample less stiff or the geometry is changed altogether to obtain the desired sample compliance It is critical that the sample compliance is within the operational range of the instrument otherwise inconsistent or incorrect results will be obtained ARES User Manual Determination of Operational Range
240. which the fundamental is multiplied by to determine the frequency for a given harmonic A value of 0 0 zero is used to indicate that that zone is not used Strain This is defined as the strain amplitude of the given harmonic Note that a value of 0 0 zero can be used to signal the instrument to make a measurement at the given harmonic without any applied strain at that frequency which can be used to monitor distortions in the stress sine wave that can indicate nonlinear behavior The MultiWave setup menu is displayed following selection of either single point Figure 3 8 or temperature ramp Figure 3 9 test methods Here you must select a fundamental frequency between 2 rad sec and 1x10e rad sec 0 318 and 1 59x10e Hz The strain level for the fundamental frequency must also be entered 5 ARES User Manual You can select up to seven harmonics multiples of the fundamental and assign a strain to each harmonic As a general rule the sum of all strains should not exceed the linear viscoelastic region of the material A strain sweep can be used to determine the limits of linear behavior if that information is not known If a value of zero is entered for both the stain and harmonic then that column is not used If a nonzero frequency is entered with a strain level of zero data will still be acquired at that frequency This provides a means for measuring the amount of harmonic stress generated by other frequencies and can provide insigh
241. x When the checkbox is selected the instrument reads and stores the actual gap immediately prior to the start of a test It then rechecks strain error limits using the actual gap overriding the gap entered in the specific geometry form Out of range limits are then reported For Stored Geometries the Read Test Fixture Gap checkbox is displayed only if you saved a Stored Geometry while the Remote Gap Monitoring option was enabled using the Instrument Configuration function Displaying the Instrument Gap The gap read from the instrument can be displayed as the online parameter CurrGap Max Allowed Force While Setting the Gap The Max Allowed Force option when setting the gap provides two benefits First it allows an operator to set the gap in a repeatable documentable way Loading the sample the same way each time leads to more reproducible results between different operators or with different geometries Additionally it helps avoid internal pre stressing a sample during loading which again could lead to erratic or inconsistent results This feature is also helpful when loading soft samples that may squeeze out from between the test tool if to much force is applied Setup Instrument Options El ES Instrument Testing Limits Instrument Setup Stepper or Linear Motor Ho 0 Yez Autoranging Transducer f No Yes Normal Force Measured ooo No f amp Yez Remote Gap Monitoring f No 0 ves AOA Option Connect
242. x Viscosity Viscosity In phase Viscosity u sin d Out of phase Viscosity u cos 0 Measurement Method During dynamic mechanical testing the ARES control computer makes a digital cross correlation of measured strain and force by comparing the amplitude and phase shift between the imposed motion strain and the force stress When a test is started the computer measures strain and force 2 048 times to determine the average amplitude and phase shift of both The measurements are made relative to two reference sine waves command of fixed amplitude and having phase angles of 0 and 90 as shown in Figure 3 14 The result is a strain and force phaser relative to the reference as shown in Figure 3 1B Using fundamental geometric techniques the phasers in Figure 3 1B can be rotated so that strain becomes the reference axis as shown in Figure 3 1C The force vector can now be defined in terms of an in phase and out of phase component of force proportional to angle 6 Using equations appropriate to the geometry under test the average force phaser is converted to stress and the average angular strain phaser is converted to percent strain Dividing the stress by the strain produces the complex modulus G which indicates the total energy required to deform the material Multiplying G by the cosine of the phase angle gives the in phase component of the stress G which is proportional to the energy stored elastically Multiplying G by
243. y the center of the clamping range is stamped on two of the anvil faces opposite sides The setting anvil should be mounted such that the desired nominal thickness is visible from the outside back of the tool opposite the actual sample 3 Place the sample into the lower tool Center the sample in the tool using the reference lines scribed in the setting anvil and sliding clamp Partially tighten the clamp using the adjusting screw to hold the sample 4 Lower the stage until the upper tool is about 1 4 inch from the sample 5 Use the Motor Position Offset button in the Set Gap Instrument Control function in Orchestrator to radially align the sample with the upper tool if necessary CAUTION In the next step do not generate a Torque or Normal Force greater than 50 of full scale Failure to observe this caution may result in damage to the transducer 6 While confirming the sample fits into the upper tool lower the stage until a compressive downward Normal Force of about 10 of full scale is generated If the sample is not aligned properly re raise the stage and carefully realign the sample and tool using the Motor Position Offset button Ensure visually that the sample is completely inserted into the tools 8 Tighten the lower and upper sliding clamps using the adjusting screw to the desired torque using the torque screwdriver 9 Raise the stage until a force of approximately 10 of full scale is generated Please n

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