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TA I

NSTRUMENTS

TMA 2940 CE

3–1

CHAPTER 3: Running Experiments

Overview .................................................... 3-3

Before You Begin ................................ 3-4

Calibrating the TMA ................................... 3-5

Force Calibration .................................. 3-5

Probe Calibration .................................. 3-6

Temperature Calibration ....................... 3-6

Cell Constant ........................................ 3-8

Running a TMA Experiment ..................... 3-10

Experimental Procedure ..................... 3-10

Selecting a Probe ................................ 3-11

Zeroing the Auto Measure System .... 3-12

Sample Preparation and Loading ........ 3-13

Sample Preparation ...................... 3-13

Sample Loading ............................ 3-13

Thermocouple Positioning................... 3-15

Measuring the

Sample Length .................................... 3-15

Setting Up an Experiment................... 3-16

Содержание TMA 2940 CE

Страница 1: ...40 CE Thermomechanical Analyzer Operator s Manual PN 825615 001 Rev C Text and Binder PN 825615 002 Rev C Text Only Issued November 1999 109 Lukens Drive New Castle DE 19720 Thermal Analysis Rheology...

Страница 2: ...s publication is not a license to operate under nor a recommendation to infringe upon any process patents TA Instruments TA Operating Software and Instrument Data Analysis and Utility Software and the...

Страница 3: ...ompliance xiii InstrumentSymbols xiv Electrical Safety xv HandlingLiquidNitrogen xv Lifting the Instrument xvii Using This Manual xvii CHAPTER 1 Introducing the TMA 2940 CE 1 1 Introduction1 3 Compone...

Страница 4: ...npacking the 2940 CE 2 3 RemovingtheShippingMaterial 2 6 Repacking the 2940 CE 2 8 InstallingtheInstrument 2 9 Inspecting the System 2 10 Choosing a Location 2 11 Installing the Weight Tray Door 2 12...

Страница 5: ...efore You Begin 3 4 Calibrating the TMA 3 5 ForceCalibration 3 5 ProbeCalibration 3 6 TemperatureCalibration 3 6 Heater Temperature Calibration 3 8 Cell Constant 3 9 Running a TMA Experiment 3 10 Expe...

Страница 6: ...ries 3 17 Using Air Cool 3 17 Using a Purge Gas 3 18 Suggestions 3 18 Starting an Experiment 3 19 StoppinganExperiment 3 20 RemovingSamples 3 20 SubambientExperiments 3 22 Performing a Cooling Experim...

Страница 7: ...4 8 Calculating the Offset 4 9 Calibration 4 11 Sample Preparation 4 12 UsingtheAluminumBalls 4 12 Using the Stainless Steel Clamps 4 14 Flexure Accessory 4 17 Description 4 17 Accessory Installation...

Страница 8: ...30 Sample Preparation 4 31 Sample Encapsulating Press 4 31 Preparing Moldable Powders 4 35 Preparing Resinous Materials 4 38 Preparing Sheet Materials 4 40 SampleLoading 4 41 Cleanup 4 42 Calculation...

Страница 9: ...1 Overview 6 3 Routine Maintenance 6 4 Inspection 6 4 Cleaning 6 5 Cleaning the Keypad 6 5 Cleaning the Probe Assembly 6 5 Cleaning the Stage 6 6 Cleaning the Thermocouple 6 7 Replacements 6 8 Replac...

Страница 10: ...TA INSTRUMENTS TMA 2940 CE X Table of Contents continued TMA 2940 CE Test Functions 6 15 The TMA Confidence Test 6 15 Replacement Parts 6 18 APPENDIX A Ordering Information A 1 INDEX I 1...

Страница 11: ...instructions under the guidelines described below Highlights important information about equip ment or procedures Emphasizes a procedure that may damage equipment or cause loss of data if not followe...

Страница 12: ...TA INSTRUMENTS TMA 2940 CE XII Helplines To TA Instruments For Technical Assistance 302 427 4070 To Order Instruments and Supplies 302 427 4040 For Service Inquiries 302 427 4050 Sales 302 427 4000...

Страница 13: ...as amended by Council Directive 93 68 EEC the following specifications apply to the TMA 2940 CE instrument when used with the stepdown transformer PN 994560 901 Safety EN 61010 1 1993 A2 1995 Installa...

Страница 14: ...on the stage can of the TMA 2940 CE indicates that a hot surface may be present Take care not to touch these areas or allow any material that may melt or burn to come in contact with these hot surfac...

Страница 15: ...fter transport or storage in humid condi tions this equipment could fail to meet all the safety requirements of the safety standards indicated Refer to the NOTE on page 2 10 for the method of drying o...

Страница 16: ...otection wear high topped sturdy shoes and leave your pant legs outside the shoe tops 2 Transfer the liquid slowly to prevent thermal shock 3 Use containers that have adequate low temperature properti...

Страница 17: ...ld compresses 2 See a doctor IMMEDIATELY if the skin is blistered or if there is a chance of eye infection Lifting the Instrument The TMA 2940 CE is a fairly heavy instrument In order to avoid injury...

Страница 18: ...ncludingsubambi ent operations CHAPTER 4 Contains the procedures used to operate the TMA with the optional accesso ries CHAPTER 5 Explains thetechnical aspects of the TMA and itsoperation CHAPTER 6 Pr...

Страница 19: ...arning Store and use in an area with adequate ventilation Do not enter confined spaces where nitrogen gas may be present unless the area is well ventilated The warning shown above applies to the use o...

Страница 20: ...TA INSTRUMENTS TMA 2940 CE XX...

Страница 21: ...ducing the TMA 2940 CE Introduction 1 3 Components 1 3 The 2940 CE Instrument 1 5 2940 CE Display 1 7 2940 CE Keypad 1 7 HEATER Switch 1 11 POWER Switch 1 11 Accessories 1 12 Standard Accessories 1 12...

Страница 22: ...Introduction 1 2 TA INSTRUMENTS TMA 2940 CE...

Страница 23: ...the analysisinstruments Enables you to set up experiments and enter constants Stores experimental data Runs data analysis programs Components Your instrument consists of two major parts the TMA cabine...

Страница 24: ...oling container and the furnace monitor thermocouple The weight tray located behind the weight tray door holds the weights to exert a known force on the sample The chromel alumel sample thermocouple s...

Страница 25: ...et The display provides valuable realtime information on the experiment in progress The TMA was developed by TA Instruments with the following features Operates over a temperature range of 150o C to 1...

Страница 26: ...dilatometry with the optional accessories that can be used with the instrument The cabinet contains the keypad used to control the mechanical movements of the instrument and the display used to obser...

Страница 27: ...status the right nine characters show the sample temperature and the bottom line is a realtime signal display Status codes are dsscribed in the Technical Reference chapter of this manual 2940 CE Keypa...

Страница 28: ...the probe or stage is changed MEASURE Measures your sample s LENGTH lengthautomatically use this key before beginning the run The measured length is transferred to the control ler and the value is re...

Страница 29: ...action occurs centering the LVDT coil If the probe is moving up and Probe is pushed the probe will stop and reverse its direction Raises or lowers the FURNACE furnace You can stop the furnace movement...

Страница 30: ...This is the same function as Stop on the controller If an experiment is not running the instrument is in a stand by or method end state the STOP key will halt any activity air cool allmechanical motio...

Страница 31: ...he STOP key HEATER Switch The HEATER switch see Figure 1 2 turns the power to the instrument heater on and off The switch should be in the ON 1 position before you start an experiment The light in the...

Страница 32: ...allow you to perform various basic analyses These probes are as follows The expansion probes are used to measure the thermal coefficient of expansion and glass transition The standard expansion probe...

Страница 33: ...40 CE These optional accessories will allow you to perform experiments on different types of samples Film Fiber Accessory Dilatometer Accessory Parallel Plate Rheometer Accessory Flexure Accessory Hem...

Страница 34: ...ns Depth 45 5 cm 18 in Width 58 5 cm 23 in Height 66 cm 26 in Weight approx 27 2 kg 60 lb Power 120 V ac 50 60 Hz 10 amps Temperature 150 to 1000o C range Sampleheight 25 mm 1 inch maximum Sample diam...

Страница 35: ...TA INSTRUMENTS TMA 2940 CE 1 15 Table 1 3 Temperature Control Programmed 0 01 to 200o C min heating rate Temperature 2o C reproducibility Specifications...

Страница 36: ...Introduction 1 16 TA INSTRUMENTS TMA 2940 CE...

Страница 37: ...llingtheInstrument 2 9 Inspecting the System 2 10 Choosing a Location 2 11 Installing the Weight Tray Door 2 12 Installing the Stage 2 13 InstallingtheExpansion Penetration Probes 2 17 Installing a Pr...

Страница 38: ...Installation TA INSTRUMENTS TMA 2940 CE 2 2...

Страница 39: ...y wish to retain all of the shipping hardware the plywood and boxes from the instrument for reuse if you want to repack and shipyourinstrument Unpacking the 2940 CE Refer to Figures 2 1 to 2 3 while u...

Страница 40: ...h one side hanging over the edge of the bench see Figure 2 2 Someone must be holding onto the unit at all times while it is in this position Figure 2 2 Removing the Plywood Board 5 While your assistan...

Страница 41: ...same manner 7 Remove the x 20 screws and mounting feet from the accessory kit Place the screws through the centers of the rubber feet 8 Have your assistant lift the entire unit while you slide the pl...

Страница 42: ...Slip off the cardboard cylinder then replace the cap on the furnace post 3 Raise the furnace and rotate it clockwise to move it off to the side 4 Take the stage shield off and discard the packing foam...

Страница 43: ...ch loosen and carefully remove the top and bottom clamp ing bars of the suspension shipping clamp 11 Using the same wrench remove the eight 8 screws from the front and rear clamping bars of the suspen...

Страница 44: ...suspension assembly Adjust if necessary by fine tuning the positions of the weights 16 Reinstall the balance enclosure and tighten the four screws 17 Plug in and turn on the power to the TMA 2940 CE...

Страница 45: ...and accessory kit Inspecting the system for shipping damage and missing parts Assembling the TMA Connecting the TMA to the TA Instruments controller Connecting the purge gas and air line accessories a...

Страница 46: ...nts offices can be found in Appendix A of this manual Drying out the instrument may be needed if it has been exposed to humid conditions Certain ceramic materials used in this equipment may absorb moi...

Страница 47: ...the instru ment sdimensions On a stable heat and fire resistant vibration free work surface Near a power outlet 120 Vac 50 or 60 Hz 10 amps A step up down line trans former may be required if the uni...

Страница 48: ...these steps to install the door 1 Locate the mounting holes on the top and bottom of the door 2 Hold the door with these mounting holes to the left 3 Put the lower hole over the small bottom post to t...

Страница 49: ...wise and pull it up off the three posts 4 Remove the stage from the accessory kit 5 Slide the wave washer washer with rippled edges down over the top of the stage so that it fits on the flange 6 Slide...

Страница 50: ...couple to the stage as follows a Position the tip of the thermocouple so that it bends at a 90 angle and lies flat against the platform It should be close to but not touchingthe sample b Hold the ther...

Страница 51: ...Attaching the Thermocouple to the Stage 11 Put the stage shield on the stage aligning the slot in the bottom over the thermocouple see figure on next page 12 Rotate the furnace into position over the...

Страница 52: ...RUMENTS TMA 2940 CE 2 16 Figure 2 7 Assembled TMA with Stage and Thermocouple 13 Install one of the probes as directed in the next section Refer to Chapter 3 for guide lines in selecting a probe Stage...

Страница 53: ...atometer andhemispheri cal probes To learn how to install the film fiber probe turn to Chapter 4 Using Your Options Installing a Probe 1 Raise the furnace and rotate it clockwise to move it off to the...

Страница 54: ...ents Removing a Probe 1 Raise the furnace and rotate it clockwise to move it off to the side 2 Grasp the top of the probe with one hand Using the other hand locate and hold the probe locking lever fou...

Страница 55: ...wer cords always handle them by the plugs not by the cords Protect power and communications cable paths Do not create tripping hazards by laying them across accessways GPIB Cable 1 Locate the GPIB con...

Страница 56: ...1 to 9 Use the rotary address dial on the TMA connector panel to set the desired address Figure 2 10 shows a instrument address of 5 If you have a multiple instruments system each instrument must hav...

Страница 57: ...eset button to enter the new address Wait 30 sec onds after releasing the Reset button the green Ready light should begin to glow steadily Reconfigure the instrument with the controller to bring the i...

Страница 58: ...nstrument For a list of the gases that can be used in the TMA see Chapter 3 Use of corrosive gases will shorten the life of the instrument 2 Make sure that the pressure of your purge source does not e...

Страница 59: ...to a flowmeter consult your compressed gas vendor for specific requirements Then connect the flowmeter to the purge gas source 4 The recommended setting for the purge rate is 100 mL per minute 100 C a...

Страница 60: ...left side of the TMA cabinet back marked with a maximum pressure warning label 840 kPa 120 psi as seen in the figure below Figure 2 13 TMA COOLING GAS Fitting 2 Make sure your compressed lab air sourc...

Страница 61: ...l outlet 1 Make sure the instrument POWER switch see Figure 2 14 is in the OFF O position Figure 2 14 Front Panel of TMA Showing POWER Switch 2 Plug the power cable into the TMA Before plugging the TM...

Страница 62: ...The instrument will run an internal confidence test each time you turn on the power 3 Watch the instrument display during the confidence test for any messages that may be indicated Confidence test de...

Страница 63: ...TA INSTRUMENTS TMA 2940 CE 2 27 Figure 2 15 TMA Standby Display TMA 2940 Thermomechanical Analyzer Standby 23 25 C DimChg 0 135 m Starting the 2940 CE...

Страница 64: ...experiment on your instrument and wish to use the thermal analysis system for some other task leave the instrument on it will not interfere with whatever else you wish to do If your system will not b...

Страница 65: ...libration 3 6 TemperatureCalibration 3 6 Cell Constant 3 8 Running a TMA Experiment 3 10 Experimental Procedure 3 10 Selecting a Probe 3 11 Zeroing the Auto Measure System 3 12 Sample Preparation and...

Страница 66: ...ccessories 3 17 Using Air Cool 3 17 Using a Purge Gas 3 18 Suggestions 3 18 Starting an Experiment 3 19 StoppinganExperiment 3 20 RemovingSamples 3 20 SubambientExperiments 3 22 Performing a Cooling E...

Страница 67: ...al method on the controller Attaching and setting up external accessories as required e g purge gas air cool gas switching accessory Zeroing the probe Preparing and loading the sample Adjustingthether...

Страница 68: ...properly Make sure you have Made all necessary cable connections between the TMA and the TA controller Connected all gas lines Powered on each unit Installed all appropriate options Configured the in...

Страница 69: ...ware online documentation Force Calibration Force calibration calibrates the force exerted by the probe on the sample during experiments using two weights and can be performed with any probe in place...

Страница 70: ...rument mode or when you change a probe on the TMA 2940 CE This calibration is performed from the TA controller Temperature Calibration Temperature calibration is based on a run in which a temperature...

Страница 71: ...e crimped into the aluminum balls and used for calibration When to Calibrate The sample thermocouple should be calibrated in thefollowingsituations When the TMA is first installed When the sample ther...

Страница 72: ...ell constant value of 1 000 is usually adequate however for greatest accu racy calibration should be performed It is recommended that you follow the proce dures of ASTM Standard Test Method E831 to pe...

Страница 73: ...TA INSTRUMENTS TMA 2940 CE 3 9 5 Calculate the cell constant using the follow ingequation Expected literature expansion Observed expansion Kcell Calibrating the TMA...

Страница 74: ...robe Selecting and preparing a sample This involves preparing a sample of the appropriate size and placing the sample in the sample stage Enteringexperimentalinformationthrough the TA controller Creat...

Страница 75: ...ble 3 1 TMA 2940 CE Probes Probe Type Contact Pressure Types Diameter Exerted by of Tests mm in 0 01 N Load Yielded Penetration 0 89 0 035 16 kPa Softeningpoint Melting point Expansion 2 54 0 100 1 9...

Страница 76: ...nstall any optional probes 3 Select the mode that is appropriate for the type of probe installed Refer the the instrument control software documentation forinformation 4 Calibrate a newly installed pr...

Страница 77: ...may experience temperature gradients during high heating rates Thermoplastic samples can be heated and formed into suitable specimens and then cooled however this process may change importantthermalhi...

Страница 78: ...en the stage and any thermoplastic samples to prevent damage to the stage Figure 3 1 Loading a Sample 6 Adjust the sample thermocouple if needed as directed on the next page 7 Program the force on the...

Страница 79: ...f the size or shape of the sample that you are running on the TMA position the tip of the thermocouple so that it bends at a 90 angle and lies flat against the platform It should be close to but not t...

Страница 80: ...tions Refer to the software online documenta tion to learn how to perform the following steps 1 Select the Instrument 2 Select the Instrument Mode 3 Enter Sample Information 4 Enter Instrument Inform...

Страница 81: ...segments in the method This section describes how to use the following accessories with the TMA 2940 CE Aircooloption Purge gas TA Instruments Gas Switching Accessory Using Air Cool Before you start...

Страница 82: ...the furnace and purge the system with nitrogen for 10 minutes Then switch to helium gas for the experiment if desired To ensure an inert environment for your sample a purge rate of 100 mL min is sugge...

Страница 83: ...a denser purge gas than helium is used for subambient experiments it is recommended that the silicon washer found in the accessory kit be attached to the probe Raise the probe to the fully open posit...

Страница 84: ...ed The REJECT function discards all experiment data Removing Samples After the experiment has completed allow the sample to cool down so that you can touch it then the sample can be removed as follows...

Страница 85: ...he probe and stage in an acid solution Use extreme caution when working with acid solutions Heat is not recommended with metallic materials as heat causes the metal to diffuse into the quartz and will...

Страница 86: ...turn to temperature range method end condition is activated press the STOP key to deactivate it before trying to cool the TMA Performing a Cooling Experiment To run a subambient experiment perform the...

Страница 87: ...er to perform subambient experiments the furnace must work against the coolant in the furnace reservoir Ideally you should use the least amount of coolant necessary to keep the furnace drawing power o...

Страница 88: ...as than helium is used for subambient experiments it is recommended that the silicon washer found in the accessory kit be attached to the probe Raise the probe to the fully open position then place th...

Страница 89: ...isting Probe 4 6 Removing the Stage 4 6 Changing the Instrument Mode 4 7 InstallingtheFilm FiberProbe 4 7 InstallingtheFilm FiberStage 4 8 Calculating the Offset 4 9 Calibration 4 11 Sample Preparatio...

Страница 90: ...ibration 4 24 DisplacementCalibration 4 25 Sample Preparation 4 26 Parallel Plate Rheometer Accessory 4 29 Description 4 29 Accessory Installation 4 29 Calibration 4 30 Sample Preparation 4 31 Sample...

Страница 91: ...iew This chapter explains the optional accessories that you can purchase to use on your TMA 2940 CE includingthefollowinginformationforeach option Description Operating procedures Accessoryinstallatio...

Страница 92: ...ilms as a function of force temperature or time Sample tensile stress is calculated using the followingequation ST F A where ST stress at temperature T Pascals F force Newtons A cross sectional area m...

Страница 93: ...ing rate See the instrument control software online documentation for details When comparing run data make sure that all comparison scans are made with the thermo couple in the same position and at th...

Страница 94: ...gently and twist slightly to aid its removal from the stage opening Removing the Stage 1 Remove the stage shield from the base of the stage by lifting it straight up This is a frictionfit 2 Take off t...

Страница 95: ...configuration of the film fiber accessory requires the installation of the probe before the stage 1 Insert the core end of the probe carefully into the opening in the top plate 2 Open the weight tray...

Страница 96: ...the flange 3 Slide the stage retainer ring carefully over the top of the stage and probe assembly so that it rests on top of the wave washer Push down and turn clockwise to tighten the retainer ring...

Страница 97: ...the stage assembly and put on the spring clip to hold the thermocouple in place 7 Replace the stage shield on the base of the stage 8 Move the furnace back into position and lower it See Figures 4 4 a...

Страница 98: ...m fiber probe and stage assembly Change the Auto Measure Offset as follows 1 Record the value listed as Auto Measure Offset from the TA controller 2 Use calipers to measure the gap in the Auto Measure...

Страница 99: ...7 Remove the Auto Measure Gauge and proceed with your experiment Calibration You should perform probe temperature and cell constant calibration for the film fiber accessory as you would normally calib...

Страница 100: ...s Using the Aluminum Balls The aluminum balls are generally used with fiber samples as follows 1 Measure and cut the fiber sample slightly longer than desired length typically 12 to 25 mm 0 5 to 1 0 i...

Страница 101: ...slot in the stage with the fiber hanging down through the slot and allow the other ball to hang freely 7 Position the second ball below the slot in the film fiber probe so that the fiber is suspended...

Страница 102: ...Measure and cut the sample to the desired length typically 12 to 25 mm 0 5 to 1 0 inch Films should have a uniform width 2 Separate the jaws of one clamp Position the clamp so that the clamp relief no...

Страница 103: ...sample see Figure 4 5 5 Move the clamp into the desired notch position for either a 9 13 or 25 mm sample 6 Tighten the screws so that the sample is flat in the block and is positioned perpendicular to...

Страница 104: ...second clamp below the slot in the film fiber probe so that the film is suspended between the two clamps as shown in Figure 4 7 10 Measure the sample length 11 Position the thermocouple close to but...

Страница 105: ...obe and a sample platform with two knife edges spaced 5 08 mm 0 2 inches apart This acces sory permits the determination of deflection temperature under load Requiredloadingiscalculatedusingthefollowi...

Страница 106: ...rd stage if it is not already in place For instructions on installing the stage refer to page 2 13 3 Install the flexure probe in the same manner as the standard expansion and penetration probes using...

Страница 107: ...rotate it clockwise to move it off to the side 2 Remove any previously run samples from the stage and ensure that no residue re mains 3 Open the probe 4 Place the flexure platform on top of the stage...

Страница 108: ...ptions TA INSTRUMENTS TMA 2940 CE 4 20 Figure 4 8 Probe Setup Using Flexure Samples 8 Adjust the thermocouple position so that it is in close proximity to the sample 9 Move the furnace into position a...

Страница 109: ...f expansion The cubic expansion of a sample is calculated usingthefollowingequation K S B V where coefficient of expansion m3 m3 o C K vial constant cm3 m S slope m o C V sample volume cm3 This volume...

Страница 110: ...m3 m3 o C ref 3 ref Where ref is the coefficient of linear expansion of standard material m m o C measured over the same temperature range V sample volume cm3 This volume may be obtained by dividing t...

Страница 111: ...e data runs make sure that all comparison scans are made with the vial filled to the same level with filling medium with the thermocouple in the same position and heated at the same rate Accessory Ins...

Страница 112: ...seline and displacement using the procedures described as follows Baseline Calibration The dilatometer filling medium must be kept dry Store it in a desiccator when it is not being used If the sample...

Страница 113: ...mple 2 Weigh the three aluminum balls and prepare the sample and vial as instructed on the following pages Make sure that the alumi num balls do not touch the walls of the vial and that they do not to...

Страница 114: ...the filling medium 3 Select a sample that is small enough to easily fit inside the dilatometer vial without touch ing the walls 4 Place the sample on the filling medium in the center of the vial Make...

Страница 115: ...rom the stage and ensure that no residue re mains 9 Open the probe 10 Place the vial on the stage 11 Close the probe until the probe tip is posi tionedabovethefillingmedium 12 Tap lightly on the upper...

Страница 116: ...hermocouple position so that it is in close proximity to the vial To avoid false thermocouple readings make sure that the thermocouple tip does not touch the sample vial 16 Move the furnace into posit...

Страница 117: ...lates Alignment cage Accessory Installation The parallel plate rheometer accessory uses the macro expansion probe the rheometer sample holder assembly and the standard stage 1 Remove the existing prob...

Страница 118: ...ouple readings make sure that the thermocouple tip does not touch the alignment cages or plates Exposed portions of the two thermocouple leads must not touch each other Calibration The parallel plate...

Страница 119: ...e of the Sample Encapsulating Press PN 900680 902 and a special set of dies the pellet press die set To prepare samples follow the instructions found in these sections Sample Encapsulating Press__ see...

Страница 120: ...bly The plunger in the upper hermetic die assem bly is spring loaded and should be removed with care 1 Lower the Encapsulating Press handle Then rotate the die holder assembly and upper crimping die i...

Страница 121: ...ither hermetic or crimping just meets the upper hermetic die 5 Loosen the setscrew in the Encapsulating Press upper die holder assembly to unlock the upper hermetic die The upper hermetic die is now h...

Страница 122: ...nd screw in the pellet press base screw until it is nearly flush with the bottom of the press 4 Place the pellet press cylinder head cavity side down on top of the pellet press base screw 5 Lower the...

Страница 123: ...ollowtheseinstructions 1 Install the pellet press die set in the Encapsu lating Press as previously described 2 Pour sufficient sample material 30 to 50 mg into the pellet press cylinder to produce a...

Страница 124: ...he cylinder Note the position shown in Figure 4 13 Figure 4 13 Cylinder Head Positions 6 Replace the cylinder head and cylinder in the Encapsulating Press Lower the piston with the press handle This w...

Страница 125: ...TA INSTRUMENTS TMA 2940 CE 4 37 Figure 4 14 Parallel Plate Sample Assembly 9 Load your sample according to the directions on page 4 41 Parallel Plate Rheometer Accessory...

Страница 126: ...r head Piston 1 Assemble the pellet press cylinder and cylinder head in the sample forming posi tion for use as a mold as shown see Figure 4 15 Figure 4 15 Sample Forming Position 2 Heat up a hot plat...

Страница 127: ...he piston willsettle 7 Using tongs remove the weight when the piston sinks to its maximum depth 8 Remove the mold assembly from the hot plate using tongs and allow it to cool to room temperature 9 Dis...

Страница 128: ...these instructions 1 Cut a sample from a sheet of material 0 25 to 1 00 mm in thickness using a standard 9 5 mm hole punch 2 Measure the sample thickness using cali pers to within 0 02 mm 3 Place the...

Страница 129: ...it is in close proximity to the sample To avoid false thermocouple readings make sure that the thermocouple tip does not touch the alignment cage sample or plates Exposed portions of the two thermocou...

Страница 130: ...ts the parallel plates together inside the cage If you want to reuse the parts followthesedirections These procedures involve the use of heat or chemicals appropriate safety measures should be observe...

Страница 131: ...Correction Calculations for Thermal Expansion of Parallel Plates 1 Calculate the apparent distance between the plates h at a given temperature or time by subtracting the decrease in distance between...

Страница 132: ...Multiply this by the total plate thick ness and the temperature change to obtain the thermal expansion correction factor c Subtract the correction factor from the apparent distance between the plates...

Страница 133: ...Plate Rheometer Accessory Table 4 1 Stainless Steel Coefficient of Expansion1 T o C Coefficient of Expansion m mo C 18 14 8 93 16 0 149 16 6 204 16 7 260 16 9 316 17 3 371 17 5 427 17 6 482 17 8 538 1...

Страница 134: ...rected for expansion of the parallel plates as previously shown on page 4 43 Then this corrected data is applied to equations developed by Dienes and Klemm J Appl Phys 17 458 1946 and Cessna and Jablo...

Страница 135: ...dard quartz stage to obtain softening point data on substances It is installed operated and calibrated using the same proce dures as for the standard expansion and penetra tion probes Refer to Chapter...

Страница 136: ...Using Your Options TA INSTRUMENTS TMA 2940 CE 4 48...

Страница 137: ...MENTS TMA 2940 CE 5 1 CHAPTER 5 Technical Reference Description of the TMA 2940 CE 5 3 Uses of ThermomechanicalAnalysis 5 4 Calculatingthe Coefficient of Expansion 5 5 MethodConsiderations 5 6 Status...

Страница 138: ...Technical Reference TA INSTRUMENTS TMA 2940 CE 5 2...

Страница 139: ...artz probe placed in contact with the sample is used to determine any linear or volumetric changes in dimension at the selected temperature and force Valuable data on melting points glass transition t...

Страница 140: ...and labs It is used for quality control studies analysis of processing conditions and performance characterization of samples The samples analyzed using the TMA vary widely They can include materials...

Страница 141: ...ile of a sample To calculate the coefficient of expansion experi mental from the expansion profile you can use the Data Analysis program or the following equation L x K T x L Where measured coefficien...

Страница 142: ...ftening temperatures studies of penetration temperature vs force are helpful to eliminate false values A heating rate of 5o C min or less is best for polymeric and elastomeric materials Temperature pr...

Страница 143: ...ool solenoid is opened to allow cooling air flow to the furnace Balance Force is being applied to balance the system at the center of the displacement range This is used for force calibration Calib Th...

Страница 144: ...ing Equilib The temperature is being equilibrated to the desired set point Err xxx An error has occurred xxx appears as a two or three digit code The TMA display gives the Error Code number the contro...

Страница 145: ...ure or by running a coolingramp Initial The temperature is equilibratingtothedesired set point When the temperature has reached equilibrium thestatuswill change to Ready Iso The thermal program is hol...

Страница 146: ...brated at the initial temperature and is ready to begin the next segment Press the START key to continue the method Reject The experiment has been terminated and the data erased Repeat The method is...

Страница 147: ...tatus Codes cont d Code Meaning Unstable The Isostrain segment has been initiated but the instrument has not or cannot meet the criteria specified Zeroing The LVDT is being positioned to center the pr...

Страница 148: ...Technical Reference TA INSTRUMENTS TMA 2940 CE 5 12...

Страница 149: ...e Keypad 6 5 Cleaning the Probe Assembly 6 5 Cleaning the Stage 6 6 Cleaning the Thermocouple 6 7 Replacements 6 8 Replacing the Thermocouple 6 8 Diagnosing Power Problems 6 11 Fuses 6 11 Furnace Powe...

Страница 150: ...Maintenance and Diagnostics TA INSTRUMENTS TMA 2940 CE 6 2...

Страница 151: ...nt operation of the TMA as follows Maintenance procedures needed to keep your instrument clean and in good working order Instructions on how to replace certain parts when needed Details on diagnosing...

Страница 152: ...d be performed by a representative of TA Instruments or other qualified service personnel Because there are high voltages in this instrument untrained personnel must not attempt to test or repair any...

Страница 153: ...e best for cleaning the keypad Wet the towel not the keypad with the glass cleaner and then wipe off the keypad and display Cleaning the Probe Assembly After each experiment check the probe assem bly...

Страница 154: ...r acetone on a soft cloth to wipe the top of the stage For thorough cleaning 1 Raise the furnace and rotate it clockwise to move it off to the side 2 Remove the stage shield 3 Take off the spring clip...

Страница 155: ...al or glassfiller The stage may also be cleaned in a nitric acidsolution Cleaning the Thermocouple Sample residue and dirt may interfere with the accuracy of the thermocouple readings To clean thether...

Страница 156: ...w thermocouple PN 944344 902 as a result of normal wear and tear accidental breakage contamination of the thermocouple etc Before removing the thermocouple you will need to perform the following steps...

Страница 157: ...CE 6 9 Figure 6 1 Plugging in the Thermocouple 4 Carefully thread the thermocouple tip first up through the hole in the top of the balance enclosure See the following figure Figure 6 2 Threading the T...

Страница 158: ...te the thermocouple through the guide to prevent interference with the balance mechanism A service loop is recommended to take up excess length 7 Slide the balance enclosure into position 8 Replace th...

Страница 159: ...e representative The only fuses that you should service yourself are the external fuses located on the instrument s control panel Both of these fuses are housed in safety approved fuse carriers labele...

Страница 160: ...ernal components including the furnace If this fuse blows you will get no response from the instrument when you attempt to turn it on Furnace Power Check Furnace power is always checked at the begin n...

Страница 161: ...light may be defective or a hardware problem may exist in the TMA 2940 CE call your TA Instruments Service Represen tative The heater light may also remain on after a method has terminated This can h...

Страница 162: ...sage means that the system has detected a power failure and has shut down The instrument will not restart until reset To reset press the Reset button on the TMA 2940 CE s back panel If ERR F02 appears...

Страница 163: ...ng and service personnel in checking and repairing the instrument The TMA Confidence Test The TMA runs a confidence test every time it is started or reset The confidence test checks most of the comput...

Страница 164: ...pends on the options installed The base level system takes about 12 seconds The longest tests are the RAM tests which take about 6 seconds After the tests are completed a sign on message is displayed...

Страница 165: ...MA has failed the confidence test the instrument cannot reliably perform any further functions Table 6 1 summarizes the primary confidence tests for the TMA 2940 CE Table 6 1 Primary Confidence Test a...

Страница 166: ...901 Standard TMA Accessory Kit consisting of 944122 901 1 Expansion Probe Assembly 944126 901 1 Penetration Probe Assembly 944123 901 1 Macro Expansion Probe Assembly 944120 901 1 Sample Stage 944017...

Страница 167: ...semblies 944144 001 1 Film Clamp Fixture 269789 001 1 Jeweler s Screwdriver 0 080inch 269793 001 10 Film Clamp Screws 0 80 944202 901 Dilatometer Accessory Kit consistingof 944124 901 1 Dilatometer Pr...

Страница 168: ...d Part Number Description 944204 901 Parallel Plate Rheometer Accessory Kit consisting of 943147 901 1 Rheometer Sample Forming Die Set 943125 000 3 Rheometer Alignment Cages 943126 000 6 Rheometer Pa...

Страница 169: ...Desk at 1 302 427 4070 SERVICE U S A For instrument service and repairs please call 1 302 427 4050 TA Instruments Ltd Europe House Bilton Centre CleeveRoad Leatherhead Surrey KT22 7UQ England Telephon...

Страница 170: ...e B P 608 78056Saint Quentin Yvelines Cedex France Telephone 33 1 30 48 94 60 Fax 33 1 30 48 94 51 TA Instruments Spain Waters Cromatograf a S A Divisi n TA Instruments Avda Europa 21 Pta Baja 28108 A...

Страница 171: ...n calculation 4 45 5 5 components 1 3 Confidence test 2 26 6 15 6 17 failure 6 17 numbers 6 17 connecting cables 2 19 controller keyboard 1 7 A accessories 1 12 installation 4 5 optional 1 13 4 3 sett...

Страница 172: ...4 4 vial constant 4 22 viscosity 4 46 wall shear rate 4 46 error codes fatal 6 17 nonfatal 6 17 expansion coefficient 4 44 experiment cooling type 3 22 example 3 3 3 16 setting up 3 16 startup 3 10 3...

Страница 173: ...9 location 2 11 power requirements 2 11 repacking See TMA 2940 unpack ing unpacking See TMA 2940 un packing Instrument Control 3 16 instrument keypad See TMA 2940 keypad Instrument Parameters 4 41 K...

Страница 174: ...ers A 1 powder samples preparing 4 35 power cable installation 2 25 POWER on off 1 11 power problems HEATER indicator light 6 13 power failures 6 14 POWER switch 1 11 2 25 2 26 probe calibration 3 6 f...

Страница 175: ...on 3 13 removal 3 20 Sample Encapsulating Press 4 31 description 4 31 sample preparation 3 13 dilatometer accessory 4 26 fiber 4 12 films 4 15 flexure accessory specifications 4 19 moldable powders 4...

Страница 176: ...ting material 4 43 TMA 2940 CE accessory kit 1 12 assembling 2 9 assembly 1 3 cabinet 1 3 calibration 3 5 See also Calibra tion TMA 2940 CE cont d cleaning 6 5 components 1 4 confidence test 2 26 6 16...

Страница 177: ...TA INSTRUMENTS TMA 2940 CE I 7 Index W wave washer removal 6 6 weight tray door installation 2 12 function 1 4 Z Zero Length 4 19 ZERO LENGTH key 1 8 3 12...

Страница 178: ...Index TA INSTRUMENTS TMA 2940 CE I 8...

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