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Preparing Samples

5–22

TA I

NSTRUMENTS

DSC A

UTOSAMPLER

Table 5.1

Specifications for

Properly Crimped Pans

Description

Illustration

Uniform folding of lid

around circumference

Flat surface on the

bottom of the pan;

no ridge around

circumference

No visible gaps between

lid and pan

Diameter of pan slightly

greater than 1/4 in.

(0.270 to 0.275 in.)

Содержание DSC Autosampler CE

Страница 1: ...R CE i DSC Autosampler CE Operator s Manual PN 825616 001 Rev B Text and Binder PN 825616 002 Rev B Text Only Issued November 1999 109 Lukens Drive New Castle DE 19720 Thermal Analysis Rheology A SUBS...

Страница 2: ...ity Thispublicationisnota license to operate under or a recommendation to infringe upon any process patents TA Instruments Operating Software Instrument Data Analysis and Utility Software and their as...

Страница 3: ...xi Autosampler CE Safety Labels xii Operation Safety xii Lifting the Instrument xiii Using This Manual xiv CHAPTER 1 Introducing the DSC Autosampler CE 1 1 Overview 1 3 General Features 1 4 Relationsh...

Страница 4: ...gy 1 25 CHAPTER 2 Preparing the Autosampler CE 2 1 Introduction 2 3 Preparing for Operation 2 4 Connecting the Heat Exchanger Cable 2 4 Installing the Autosampler CE Lids 2 5 Installing the Dust Cover...

Страница 5: ...nging the Motor Speed 3 9 Covering and Uncovering the DSC Cell 3 10 Loading and Unloading Sample Pans 3 11 Loading Pans 3 11 Unloading Pans 3 13 Stopping the Autosampler CE 3 15 The HALT Key 3 15 The...

Страница 6: ...libratingLidStoragePositions 4 21 Calibrating the Sample Tray 4 25 CheckingYourCalibration 4 29 The LOAD LIDS Test 4 30 The Verify Test 4 34 The Cycle Pans Test 4 35 CHAPTER 5 Preparing Samples 5 1 Ov...

Страница 7: ...PTER 6 Diagnostics 6 1 Using the Confidence Test Ready Light 6 3 Testing Autosampler CE Functions 6 6 The Cycle Lids Test 6 7 The Cycle Pans Test 6 8 The Sensors Test 6 9 The Rear Switches Test 6 16 T...

Страница 8: ...viii Table of Contents continued Messages on the Autosampler CE Display 6 25 Fatal Error Messages 6 25 Nonfatal Error Messages 6 29 Error Messages on the Controller Screen 6 48 Appendix A Parts Lists...

Страница 9: ...mportant and critical instructions Highlights important information about equip ment or procedures Emphasizes a procedure that may damage equipment or cause loss of data if not followed correctly Indi...

Страница 10: ...A INSTRUMENTS DSC AUTOSAMPLER CE x Help Lines To TA Instruments For Technical Assistance 302 427 4070 To Order Instruments andSupplies 302 427 4040 For Service Inquiries 302 427 4050 Sales 302 427 400...

Страница 11: ...rective 73 23 EEC on safety as amended by 93 68 EEC thefollowingspecificationsapply to the DSC Autosampler CE Safety EN 61010 1 1993 EN61010 2 010 1994 Emissions EN 55011 1991 CISPR 11 1990 Group 1 Cl...

Страница 12: ...ceable parts are contained within the electronics enclosure and hazardous voltages are present within NEVER put your fingers in the Autosampler CE s path when the turret assembly is moving The gripper...

Страница 13: ...move the turret assembly by pushing it with your hand Doing so could cause mechanical damage and calibration errors NEVER slide the Autosampler CE console to the right while the instrument is in use...

Страница 14: ...tem for operation Chapter 3 Describes how to use the Autosampler CE s manual keyboard to move the turret assembly and load and unload the cell Chapter 4 Provides the calibration procedures necessary f...

Страница 15: ...tests you can run from the DSC Autosampler CE keyboard and lists control ler and Autosampler CE error messages Appendix Lists the DSC Autosam pler CE part numbers and TA Instruments offices and phone...

Страница 16: ...TA INSTRUMENTS DSC AUTOSAMPLER CE xvi...

Страница 17: ...ew 1 3 General Features 1 4 Relationship to the System 1 7 Description 1 9 The Turret Assembly 1 10 The Gripper Fingers 1 11 The Sample Tray 1 12 The Keypad 1 13 The Display 1 20 The GPIB 1 20 System...

Страница 18: ...Introducing the DSC Autosampler CE TA INSTRUMENTS DSC AUTOSAMPLER CE 1 2...

Страница 19: ...ent The Autosampler CE will detect the presence of a single or dual sample cell and adjust its actions and displays accord ingly Once the Autosampler CE loads the pans and covers the DSC cell the cont...

Страница 20: ...pans with the Autosampler CE s tactile feedback gripper fingers The tactile feedback programming also detects improperly gripped or dropped objects and prevents the grippers from puncturing the floor...

Страница 21: ...it and save it on disk You can even change parts of an AS run sequence as it is beingrun Up to 62 DSC runs can be preprogrammed on the controller The Autosampler CE s accuracy of pan placement 0 008...

Страница 22: ...100 o C at the beginning of each run by using compressed ambient air to rapidly cool or warm the DSC cell as needed You can further narrow this temperature range if you wish when you create your AS r...

Страница 23: ...1 Figure 1 1 Schematic Diagram of the DSC Autosampler CE System The TA Instruments LNCA Liquid Nitrogen Cooling Accessory and RCS Refrigerated Cooling System can be used for cooling experi ments with...

Страница 24: ...h LNCA Figure 1 3 Autosampler CE System with RCS DSC with the AUTOSAMPLER CE GPIB 15 TO 120 PSI LAB AIR CELL LNCA Coolant Line GPIB CELL CONTROLLER RCS Gas Connections ELECTRICAL CABLE PNEUMATIC TUBE...

Страница 25: ...ssembly that mounts on the instrument see Figures 1 4 and 1 5 The functions of the DSC instrument keypad and display will not change when the Autosampler CE is mounted See the appropriate DSC Operator...

Страница 26: ...re 1 6 Rotary stepper motors rotate the turret assembly in the clockwise or counter clockwise direction along the q axis and move the turret arm in and out along the r axis A linear stepper motor move...

Страница 27: ...ure 1 7 open and close to firmly grasp each sample pan while not disturbing the material in the pan They are made of conductive stainless steel and are controlled by tactile feedback sensors that dete...

Страница 28: ...OSAMPLER CE 1 12 The Sample Tray The sample tray is constructed of anodized aluminum and has a clear acrylic cover see Figure 1 8 It holds up to 62 pans Chapter 5 describes how to set up the sample tr...

Страница 29: ...open the keypad cover by loosening the captive thumbscrews in the cover see Figure 1 9 and tilting the cover down When you are ready to start a method close the keypad cover and finger tighten the th...

Страница 30: ...ts of four types of keys see Figure 1 10 Autosampler CE control keys ENTER MANUAL AUTOMATIC ESCAPE CLEAR RESET SAMPLER HALT RESUME Command keys which tell the Autosampler CE to execute a series of mov...

Страница 31: ...mined by the stage of operation of the Autosampler CE The numeric entry function is active only when the Autosampler CE is requesting numeric input otherwise the com mand or direction on the upper hal...

Страница 32: ...lid andtraypositions on the Autosampler CE see Chapter 4 ENTER Enters numeric re sponses selects items from a menu and stores calibrationpositions ESCAPE Terminates any Autosam CLEAR pler keypad entr...

Страница 33: ...uested indicated byblinkingcursor you can clear the current entry by pressing the ES CAPE CLEAR key In this case the CLEAR function is active HALT Provides two major functions see Chapter 3 Temporaril...

Страница 34: ...mpler AUTOMATIC CE back and forth between manual and automatic modes see Chapter 3 Motion Move the turret assembly Keys inthedirectionindicated on each key see Chapter 3 RESET Clears all commands and...

Страница 35: ...to change the speed of manual Auto sampler CE movement see Chapter 3 In automatic mode the Autosampler CE operates at preselected speeds dependingon the function being performed TEST Runs diagnostic...

Страница 36: ...play is independent of the DSC instrument display refer to the DSC Operator s Manual for details on theinstrumentdisplay Figure 1 11 Autosampler CE Screen The GPIB The GPIB General Purpose Interface B...

Страница 37: ...crimping die included with the DSC Autosampler CE These optional components can be included A nitrogen gas purge An additional gas purge controlled by the TA Instruments Gas Switching Accessory The T...

Страница 38: ...mal Solutions Advantage User Reference Guide for information on the automatic mode Once the Autosampler CE is in automatic mode it can be in one of two states Online remote in which the controller is...

Страница 39: ...run sequences that automatically load samples run methods and unload samples at the end of the experiment Maintain a log that records all activities of the Autosampler CE Axis Terms The terms r axis...

Страница 40: ...er CE TA INSTRUMENTS DSC AUTOSAMPLER CE 1 24 Rotational movement clockwise and counter clockwise occurs along the q axis theta axis Figure 1 13 The q Axis Upward and downward movement occurs along the...

Страница 41: ...tandard thermal analysis method is executed The DSC cell is returned to a near ambient temperature The DSC furnace is uncovered The reference and sample pans are removed from the DSC furnace An AS run...

Страница 42: ...Introducing the DSC Autosampler CE TA INSTRUMENTS DSC AUTOSAMPLER CE 1 26...

Страница 43: ...PLER CE 2 1 CHAPTER 2 Preparing the Autosampler CE Introduction 2 3 Preparing for Operation 2 4 Connecting the Heat Exchanger Cable 2 4 Installing the Autosampler CE Lids 2 5 Installing the Dust Cover...

Страница 44: ...Preparing the Autosampler CE 2 2 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 45: ...section contains certain procedures that need to be performed occasion ally as part of the Autosampler CE setup Once you have completed setting up your Autosampler CE as directed in this chapter you...

Страница 46: ...mpler CE you need to connect the heat exchanger cable to the instrument The LNCA Operator s Manual contains more details on installing the heat exchanger Connect the heat exchanger as follows 1 Make s...

Страница 47: ...ateri als In order to ensure that the Autosampler CE operates correctly while picking up and placing each lid in the appropriate place you must make sure that the lids are installed in the proper loca...

Страница 48: ...henever you leave the Autosampler CE to run a series of samples This will prevent dust and dirt from interfering with your experiments To put the dust cover on simply insert the lip into the slot on t...

Страница 49: ...you will need to calibrate it so that it will properly pick up and deposit pans Calibration is done using the manual mode functions which are described in the next chapter If you need information on...

Страница 50: ...Preparing the Autosampler CE 2 8 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 51: ...3 5 Understanding the Confidence Tests 3 6 Moving the Turret Assembly 3 7 The Motion Keys 3 8 Changing the Motor Speed 3 9 Covering and Uncovering the DSC Cell 3 10 Loading and Unloading Sample Pans...

Страница 52: ...Using the Autosampler CE in the Manual Mode 3 2 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 53: ...apter describes the following manual mode procedures Switching to manual mode Moving the turret assembly manually Covering and uncovering the DSC cell Loadingandunloadingpans Stopping Autosampler CE m...

Страница 54: ...ER switch on the DSC Autosampler CE The Autosampler CE displays Confidence Test Version x x then Copyright 1986 TA Instruments Inc See page 3 6 for a discussion of the confidence tests When the confid...

Страница 55: ...ey on the Autosampler CE keypad The display reads Automatic Mode Halted 3 Press the MANUAL AUTOMATIC key The display reads Manual Mode Idle The Autosampler CE is now in manual mode and is ready for a...

Страница 56: ...t If the display fails it may remain blank or display random letters and symbols If the Autosampler CE test error is noncritical to the remaining tests the confidence tests finish but the last error m...

Страница 57: ...igure 3 1 are used to move the turret assembly in the direction indi cated on the key You can change the speed of the turret motion with the SPEED key The motion and SPEED keys are explained on the fo...

Страница 58: ...Moves the turret counterclockwise untilthecounterclock wise limit is reached RAISE Raises the turret until the upper limit is reached LOWER Lowers the turret until the lower limit is reached EXTEND Ex...

Страница 59: ...ur selection 1 Access the Autosampler CE keypad by loosening the captive thumbscrews on the keypad cover and tilting the cover down 2 Press the SPEED key The Autosampler CE displays the current speed...

Страница 60: ...ver or 2 Cover Uncover 1 or Cover 2 1 3 Select an option by pressing a numeric key then pressing ENTER If you select option 1 the Autosampler CE uncovers the cell and returns all cell lids to their st...

Страница 61: ...he DSC cell when its tempera ture is above 100o C Loading Pans To load sample pans to the DSC cell in manual mode follow these steps 1 Access the Autosampler CE keypad by loosening the captive thumbsc...

Страница 62: ...an Number 1 5 Type a number between 1 and 62 then press ENTER The Autosampler CE loads the pan to the cell position you chose in step 3 If there is already a pan in the cell position you selected the...

Страница 63: ...ng the captive thumbscrews on the keypad cover and tilting the cover down 2 Press the LOAD key You are prompted to select option 1 Load or 2 Unload Load 1 or Unload 2 1 3 Select the Unload option by p...

Страница 64: ...AMPLER after loading them with the LOAD key you must enter a returning pan number you cannot use sample pan number 0 Press RESET SAMPLER to clear the Autosam pler CE s memory whenever you remove a pan...

Страница 65: ...me action with the Autosampler CE RESUME key The Autosampler CE then completes the task that was interrupted When the Autosampler CE is in manual mode you can use the motion keys to move the turret as...

Страница 66: ...vious command after you press the RESET SAMPLER key The RESET SAMPLER Key When the RESET SAMPLER key is pressed in manual mode all commands are cleared the cell is assumed to be empty and all pans to...

Страница 67: ...u press ENTER to continue the reset the displayshows Manual Mode Resetting When the Autosampler CE reaches home position thedisplaydisplays Manual Mode Idle and the Autosampler CE is ready for a com m...

Страница 68: ...move them manually with tweezers or the Autosampler CE motion keys The Autosam pler CE does check that all lids are in their storage positions and displays an error message if they are not If you pres...

Страница 69: ...brationChecklist 4 8 PerformingtheCalibration 4 9 CalibratingtheCellLidPositions 4 11 Calibrating the Cell Pan Positions 4 15 CalibratingtheLid Storage Positions 4 21 Calibrating the Sample Tray 4 25...

Страница 70: ...Calibrating the Autosampler CE 4 2 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 71: ...listed and illustrated in Table 4 1 beginning on the next page You will need to calibrate the cell lid and cell pan positions using the procedures described on pages 4 11 to 4 20 The lid storage and...

Страница 72: ...ate Verify Lid 2 Cell Calibrate Verify Lid 3 Cell Table 4 1 Autosampler CE Calibration Position Screen Display Autosampler CE Position Thesmall silverlid spositionon the DSC cell Themedium sized stain...

Страница 73: ...ition The dimple in a DSC cell where the sample pan is placed For dual sample cells not shown choose side A or B The small silver lid s storage position table continued Calibrate Verify Sample Pos Cal...

Страница 74: ...Calibrate Verify Lid 2 Storage Calibrate Verify Lid 3 Storage Table 4 1 Autosampler CE Calibration Position continued Screen Display Autosampler CE Position Themedium sized stainless steel lid sstora...

Страница 75: ...e 4 1 continued Screen Display Autosampler CE Position Position 1 on the sample tray Position 11 on the sample tray Position 59 on the sample tray Calibrate Verify Tray Pos 11 Calibrate Verify Tray Po...

Страница 76: ...not recommended for calibration When you have finished and checked your calibration you can cycle hermetic or open pans for furtherverification The DSC cell is level and properly installed Air lines...

Страница 77: ...osampler CE was performing a Verify function press RESET SAMPLER and repeat the Verify operation to recheck the position If it is incorrect HALT the Auto sampler CE again press ESCAPE CLEAR to cancel...

Страница 78: ...peeds when you are moving the turret for longer distances For more information on the SPEED key please see Chapter 3 5 If the grippers either empty or holding a pan or lid contact the DSC cell furnace...

Страница 79: ...omeposition 3 Make sure all lids are in their storage positions see Table 4 1 4 Press the LIDS key The screen displays Uncover 1 or Cover 2 1 5 Select option 2 Cover by pressing the 2 key then pressin...

Страница 80: ...ositioned press the CALIBRATE key until you see the correct cell lid position on thedisplay Calibrate Verify Lid 1 Cell 9 Press ENTER The screen displays Verify 1 or Store 2 1 LID IN OPEN POSITION FIN...

Страница 81: ...splay Calibrate Verify Lid 1 Cell 12 Press ENTER The screen displays Verify 1 or Store 2 1 13 Press ENTER to select default option 1 Verify 14 When the turret stops moving close and open the grippers...

Страница 82: ...return the lids to their storage positions select option 1 Uncover 17 Press ESCAPE CLEAR to exit the calibra tion procedure 18 If you are calibrating a newly installed Autosampler CE go on to Calibrat...

Страница 83: ...e captive thumbscrews on the keypad cover and tilting the cover down 2 Press RESET SAMPLER and ENTER to bring the Autosampler CE to the home position 3 Make sure the cell lids are in their storage pos...

Страница 84: ...ENTER The Autosampler CE picks up the pan in tray position 1 and begins moving toward the cell 8 Press ESCAPE CLEAR when the Auto sampler CE reaches the DSC cell area 9 Use the motion keys to positio...

Страница 85: ...tion 2 Store to store the calibra tion position press the 2 key then press ENTER The screen displays Cell Ref Pos Calibrated 13 Release the pan press the RELEASE key Press RESET SAMPLER and ENTER to b...

Страница 86: ...een displays Load Ref 1 or Sample 2 1 19 Select option 2 Sample by pressing 2 then ENTER The screen displays Sample Pan Number 1 20 Select tray position 2 press the 2 key then press ENTER The Autosamp...

Страница 87: ...or Store 2 1 25 Select option 2 Store to store the calibra tion position press the 2 key then press ENTER The screen displays Sample Pos Calibrated 26 Release the pan press the RELEASE key Press RESET...

Страница 88: ...riteria in Figure 4 2 Remember to release the pan and raise the turret out of the cell with the RAISE key 30 Use the LOAD key to remove the pans from the cell 31 Press ESCAPE CLEAR to end the calibra...

Страница 89: ...Press RESET SAMPLER and ENTER to bring the Autosampler CE to home position 3 Check that the three cell lids are in their storage positions see Table 4 1 4 Use the motion keys to position the grippers...

Страница 90: ...position on thedisplay Calibrate Verify Lid 1 Storage 6 Press ENTER The screen displays Verify 1 or Store 2 1 7 Select option 2 Store to store the calibra tion position press the 2 key then press ENTE...

Страница 91: ...displays Verify 1 or Store 2 1 10 Press ENTER to select default option 1 Verify 11 When the turret stops moving close and open the grippers again and check your calibration against the criteria in Fi...

Страница 92: ...rage or Calibrate Verify Lid 3 Storage Step 7 Lid 2 Storage Calibrated or Lid 3 Storage Calibrated 13 Press ESCAPE CLEAR to exit the calibra tion procedure When you have finished using the Autosampler...

Страница 93: ...ive thumbscrews on the keypad cover and tilting the cover down 2 Press RESET SAMPLER and ENTER to bring the Autosampler CE to the home position 3 Make sure the sample tray is fully inserted 4 Place em...

Страница 94: ...INGERS SHOULD BE EQUIDISTANT FROM THE PAN ALL FOUR FINGERS SHOULD CONTACT THE PAN AT THE SAME TIME WHEN YOU PRESS THE GRIP KEY Figure 4 4 Calibrating a Tray Position 6 Press the CALIBRATE key repeated...

Страница 95: ...Tray Pos 1 10 Press ENTER The screen displays Verify 1 or Store 2 1 11 Press ENTER to select default option 1 Verify 12 When the turret stops moving close and open the grippers again and check your c...

Страница 96: ...Pos 11 or Calibrate Verify Tray Pos 59 Step 8 Tray Pos 11 Calibrated or Tray Pos 59 Calibrated 14 Press ESCAPE CLEAR to exit the calibra tion procedure When you have finished using the Autosampler CE...

Страница 97: ...ess the HALT key if the Autosampler CE turret arm starts to run intosomething If the Autosampler CE has trouble completing any of the tests or displays any error messages note the position s showing a...

Страница 98: ...he cover down Step A Use the LOAD key to test the Autosampler CE s ability to load and unload pans from the tray to the DSC cell 1 Press RESET SAMPLER and ENTER to bring the Autosampler CE to the home...

Страница 99: ...ng the 2 key then pressing ENTER 10 Select tray position 45 press 45 then press ENTER The Autosampler CE loads the pan in tray position 45 into the cell sample or sample A position 11 Press the LOAD k...

Страница 100: ...17 Select option 1 Ref by pressing ENTER The screen displays Sample Pan Number 0 18 Select default tray position 0 by pressing ENTER tray position 0 tells the Autosam pler CE to return the pan to the...

Страница 101: ...2 key then pressing ENTER The Autosam pler CE removes all lids from their storage positions and places them on the cell 4 Press the LIDS key again The screen displays Uncover 1 or Cover 2 1 5 Select...

Страница 102: ...position you want to check 4 Press ENTER The screen displays Verify 1 or Store 2 1 5 Select option 1 Verify by pressing ENTER The Autosampler CE should move to the position you selected in step 2 6 U...

Страница 103: ...he keypad cover and tilting the cover down 2 Press RESET SAMPLER and ENTER to bring the Autosampler CE to home position 3 Load the sample tray with at least five empty crimped pans Use sample tray pos...

Страница 104: ...n the cell The lids are removed The pans are returned to their storage positions If you must stop the test because of calibra tion errors press the ESCAPE CLEAR key 7 Press ESCAPE CLEAR to stop the Cy...

Страница 105: ...amples Overview 5 3 InstallingtheCrimpingDie 5 4 Setting Up the Sample Tray 5 9 Autosampler CE Run Capacity 5 10 Reuse of Pans 5 11 Order of Runs 5 12 Pan Metal and Type 5 13 Preparing Sample Pans 5 1...

Страница 106: ...Preparing Samples 5 2 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 107: ...AUTOSAMPLER CE 5 3 Overview This chapter explains how to Install the TA Instruments crimping die in the Sample Encapsulating Press Set up the sample tray Prepare crimped and hermetic pans for Autosamp...

Страница 108: ...ng die designed to work with the TA Instruments Autosampler CE crimped pans Follow the steps below to install the crimping die in the Sample Encapsulating Press before preparing crimped pans for Autos...

Страница 109: ...2 Turn the sample press on its back Figure 5 2 Turning the Sample Encapsulating Press on its Back 3 Turn the base screw counterclockwise to lower the height of the lower die Figure 5 3 Lowering the B...

Страница 110: ...mples 5 6 TA INSTRUMENTS DSC AUTOSAMPLER CE 4 Set the sample press upright Figure 5 4 Setting the Sample Encapsulating Press Upright 5 Lift the lower die out of the sample press Figure 5 5 Removing th...

Страница 111: ...e 5 6 then lift the inner core out of the die Figure 5 6 Removing the Inner Core from the Lower Die 7 Insert the new inner core included with the Autosampler CE see Figure 5 7 into the die Retighten t...

Страница 112: ...er die 10 Tilt the sample press back up and bring the lever down to test the height of the lower die The upper die should just touch the lower die when the lever is fully down 11 Repeat steps 9 and 10...

Страница 113: ...ay Before you prepare your sample pans and set up the sample tray you should consider the follow ing Sample and run capacity Reuse of pans Order of runs Pan metal and type Each of these considerations...

Страница 114: ...g runs in an AS run sequence is limited by the amount of liquid nitrogen in the LNCA tank The rate at which the liquid nitrogen is used up depends of course on your method the temperature you use how...

Страница 115: ...decrease the number of actual samples in the AS run sequence Reuse of Pans Because thermal analysis experiments can sometimes deform the pans or cause the sample material to boil out we do not recomm...

Страница 116: ...d at a minimum by putting all cooling only runs at the beginning of the AS run sequence If you plan to runcombinationcooling heatingmethods these methods should come next followed finally by anyheatin...

Страница 117: ...mpler CE operates using the following types of TA Instruments pans Autosampler CE crimped pans Hermetic pans Open pans These pans are available in a variety of metals Any pan metal can be used with th...

Страница 118: ...the Auto sampler CE cannot remove a pan from the cell because of deformation or boiled out material operation is halted until the problem is corrected Thus before you use the Autosampler CE for unatte...

Страница 119: ...ting Press we recommend that you practice the following procedures with empty pans before attempting to seal a sample If you wish to prepare additional trays of samples while a tray is being run on th...

Страница 120: ...Preparing Samples 5 16 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 121: ...TS DSC AUTOSAMPLER CE 5 17 Tray Cell Reference Sample Name or Sample Method Position Position Pan Reference Pan Type Weight File 3 6 9 14 29 31 1 2 4 5 7 8 10 11 12 13 15 16 17 18 19 20 21 22 23 24 25...

Страница 122: ...INSTRUMENTS DSC AUTOSAMPLER CE Tray Cell Reference Sample Name or Sample Method Position Position Pan Reference Pan Type Weight File 32 33 34 36 37 35 38 42 48 56 59 60 61 62 58 57 55 54 53 52 51 50 4...

Страница 123: ...0001 gram and record the weight Figure 5 8 TA Instruments Crimped Pan 2 Leave the pan and cover in the balance and place your sample in the pan Record the weight 3 Subtract the weight you obtained in...

Страница 124: ...le Encapsulating Press Set Up for Nonhermetic Crimping 5 Place the cover over the pan If the sample is small or thin align the cover with the pan see Figure 5 10 If the sample is large invert the cove...

Страница 125: ...e the lever and remove the pan from the well Check the pan to ensure that it meets the specifications outlined in Table 5 1 next page If the pan does not meet the specifications in Table 5 1 you may n...

Страница 126: ...cifications for Properly Crimped Pans Description Illustration Uniformfoldingoflid around circumference Flat surface on the bottom of the pan no ridge around circumference No visible gaps between lid...

Страница 127: ...ay and record the cell position corresponding reference pan number and sample name in the Sample Information Chart see example in Figure 5 11 A column is also provided in this chart for the thermal me...

Страница 128: ...ic pan and cover see Figure 5 12 in a milligram balance measur ing accuracy of the balance must be 0 0001 gram and record the weight Figure 5 12 TA Instruments Hermetic Pan 2 Leave the pan and cover i...

Страница 129: ...pan in the well of the lower die of the Sample Encapsulating Press see Figure 5 13 Figure 5 13 The DSC Sample Press Set Up for Hermetic Sealing 5 Place the cover over the pan as shown in Figure 5 14 L...

Страница 130: ...TA INSTRUMENTS DSC AUTOSAMPLER CE Figure 5 14 Placing the Cover over the Hermetic Pan 6 Place the hermetic preforming tool grooved side down around the upper die plunger see Figure 5 15 Figure 5 15 Us...

Страница 131: ...it around the upper die plunger 9 Lower the lever again and push down gently untilitstopsmoving 10 Raise the lever and remove the pan from the well Check the pan to ensure that it meets the specificat...

Страница 132: ...Description Illustration Complete seal around circumference of pan Diameter of pan approximately5 16in 0 300 to 0 310 in 11 Place the pan in the Autosampler CE tray and record the cell position corres...

Страница 133: ...ycle Pans Test 6 8 The Sensors Test 6 9 The Rear Switches Test 6 16 The Keyboard Test 6 17 The GPIB Test 6 18 The Display Test 6 19 The Motion Test 6 20 The Cycle A B Test 6 22 Error Messages 6 24 Gen...

Страница 134: ...Diagnostics 6 2 TA INSTRUMENTS DSC AUTOSAMPLER CE...

Страница 135: ...p you can use the red Ready light on the unit s back panel see Figure 6 1 to determine whether the other confidence tests detect any errors Figure 6 1 The Autosampler CE Confidence Test Ready Light Fo...

Страница 136: ...r a long 3 4 second flash to indicate whether the system has passed or failed A short flash means that the system being tested has passed a long flash means that it has failed Table 6 1 on the next pa...

Страница 137: ...umber 1 EPROM checksum 2 Variable RAM 3 Liquidcrystaldisplay 4 8155 5 Keyboard 6 Location RAM 7 GPIB 8 RS 232 C 9 Timerinterrupt 10 Watchdog timer 11 Up down z axis motor and sensor 12 In out r axis m...

Страница 138: ...al mode key calls up a menu of tests that check the Autosampler CE s Calibration Cycle Lids test Cycle Pans test Sensors Configurationjumpers Keyboard operation GPIBconfiguration Display screen Motors...

Страница 139: ...displayed on the screen The Autosampler CE begins moving the cell lids from their storage positions to the cell When the cell is cov ered the Autosampler CE returns the lids to their storage position...

Страница 140: ...Press ENTER to select the test displayed on the screen The Autosampler CE begins loading the pan in tray position 1 into the cell reference position as indicated on the screen Cycle Pans 0001 Loading...

Страница 141: ...ors test displays a series of digits that indicate whether or not the Autosampler CE sensors are detecting an object 1 Access the Autosampler CE keypad by loosening the captive thumbscrews on the keyp...

Страница 142: ...its storage position and watch the screen If the digit changes from 0 to 1 or from 1 to 0 as you move the object the sensor is working correctly Table 6 3 pages 6 12 to 6 13 explains what each sensor...

Страница 143: ...AMPLER CE 6 11 Table 6 2 The Sensor Test Digits 0 0 0 0 0 0 0 0 0 0 0 Lid 3 storage Lid 2 storage Lid 1 storage Tray R axis Q axis cell Z axis not used Grippers Contact finger B Contact finger A Autos...

Страница 144: ...ed lid is in its storageposition 0 Lid 2 is not in its storageposition Lid 1 storage 1 Lid 1 the small lid is in its storage position 0 Lid 1 is not in its storageposition Tray 1 The sample tray is fu...

Страница 145: ...ingers are touching each other 0 The grippers are open Contact finger B 1 A finger one side of the grippers is contacting the cell 0 No contact Contact finger A 1 A finger one side of the grippers is...

Страница 146: ...Diagnostics 6 14 TA INSTRUMENTS DSC AUTOSAMPLER CE Figure 6 3 Arm Centered Over Turret Assembly Figure 6 4 Turret Over Cell...

Страница 147: ...TA INSTRUMENTS DSC AUTOSAMPLER CE 6 15 Figure 6 5 Turret in Full Up Position Autosampler CE Test Functions...

Страница 148: ...lting the cover down 2 Press the TEST key four times The Auto sampler CE screen displays Test Rear Switches 3 Press ENTER to select the test displayed on the screen The Autosampler CE displays a serie...

Страница 149: ...est displayed on the screen 4 Press each key on the Autosampler CE keyboard except the ESCAPE CLEAR key and watch the screen to ensure that the key displayed on the screen matches the one you are pres...

Страница 150: ...2 Press the TEST key six times The Auto sampler CE screen displays Test GPIB 3 Press ENTER to select the test displayed on the screen The screen should display a numeral ten higher than the address y...

Страница 151: ...d tilting the cover down 2 Press the TEST key seven times The Autosampler CE screen displays Test Display 3 Press ENTER to select the test displayed on the screen Strings of characters continu ously m...

Страница 152: ...s on Autosampler CE motor movement so that service personnel can perform motor diagnostics tests The software limits protect the hardware from damage and prevent the motors from being overdriven The f...

Страница 153: ...mbly reaches an obstacle Note that the GRIP and RELEASE keys move the fingers incrementally instead of fully opening and closing them in single keystrokes Once the turret stops moving release the moti...

Страница 154: ...collisions of the turret arm with the enclosure cell or sample tray are possible NEVER leave this test operat ing unattended Please contact an authorized service representative for further information...

Страница 155: ...nuously cycles between points A and B Be ready to press the HALT key to prevent possible collisions of the turret arm with the enclosure tray or cell Once you are sure that the path the Auto sampler C...

Страница 156: ...r messages please access the online help provided with the Thermal Solutions Advantage software for detailed instructions and read the guidelines given here You can access online help by opening the E...

Страница 157: ...intervention Fatal Error Messages Fatal error messages indicate a condition that must be corrected for operation to continue The Autosampler CE always stops operating when a fatal error occurs Fatal...

Страница 158: ...epresentative Fatal Error EPROM Checksum Problem The confidence test has detected that the EPROM erasable programmable read only memory containing the Autosampler CE programming has been partially era...

Страница 159: ...er CE is not operating correctly Solution Turn off the Autosampler CE and power up again If you still receive this message call a qualified service representative Fatal Error Timer Interrupt Problem T...

Страница 160: ...on Solution Turn off the Autosampler CE and power up again If you still receive this message call a qualified service representative Fatal Error Watchdog Timeout Problem The Autosampler CE has detecte...

Страница 161: ...tion has been erased Solution Recalibrate the position displayed on the screen see Chapter 4 Contact Error Finger X X A or B Problem One of the gripper fingers has touched the DSC cell Motion is stopp...

Страница 162: ...e gripper fingers have touched the DSC cell Motion is stopped when this occurs to prevent damage to the cell or gripper fingers All motion keys except the RAISE key become inoperable Solution Press th...

Страница 163: ...ect Problem 1 The Autosampler CE was switched to automatic mode while it was holding an object or was halted with the Halt Motion key while the grippers were closing on an object OR 2 You manually gri...

Страница 164: ...ve Error Lid x dropped Problem The Autosampler CE has dropped a lid lid 1 2 or 3 or had trouble picking it up This can be caused by 1 incorrect calibration 2 bent or damaged gripper fingers or 3 a fau...

Страница 165: ...ampler CE is gripping a lid the gripper sensor may be malfunc tioning test the gripper sensor with the TEST key Error Lid x not strd Lid x not stored Problem The Autosampler CE has been reset with one...

Страница 166: ...brating the related position s then repeat the task If the error occurs again call a qualified service representative Error Pan xx missing Problem A pan that the Autosampler CE is attempting to load o...

Страница 167: ...tosampler CE has been reset Errorr axis motor or sensor Problem The confidence test has detected that the r axis in out motor is not running properly or that motion of the turret arm is not being sens...

Страница 168: ...moving the q axis motor by pressing the ROTATE CW and ROTATE CCW keys If the turret assembly does not move the motor needs to be serviced If the turret moves test the q axis sensor with the TEST key s...

Страница 169: ...t move the motor needs to be serviced If the turret moves test the z axis sensor with the TEST key see page 6 9 If the sensor is malfunctioning have the sensor serviced GPIB Error 50 no command found...

Страница 170: ...ontroller to the Auto sampler CE Solution Close the DSC Instrument Control window and turn off the Autosampler CE Then restart the Autosampler CE reopen DSC Instrument Control and retry your operation...

Страница 171: ...CE reopen DSC Instrument Control and retry your operation GPIB Error 55 unknown AC type Problem An undefined GPIB command was sent from the controller to the Auto sampler CE Solution Close the DSC In...

Страница 172: ...CE does not contain a se quence number Solution Close the DSC Instrument Control window and turn off the Autosampler CE Then restart the Autosampler CE reopen DSC Instrument Control and retry your op...

Страница 173: ...ler CE Then restart the Auto sampler CE reopen DSC Instrument Control and retry your operation GPIB Error 60 bad pan number Problem The sample pan number in a GPIB command does not exist Solution Clos...

Страница 174: ...the DSC Instrument Control window and turn off the Autosampler CE Then restart the Autosampler CE reopen DSC Instrument Control and retry your operation GPIB Error 64 no pan in ref no pan in reference...

Страница 175: ...one of the Reset Sampler keys Solution Close the DSC Instrument Control window and turn off the Autosampler CE Then restart the Autosampler CE reopen DSC Instrument Control and retry your operation I...

Страница 176: ...operation GPIB Error 70 interface error Problem A GPIB interface error has occurred Solution Close the DSC Instrument Control window and turn off the Autosampler CE Then restart the Autosampler CE re...

Страница 177: ...steps or xxxxx steps Problem The r axis motor executed the wrong number of steps to complete a move ment The number is positive when the motor is retracting and negative when the motor is extending S...

Страница 178: ...direction and negative for the clockwise direction Small numbers of lost steps 25 indicate a loose or worn gear whereas frequent errors involvinglargernumbersindicatethat the motor is binding Solutio...

Страница 179: ...eps or xxxxx steps Problem The z axis motor had to execute the wrong number of steps to complete a movement The number is positive when the turret assembly is moving down and negative when it is movin...

Страница 180: ...he message number Further information on these A messages can be found when you access the online help provided with Thermal Solutions Advantage You can access online help by opening the Error Log in...

Страница 181: ...Printed Circuit Boards Part Number Description 911110 901 Motor Drive 984270 901 CommunicationsBoard Table A 2 Motors and Sensors Part Number Description 990720 901 Gripper Motor Assembly 990737 901 R...

Страница 182: ...Table A 4 Miscellaneous Parts Part Number Description 990732 901 Autosampler CE Sample Tray 62 position 990685 001 Die Punch for Crimped Sample Pan 990717 901 Gripper Finger Assembly 990687 001 Lid 1...

Страница 183: ...s Help Desk at1 302 427 4070 SERVICE U S A For instrument service and repairs pleasecall1 302 427 4050 TA Instruments Ltd Europe House Bilton Centre Cleeve Road Leatherhead Surrey KT22 7UQ England Tel...

Страница 184: ...8 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 28108Alcobendas Madrid Spain Telephone 34 91 661 8448 Fax 34 91 661 0855 TA I...

Страница 185: ...s features 1 6 display description 1 20 Display test 6 19 dust cover installing 2 6 Index A AS run sequences See Thermal Solutions User Reference Guide definition 1 25 automatic mode definition 1 22 s...

Страница 186: ...ge positions 4 21 to 4 25 installing 2 5 positions 2 5 testing 4 34 LNCA heat exchanger cable connecting 2 4 relationship to Autosampler 1 8 LOAD LIDS test 4 30 loading testing 4 35 E equipment requir...

Страница 187: ...1 3 13 to 3 15 parts lists A 1 to A 3 miscellaneous parts A 2 motors and sensors A 1 PC boards A 1 supplies A 2 POWER switch starting Autosampler with 3 4 R r axis definition 1 10 1 23 M manual mode c...

Страница 188: ...ogy 1 22 to 1 25 testing 1 25 testing Autosampler functions 6 6 Autosampler positions 6 22 calibration 4 29 to 4 36 Rear Switches test 6 16 requirements for running Autosampler CE equipment 1 21 syste...

Страница 189: ...1 10 1 24 tests Cycle Pans 4 35 6 8 to 6 9 Display 6 19 GPIB 6 18 Keyboard 6 17 LOAD LIDS 4 30 Motion 6 20 Rear Switches 6 16 Sensors 6 9 to 6 16 Verify 4 34 Thermal Solutions online help 6 48 q axis...

Страница 190: ...Index I 6 TA INSTRUMENTS DSC AUTOSAMPLER...

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