TA Instruments TGA 2950 Bedienungsanleitung

TA I

NSTRUMENTS

TGA 2950 i

Thermal Analysis & Rheology

TGA 2950

Thermogravimetric Analyzer

Operator’s Manual

PN 925602.001 Rev. D (Text and Binder)

PN 925602.002 Rev. D (Text Only)

Issued July 2000

TA I

NSTRUMENTS

TGA 2950ii

TA Instruments, Inc.

109 Lukens Drive

New Castle, DE 19720

Notice

The material contained in this manual is be-

lieved adequate for the intended use of this

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. This publica-

tion is not a license to operate under or a

recommendation to infringe upon any process

patents.

TA Instruments Operating Software and Mod-

ule, Data Analysis, and Utility Software and

their associated manuals are proprietary and

copyrighted by TA Instruments, Inc. 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 consent of TA Instruments.

Each licensed program shall remain the exclu-

sive property of TA Instruments, and no rights

or licenses are granted to the purchaser other

than as specified above.

TA I

NSTRUMENTS

TGA 2950 iii

Table of Contents

Notes, Cautions, and Warnings ................ xii

Hotline Numbers........................................xiv

Safety............................................................xv

Using This Manual.................................. xviii

CHAPTER 1: Introducing

the TGA 2950 ............................................1-1

Introduction................................................. 1-3

Components..........................................1-4

The 2950 Instrument...................................1-5

2950 Display ........................................ 1-5

2950 Keypad ........................................ 1-6

HEATER Switch ......................... 1-10

POWER Switch ...........................1-10

Accessories ...............................................1-11

Gas Switching Accessory...................1-11

Other Accessories ..............................1-11

Specifications............................................1-12

TA I

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TGA 2950iv

Table of Contents

(continued) CHAPTER 2: Installing

the TGA 2950 ............................................ 2-1

Unpacking/Repacking the 2950................... 2-3

Unpacking the 2950 .............................. 2-3

Repacking the 2950............................... 2-6

Installing the Instrument ............................. 2-7

Inspecting the System........................... 2-8

Choosing a Location ............................ 2-9

Filling the Heat Exchanger................. 2-10

Connecting Cables and Gas Lines...... 2-12

Heat Exchanger Cable

and Water Lines........................... 2-12

GPIB Cable.................................. 2-15

Purge Lines.................................. 2-17

Cooling Gas Line......................... 2-18

Power Cable................................. 2-19

Unpacking the Balance ............................. 2-20

Installing the Hang-Down Wires .............. 2-22

Aligning the Sample

Hang-Down Wire ............................... 2-25

Adjusting the Sample Platform................. 2-29

Starting the 2950........................................ 2-30

Shutting Down the 2950 ............................ 2-32

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TGA 2950 v

Table of Contents

(continued) CHAPTER 3: Running Experiments..... 3-1

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

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

Calibrating the TGA ...................................3-5

Temperature Calibration ...................... 3-5

Weight Calibration...............................3-6

Sample Platform Calibration ................ 3-6

Running a TGA Experiment.......................3-7

Experimental Procedure.......................3-7

Preparing Samples............................... 3-8

Selecting Sample and Tare Pans....3-8

Taring the Sample Pan...................3-9

Automatic Tare ..................... 3-10

Manual Tare ..........................3-10

Loading the Sample............................3-11

Setting Up an Experiment .................. 3-14

Setting Up Accessories ...................... 3-15

Using the Air Cool Option.......... 3-16

Using a Purge Gas ...................... 3-16

Using the Gas

Switching Accessory .................. 3-19

Starting an Experiment.......................3-20

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TGA 2950vi

Table of Contents

(continued)

Stopping an Experiment.....................3-21

Unloading the Sample ................. 3-21

Use in an Oxygen-Free Atmosphere.........3-22

Purge Gas System...............................3-22

Instrument Set-Up .............................. 3-23

CHAPTER 4: Technical Reference .......4-1

Description of the TGA 2950 .....................4-3

Components......................................... 4-5

Balance .......................................... 4-6

Sample Loading Assembly............ 4-8

Furnace .......................................... 4-9

TGA Standard Furnace ...........4-9

EGA Furnace ........................ 4-11

Cabinet.........................................4-13

Heat Exchanger............................ 4-15

Theory of Operation ................................. 4-16

Status Codes .............................................4-17

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TGA 2950 vii

Table of Contents

(continued)

CHAPTER 5: Maintenance

and Diagnostics ......................................... 5-1

Overview..................................................... 5-3

Routine Maintenance .................................. 5-4

Inspection .............................................5-4

Cleaning the Instrument ....................... 5-4

Cleaning the Furnace Housing .............5-5

TGA Standard Furnace Only.........5-5

Heat Exchanger .................................... 5-6

Maintaining Heat

Exchanger Coolant ........................5-6

Draining and Refilling

the Water Reservoir.......................5-6

Replacing the Thermocouple......................5-9

Removing and

Reinstalling the Furnace ...........................5-11

Furnace Removal ...............................5-11

Furnace Replacement ......................... 5-14

Diagnosing Power Problems.....................5-16

Fuses...................................................5-16

Power Failures....................................5-18

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TGA 2950viii

Table of Contents

(continued)

TGA Test Functions ................................. 5-19

The Confidence Test .......................... 5-19

Replacement Parts .................................... 5-21

Appendix A: Ordering Information ..... A-1

Appendix B: High Resolution

TGA Option.............................................. B-1

Overview.................................................... B-5

Option Installation ..................................... B-6

Using Hi-ResTM TGA................................. B-7

Background ......................................... B-7

The TA Instruments Hi-ResTM

Technique............................................ B-8

The Hi-ResTM Ramp Segment .................... B-9

Calcium Oxalate Example Scans ...... B-13

Advanced Hi-ResTM Techniques .............. B-18

What Can Be Resolved and

What Cannot?.................................... B-18

Unresolved Transitions ..................... B-19

Selecting a Hi-ResTM Technique ....... B-22

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TGA 2950 ix

Table of Contents

(continued)

Dynamic Rate Hi-ResTM Ramp.......... B-22

Constant Reaction Rate

Hi-ResTM Ramp.................................. B-23

Weight Gain Experiments ................. B-26

Signature Analysis ............................ B-27

Sample Quantity and Orientation...... B-28

Exposed Surface Area ................ B-28

Bubble Formation ....................... B-29

Thermocouple Placement ........................ B-32

Data Analysis Effects .............................. B-32

Derivative Plots ....................................... B-33

Adjusting Heating Rate ........................... B-34

Adjusting Resolution Setting................... B-37

Useful Resolutions Settings .............. B-39

Temperature Calibration.......................... B-41

Hi-ResTM Transition Temperatures ... B-42

Hi-ResTM Sensitivity Segment ................. B-43

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TGA 2950x

Table of Contents

(continued)

Understanding Sensitivity Setting..... B-44

Adjusting Sensitivity in

Dynamic Rate Mode ......................... B-45

Adjusting Sensitivity in Constant

Reaction Rate Mode.......................... B-47

Abort Segment......................................... B-51

Stepwise Isothermal Heating............. B-53

Hi-ResTM TGA Examples......................... B-58

Mixture of Bicarbonates.................... B-58

Dynamic Rate Scans................... B-59

Varying Resolution Setting ........ B-61

Varying Sensitivity Setting......... B-62

Constant Reaction Rate Scans .... B-63

Stepwise Isothermal Scans ......... B-65

Monosodium Glutamate.................... B-68

Banana Taffy..................................... B-69

Plastic Laboratory Tubing................. B-71

References ............................................... B-75

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